#==============================================================================
data_global
loop_
_journal_name_full 'European Journal of Chemistry'
_journal_coden_ASTM EJCUA9
_journal_volume 12
_journal_issue 2
_journal_year 2021
_journal_page_first 159
_journal_page_last 164
#==============================================================================
data_mii-c3ds002-per-cr3
_audit_creation_date 2021-01-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number '2018/3'
_audit_contact_author_address ?
_audit_contact_author_email ?
_audit_contact_author_name ''
_audit_contact_author_phone ?
_publ_contact_author_id_orcid ?
_publ_section_references
;
Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann,
H. (2009). J. Appl. Cryst. 42, 339--341.
Sheldrick, G. M. (2015). Acta Cryst. C71, 3--8.
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety
'C26 H24 Co N8 O2, 2(Cl O4), 2(H2 O)'
_chemical_formula_sum 'C26 H28 Cl2 Co N8 O12'
_chemical_formula_weight 774.39
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 8.880(5)
_cell_length_b 10.529(5)
_cell_length_c 18.430(5)
_cell_angle_alpha 99.407(5)
_cell_angle_beta 102.174(5)
_cell_angle_gamma 100.652(5)
_cell_volume 1618.2(13)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 11720
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 2.4120
_cell_measurement_theta_min 28.6423
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.768
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type ?
_exptl_absorpt_process_details ?
_exptl_absorpt_special_details ?
_exptl_crystal_colour brown
_exptl_crystal_density_diffrn 1.582
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 730
_exptl_crystal_size_max 0.10
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.05
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0341
_diffrn_reflns_av_unetI/netI 0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.841
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 16135
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.576
_diffrn_reflns_theta_min 2.525
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.841
_diffrn_measurement_device_type 'Kappa CCD'
_diffrn_measurement_method ?
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5762
_reflns_number_total 7648
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement ?
_computing_data_collection ?
_computing_data_reduction ?
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution ?
_refine_diff_density_max 0.967
_refine_diff_density_min -0.637
_refine_diff_density_rms 0.087
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.081
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 509
_refine_ls_number_reflns 7648
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0917
_refine_ls_R_factor_gt 0.0663
_refine_ls_restrained_S_all 1.081
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0845P)^2^+1.6552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1676
_refine_ls_wR_factor_ref 0.22
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H,H) groups
2. Others
Sof(O11)=Sof(H11A)=Sof(H11B)=FVAR(1)
3.a Free rotating group:
O11(H11A,H11B), O12(H12A,H12B)
3.b Aromatic/amide H refined with riding coordinates:
N2(H2), N6(H6), C11(H11), C12(H12), C25(H25), C17(H17), C24(H24)
3.c Idealised Me refined as rotating group:
C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.11085(5) 0.44949(5) 0.74381(3) 0.02839(16) Uani 1 1 d . . . . .
Cl1 Cl 0.43838(14) 0.25779(14) 0.52879(7) 0.0609(3) Uani 1 1 d . . . . .
Cl2 Cl 0.08656(19) -0.00768(15) 0.83389(9) 0.0730(4) Uani 1 1 d . . . . .
N7 N 0.3017(3) 0.3987(3) 0.75035(17) 0.0313(6) Uani 1 1 d . . . . .
O2 O 0.2438(3) 0.6122(2) 0.80368(15) 0.0342(6) Uani 1 1 d . . . . .
O1 O 0.0794(3) 0.3890(2) 0.83155(14) 0.0329(5) Uani 1 1 d . . . . .
N3 N -0.0769(3) 0.5010(3) 0.74609(17) 0.0287(6) Uani 1 1 d . . . . .
N2 N -0.1465(3) 0.4691(3) 0.80274(17) 0.0325(7) Uani 1 1 d . . . . .
H2 H -0.234589 0.484835 0.809807 0.039 Uiso 1 1 calc R . . . .
N4 N 0.0988(3) 0.5314(3) 0.65769(18) 0.0336(7) Uani 1 1 d . . . . .
N6 N 0.4351(3) 0.4929(3) 0.79159(19) 0.0356(7) Uani 1 1 d . . . . .
H6 H 0.530808 0.482919 0.800719 0.043 Uiso 1 1 calc R . . . .
N8 N 0.0278(3) 0.2743(3) 0.68333(18) 0.0334(7) Uani 1 1 d . . . . .
N5 N 0.7765(4) 0.8228(4) 0.9167(2) 0.0439(8) Uani 1 1 d . . . . .
N1 N -0.0276(4) 0.2695(3) 1.01700(19) 0.0423(8) Uani 1 1 d . . . . .
C14 C 0.5120(4) 0.7215(4) 0.8543(2) 0.0360(8) Uani 1 1 d . . . . .
C20 C 0.3017(4) 0.2790(4) 0.7216(2) 0.0340(8) Uani 1 1 d . . . . .
C6 C -0.0536(4) 0.4103(4) 0.8439(2) 0.0312(7) Uani 1 1 d . . . . .
C1 C -0.0997(4) 0.3665(3) 0.9099(2) 0.0316(7) Uani 1 1 d . . . . .
C5 C 0.0013(5) 0.3081(4) 0.9555(2) 0.0394(9) Uani 1 1 d . . . . .
C19 C 0.3888(4) 0.6002(4) 0.8142(2) 0.0328(8) Uani 1 1 d . . . . .
C8 C -0.2758(5) 0.6186(5) 0.6942(3) 0.0477(10) Uani 1 1 d . . . . .
H8A H -0.337720 0.576668 0.724253 0.072 Uiso 1 1 calc GR . . . .
H8B H -0.336944 0.600838 0.642613 0.072 Uiso 1 1 calc GR . . . .
H8C H -0.246307 0.712313 0.714053 0.072 Uiso 1 1 calc GR . . . .
C9 C -0.0279(4) 0.5872(4) 0.6454(2) 0.0338(8) Uani 1 1 d . . . . .
C7 C -0.1317(4) 0.5663(4) 0.6970(2) 0.0329(8) Uani 1 1 d . . . . .
C11 C 0.0584(6) 0.6778(5) 0.5472(3) 0.0587(12) Uani 1 1 d . . . . .
H11 H 0.045358 0.727162 0.509789 0.070 Uiso 1 1 calc R . . . .
C22 C 0.1421(4) 0.2048(4) 0.6796(2) 0.0351(8) Uani 1 1 d . . . . .
C18 C 0.6665(5) 0.7146(4) 0.8819(2) 0.0388(9) Uani 1 1 d . . . . .
C2 C -0.2389(5) 0.3798(4) 0.9295(3) 0.0407(9) Uani 1 1 d . . . . .
C3 C -0.2673(6) 0.3420(5) 0.9938(3) 0.0499(11) Uani 1 1 d . . . . .
C21 C 0.4437(5) 0.2226(5) 0.7307(4) 0.0477(11) Uani 1 1 d . . . . .
O3 O 0.4173(6) 0.2412(6) 0.4500(3) 0.1113(18) Uani 1 1 d . . . . .
C4 C -0.1599(5) 0.2876(4) 1.0367(3) 0.0457(10) Uani 1 1 d . . . . .
C13 C 0.2047(5) 0.5488(4) 0.6160(2) 0.0432(9) Uani 1 1 d . . . . .
O6 O 0.5792(6) 0.3302(7) 0.5721(4) 0.143(3) Uani 1 1 d . . . . .
C23 C 0.1043(6) 0.0784(4) 0.6373(3) 0.0492(11) Uani 1 1 d . . . . .
C26 C -0.1220(5) 0.2177(4) 0.6461(3) 0.0433(9) Uani 1 1 d . . . . .
C15 C 0.4741(6) 0.8441(4) 0.8636(3) 0.0503(11) Uani 1 1 d . . . . .
C12 C 0.1875(6) 0.6230(5) 0.5609(3) 0.0555(12) Uani 1 1 d . . . . .
H12 H 0.263077 0.635824 0.533115 0.067 Uiso 1 1 calc R . . . .
C25 C -0.1641(5) 0.0916(4) 0.6029(3) 0.0546(12) Uani 1 1 d . . . . .
H25 H -0.269145 0.054185 0.577498 0.065 Uiso 1 1 calc R . . . .
C17 C 0.7432(6) 0.9428(5) 0.9254(3) 0.0606(13) Uani 1 1 d . . . . .
H17 H 0.823010 1.017800 0.948761 0.073 Uiso 1 1 calc R . . . .
C24 C -0.0511(6) 0.0217(4) 0.5976(3) 0.0555(12) Uani 1 1 d . . . . .
H24 H -0.077814 -0.063124 0.567585 0.067 Uiso 1 1 calc R . . . .
C10 C -0.0527(6) 0.6591(5) 0.5896(3) 0.0487(11) Uani 1 1 d . . . . .
O4 O 0.3036(6) 0.2773(6) 0.5499(3) 0.1111(18) Uani 1 1 d . . . . .
O7 O 0.0603(11) -0.1393(7) 0.8025(5) 0.181(4) Uani 1 1 d . . . . .
C16 C 0.5926(6) 0.9539(5) 0.8998(3) 0.0647(14) Uani 1 1 d . . . . .
O9 O -0.0351(8) 0.0487(6) 0.8041(3) 0.130(2) Uani 1 1 d . . . . .
O10 O 0.0905(7) -0.0010(7) 0.9117(3) 0.126(2) Uani 1 1 d . . . . .
O5 O 0.4459(9) 0.1271(6) 0.5455(4) 0.142(2) Uani 1 1 d . . . . .
O8 O 0.2303(8) 0.0590(9) 0.8279(5) 0.182(4) Uani 1 1 d . . . . .
H2A H -0.300(5) 0.403(4) 0.903(2) 0.030(11) Uiso 1 1 d . . . . .
H13 H 0.283(4) 0.515(3) 0.628(2) 0.020(9) Uiso 1 1 d . . . . .
H18 H 0.694(5) 0.632(4) 0.882(2) 0.044(12) Uiso 1 1 d . . . . .
H16 H 0.572(6) 1.037(6) 0.902(3) 0.068(16) Uiso 1 1 d . . . . .
H21A H 0.469(8) 0.200(7) 0.775(4) 0.10(2) Uiso 1 1 d . . . . .
H23 H 0.170(5) 0.042(4) 0.640(3) 0.041(13) Uiso 1 1 d . . . . .
H4 H -0.180(5) 0.255(4) 1.083(3) 0.053(13) Uiso 1 1 d . . . . .
H26 H -0.189(5) 0.269(4) 0.650(2) 0.039(11) Uiso 1 1 d . . . . .
H15 H 0.384(5) 0.857(4) 0.847(2) 0.041(12) Uiso 1 1 d . . . . .
H21B H 0.547(8) 0.292(6) 0.749(3) 0.083(18) Uiso 1 1 d . . . . .
H5 H 0.102(7) 0.305(5) 0.946(3) 0.072(16) Uiso 1 1 d . . . . .
H3 H -0.352(7) 0.350(5) 1.008(3) 0.069(16) Uiso 1 1 d . . . . .
H21C H 0.454(8) 0.177(7) 0.698(4) 0.10(3) Uiso 1 1 d . . . . .
H10 H -0.118(7) 0.707(6) 0.584(4) 0.09(2) Uiso 1 1 d . . . . .
O11 O 0.3672(9) 0.3197(14) 0.9303(6) 0.145(6) Uani 1 1 d . . P . .
H11A H 0.379306 0.376725 0.903000 0.218 Uiso 1 1 d G . P . .
H11B H 0.281901 0.264542 0.905779 0.218 Uiso 1 1 d G . P . .
O12 O -0.389(8) -0.082(4) 0.717(2) 0.16(2) Uani 1 1 d . . . A -1
H12A H -0.478852 -0.083773 0.726236 0.236 Uiso 1 1 d G . . A -1
H12B H -0.329411 -0.011385 0.745660 0.236 Uiso 1 1 d G . . A -1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0232(2) 0.0317(3) 0.0310(3) 0.00640(19) 0.00883(18) 0.00572(18)
Cl1 0.0455(6) 0.0839(9) 0.0506(7) 0.0077(6) 0.0085(5) 0.0174(6)
Cl2 0.0922(10) 0.0714(9) 0.0769(9) 0.0386(8) 0.0339(8) 0.0367(8)
N7 0.0248(14) 0.0377(16) 0.0330(16) 0.0072(13) 0.0112(12) 0.0070(12)
O2 0.0274(12) 0.0345(13) 0.0401(14) 0.0050(11) 0.0092(10) 0.0071(10)
O1 0.0275(12) 0.0418(14) 0.0347(13) 0.0140(11) 0.0112(10) 0.0115(10)
N3 0.0256(13) 0.0326(15) 0.0302(15) 0.0088(12) 0.0110(11) 0.0056(11)
N2 0.0256(14) 0.0442(17) 0.0336(16) 0.0129(14) 0.0141(12) 0.0104(12)
N4 0.0321(15) 0.0375(16) 0.0330(16) 0.0097(13) 0.0117(13) 0.0061(13)
N6 0.0219(13) 0.0384(17) 0.0439(18) 0.0050(14) 0.0078(12) 0.0043(12)
N8 0.0294(15) 0.0341(16) 0.0350(16) 0.0056(13) 0.0073(12) 0.0051(12)
N5 0.0372(17) 0.048(2) 0.0387(19) 0.0049(16) 0.0020(14) 0.0016(15)
N1 0.0469(19) 0.0425(19) 0.0352(18) 0.0115(15) 0.0074(15) 0.0046(15)
C14 0.0302(18) 0.038(2) 0.038(2) 0.0064(16) 0.0092(15) 0.0031(15)
C20 0.0319(18) 0.0366(19) 0.037(2) 0.0075(16) 0.0149(15) 0.0097(15)
C6 0.0273(16) 0.0338(18) 0.0331(19) 0.0084(15) 0.0096(14) 0.0048(14)
C1 0.0330(17) 0.0304(17) 0.0313(18) 0.0054(15) 0.0101(14) 0.0056(14)
C5 0.036(2) 0.043(2) 0.040(2) 0.0121(18) 0.0078(17) 0.0081(17)
C19 0.0293(17) 0.0374(19) 0.0319(19) 0.0079(15) 0.0096(14) 0.0056(14)
C8 0.045(2) 0.063(3) 0.049(2) 0.024(2) 0.0189(19) 0.027(2)
C9 0.0357(18) 0.0346(19) 0.0324(19) 0.0078(15) 0.0116(15) 0.0072(15)
C7 0.0301(17) 0.0372(19) 0.0337(19) 0.0110(16) 0.0088(14) 0.0094(14)
C11 0.072(3) 0.062(3) 0.058(3) 0.034(2) 0.032(3) 0.019(2)
C22 0.0351(18) 0.0338(19) 0.036(2) 0.0049(16) 0.0115(15) 0.0060(15)
C18 0.0355(19) 0.041(2) 0.036(2) 0.0090(17) 0.0056(16) 0.0038(16)
C2 0.040(2) 0.047(2) 0.042(2) 0.0150(19) 0.0154(18) 0.0146(18)
C3 0.051(3) 0.055(3) 0.057(3) 0.019(2) 0.031(2) 0.017(2)
C21 0.038(2) 0.051(3) 0.056(3) 0.006(2) 0.008(2) 0.022(2)
O3 0.099(3) 0.185(6) 0.064(3) 0.039(3) 0.024(2) 0.052(4)
C4 0.053(2) 0.046(2) 0.043(2) 0.014(2) 0.020(2) 0.0096(19)
C13 0.039(2) 0.052(2) 0.044(2) 0.013(2) 0.0204(18) 0.0106(19)
O6 0.081(3) 0.182(6) 0.125(5) 0.044(4) -0.029(3) -0.023(4)
C23 0.048(3) 0.039(2) 0.061(3) 0.005(2) 0.015(2) 0.014(2)
C26 0.034(2) 0.042(2) 0.048(2) 0.0047(19) 0.0048(17) 0.0037(17)
C15 0.039(2) 0.041(2) 0.066(3) 0.007(2) 0.007(2) 0.0081(18)
C12 0.063(3) 0.063(3) 0.053(3) 0.022(2) 0.037(2) 0.012(2)
C25 0.043(2) 0.046(2) 0.061(3) 0.001(2) 0.003(2) -0.0035(19)
C17 0.052(3) 0.046(3) 0.065(3) 0.001(2) -0.002(2) -0.007(2)
C24 0.057(3) 0.036(2) 0.062(3) -0.004(2) 0.009(2) 0.002(2)
C10 0.058(3) 0.055(3) 0.044(2) 0.023(2) 0.020(2) 0.021(2)
O4 0.089(3) 0.190(6) 0.093(3) 0.061(4) 0.046(3) 0.072(4)
O7 0.224(8) 0.107(5) 0.176(7) -0.035(5) -0.018(6) 0.084(5)
C16 0.061(3) 0.037(2) 0.083(4) -0.001(2) 0.003(3) 0.008(2)
O9 0.154(5) 0.161(5) 0.121(4) 0.070(4) 0.041(4) 0.105(5)
O10 0.120(4) 0.176(6) 0.082(3) 0.056(4) 0.026(3) 0.012(4)
O5 0.209(7) 0.100(4) 0.119(5) 0.022(3) 0.012(4) 0.077(4)
O8 0.119(5) 0.232(8) 0.264(10) 0.166(8) 0.103(6) 0.047(5)
O11 0.067(5) 0.242(14) 0.146(9) 0.085(9) 0.030(5) 0.041(6)
O12 0.26(5) 0.11(3) 0.13(3) 0.011(18) 0.13(3) 0.05(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N7 1.856(3) . ?
Co1 O2 1.905(3) . ?
Co1 O1 1.887(3) . ?
Co1 N3 1.853(3) . ?
Co1 N4 1.920(3) . ?
Co1 N8 1.915(3) . ?
Cl1 O3 1.402(5) . ?
Cl1 O6 1.345(5) . ?
Cl1 O4 1.374(5) . ?
Cl1 O5 1.468(6) . ?
Cl2 O7 1.368(6) . ?
Cl2 O9 1.384(5) . ?
Cl2 O10 1.418(5) . ?
Cl2 O8 1.374(6) . ?
N7 N6 1.380(4) . ?
N7 C20 1.284(5) . ?
O2 C19 1.295(4) . ?
O1 C6 1.300(4) . ?
N3 N2 1.377(4) . ?
N3 C7 1.291(5) . ?
N2 H2 0.8600 . ?
N2 C6 1.311(5) . ?
N4 C9 1.358(5) . ?
N4 C13 1.339(5) . ?
N6 H6 0.8600 . ?
N6 C19 1.307(5) . ?
N8 C22 1.363(5) . ?
N8 C26 1.336(5) . ?
N5 C18 1.323(5) . ?
N5 C17 1.342(6) . ?
N1 C5 1.324(5) . ?
N1 C4 1.338(6) . ?
C14 C19 1.486(5) . ?
C14 C18 1.379(5) . ?
C14 C15 1.386(6) . ?
C20 C22 1.466(5) . ?
C20 C21 1.480(6) . ?
C6 C1 1.476(5) . ?
C1 C5 1.395(5) . ?
C1 C2 1.384(5) . ?
C5 H5 0.95(6) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C8 C7 1.478(5) . ?
C9 C7 1.473(5) . ?
C9 C10 1.377(6) . ?
C11 H11 0.9300 . ?
C11 C12 1.371(7) . ?
C11 C10 1.388(7) . ?
C22 C23 1.370(6) . ?
C18 H18 0.94(4) . ?
C2 C3 1.368(6) . ?
C2 H2A 0.76(4) . ?
C3 C4 1.376(7) . ?
C3 H3 0.86(6) . ?
C21 H21A 0.88(7) . ?
C21 H21B 1.02(7) . ?
C21 H21C 0.74(8) . ?
C4 H4 1.01(5) . ?
C13 C12 1.381(6) . ?
C13 H13 0.84(4) . ?
C23 C24 1.387(7) . ?
C23 H23 0.75(5) . ?
C26 C25 1.372(6) . ?
C26 H26 0.88(4) . ?
C15 C16 1.375(7) . ?
C15 H15 0.84(5) . ?
C12 H12 0.9300 . ?
C25 H25 0.9300 . ?
C25 C24 1.359(7) . ?
C17 H17 0.9300 . ?
C17 C16 1.354(7) . ?
C24 H24 0.9300 . ?
C10 H10 0.84(6) . ?
C16 H16 0.92(6) . ?
O11 H11A 0.8501 . ?
O11 H11B 0.8502 . ?
O12 H12A 0.8501 . ?
O12 H12B 0.8501 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N7 Co1 O2 82.93(12) . . ?
N7 Co1 O1 93.01(12) . . ?
N7 Co1 N4 101.36(13) . . ?
N7 Co1 N8 82.50(13) . . ?
O2 Co1 N4 87.59(13) . . ?
O2 Co1 N8 165.37(12) . . ?
O1 Co1 O2 91.33(12) . . ?
O1 Co1 N4 165.34(12) . . ?
O1 Co1 N8 90.75(13) . . ?
N3 Co1 N7 175.12(13) . . ?
N3 Co1 O2 95.12(12) . . ?
N3 Co1 O1 82.56(11) . . ?
N3 Co1 N4 82.98(13) . . ?
N3 Co1 N8 99.51(13) . . ?
N8 Co1 N4 93.98(14) . . ?
O3 Cl1 O5 105.5(4) . . ?
O6 Cl1 O3 116.5(4) . . ?
O6 Cl1 O4 118.6(4) . . ?
O6 Cl1 O5 100.6(4) . . ?
O4 Cl1 O3 111.3(3) . . ?
O4 Cl1 O5 101.4(4) . . ?
O7 Cl2 O9 112.8(4) . . ?
O7 Cl2 O10 105.4(5) . . ?
O7 Cl2 O8 110.5(6) . . ?
O9 Cl2 O10 107.0(4) . . ?
O8 Cl2 O9 111.8(4) . . ?
O8 Cl2 O10 109.0(5) . . ?
N6 N7 Co1 115.9(2) . . ?
C20 N7 Co1 119.5(2) . . ?
C20 N7 N6 124.4(3) . . ?
C19 O2 Co1 107.9(2) . . ?
C6 O1 Co1 109.3(2) . . ?
N2 N3 Co1 116.4(2) . . ?
C7 N3 Co1 119.2(2) . . ?
C7 N3 N2 124.4(3) . . ?
N3 N2 H2 126.4 . . ?
C6 N2 N3 107.2(3) . . ?
C6 N2 H2 126.4 . . ?
C9 N4 Co1 112.1(2) . . ?
C13 N4 Co1 128.0(3) . . ?
C13 N4 C9 119.6(3) . . ?
N7 N6 H6 126.4 . . ?
C19 N6 N7 107.1(3) . . ?
C19 N6 H6 126.4 . . ?
C22 N8 Co1 112.5(2) . . ?
C26 N8 Co1 128.0(3) . . ?
C26 N8 C22 119.5(3) . . ?
C18 N5 C17 121.7(4) . . ?
C5 N1 C4 118.6(4) . . ?
C18 C14 C19 120.7(4) . . ?
C18 C14 C15 118.7(4) . . ?
C15 C14 C19 120.5(4) . . ?
N7 C20 C22 111.1(3) . . ?
N7 C20 C21 124.5(4) . . ?
C22 C20 C21 124.3(4) . . ?
O1 C6 N2 124.5(3) . . ?
O1 C6 C1 116.9(3) . . ?
N2 C6 C1 118.6(3) . . ?
C5 C1 C6 118.9(3) . . ?
C2 C1 C6 123.7(3) . . ?
C2 C1 C5 117.3(4) . . ?
N1 C5 C1 123.3(4) . . ?
N1 C5 H5 118(3) . . ?
C1 C5 H5 118(3) . . ?
O2 C19 N6 126.0(3) . . ?
O2 C19 C14 116.0(3) . . ?
N6 C19 C14 118.1(3) . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
N4 C9 C7 114.5(3) . . ?
N4 C9 C10 121.6(4) . . ?
C10 C9 C7 124.0(4) . . ?
N3 C7 C8 125.1(3) . . ?
N3 C7 C9 111.1(3) . . ?
C9 C7 C8 123.8(3) . . ?
C12 C11 H11 120.2 . . ?
C12 C11 C10 119.5(4) . . ?
C10 C11 H11 120.2 . . ?
N8 C22 C20 114.0(3) . . ?
N8 C22 C23 120.4(4) . . ?
C23 C22 C20 125.5(4) . . ?
N5 C18 C14 120.6(4) . . ?
N5 C18 H18 118(3) . . ?
C14 C18 H18 121(3) . . ?
C1 C2 H2A 119(3) . . ?
C3 C2 C1 119.3(4) . . ?
C3 C2 H2A 122(3) . . ?
C2 C3 C4 119.7(4) . . ?
C2 C3 H3 121(4) . . ?
C4 C3 H3 119(4) . . ?
C20 C21 H21A 112(5) . . ?
C20 C21 H21B 113(3) . . ?
C20 C21 H21C 119(6) . . ?
H21A C21 H21B 86(5) . . ?
H21A C21 H21C 116(7) . . ?
H21B C21 H21C 105(6) . . ?
N1 C4 C3 121.8(4) . . ?
N1 C4 H4 117(3) . . ?
C3 C4 H4 121(3) . . ?
N4 C13 C12 121.1(4) . . ?
N4 C13 H13 115(2) . . ?
C12 C13 H13 123(2) . . ?
C22 C23 C24 119.5(4) . . ?
C22 C23 H23 117(4) . . ?
C24 C23 H23 124(4) . . ?
N8 C26 C25 121.7(4) . . ?
N8 C26 H26 115(3) . . ?
C25 C26 H26 123(3) . . ?
C14 C15 H15 125(3) . . ?
C16 C15 C14 118.5(4) . . ?
C16 C15 H15 117(3) . . ?
C11 C12 C13 119.7(4) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C26 C25 H25 120.2 . . ?
C24 C25 C26 119.6(4) . . ?
C24 C25 H25 120.2 . . ?
N5 C17 H17 120.2 . . ?
N5 C17 C16 119.6(4) . . ?
C16 C17 H17 120.2 . . ?
C23 C24 H24 120.4 . . ?
C25 C24 C23 119.3(4) . . ?
C25 C24 H24 120.4 . . ?
C9 C10 C11 118.5(4) . . ?
C9 C10 H10 126(5) . . ?
C11 C10 H10 114(5) . . ?
C15 C16 H16 120(3) . . ?
C17 C16 C15 120.8(5) . . ?
C17 C16 H16 119(3) . . ?
H11A O11 H11B 104.5 . . ?
H12A O12 H12B 104.5 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C8 H8A N6 0.96 2.67 3.609(6) 165.1 1_455 yes
C8 H8B O3 0.96 2.65 3.374(7) 132.2 2_566 yes
C12 H12 O6 0.93 2.65 3.564(8) 166.6 2_666 yes
C17 H17 N1 0.93 2.70 3.590(6) 161.4 1_665 yes
C17 H17 O10 0.93 2.64 3.102(8) 111.5 1_665 yes
C4 H4 O2 1.01(5) 2.54(5) 3.244(5) 127(3) 2_567 yes
C26 H26 N3 0.88(4) 2.66(4) 3.147(6) 116(3) . yes
C26 H26 O6 0.88(4) 2.50(4) 3.235(8) 141(4) 1_455 yes
C5 H5 O11 0.95(6) 2.41(6) 3.361(10) 174(5) . yes
C3 H3 O11 0.86(6) 2.54(6) 3.160(9) 130(5) 1_455 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 N7 N6 C19 -2.1(4) . . . . ?
Co1 N7 C20 C22 6.4(4) . . . . ?
Co1 N7 C20 C21 -172.7(4) . . . . ?
Co1 O2 C19 N6 -3.8(5) . . . . ?
Co1 O2 C19 C14 174.9(3) . . . . ?
Co1 O1 C6 N2 -2.3(4) . . . . ?
Co1 O1 C6 C1 178.8(2) . . . . ?
Co1 N3 N2 C6 1.8(4) . . . . ?
Co1 N3 C7 C8 -177.2(3) . . . . ?
Co1 N3 C7 C9 0.5(4) . . . . ?
Co1 N4 C9 C7 -3.4(4) . . . . ?
Co1 N4 C9 C10 175.5(3) . . . . ?
Co1 N4 C13 C12 -172.6(3) . . . . ?
Co1 N8 C22 C20 -0.5(4) . . . . ?
Co1 N8 C22 C23 -178.6(3) . . . . ?
Co1 N8 C26 C25 178.1(3) . . . . ?
N7 Co1 O1 C6 -179.6(2) . . . . ?
N7 N6 C19 O2 4.0(5) . . . . ?
N7 N6 C19 C14 -174.6(3) . . . . ?
N7 C20 C22 N8 -3.6(5) . . . . ?
N7 C20 C22 C23 174.4(4) . . . . ?
O2 Co1 N7 N6 0.3(2) . . . . ?
O2 Co1 N7 C20 175.8(3) . . . . ?
O2 Co1 O1 C6 97.4(2) . . . . ?
O2 Co1 N3 N2 -93.1(2) . . . . ?
O2 Co1 N3 C7 85.1(3) . . . . ?
O1 Co1 N7 N6 -90.6(3) . . . . ?
O1 Co1 N7 C20 84.9(3) . . . . ?
O1 Co1 N3 N2 -2.4(2) . . . . ?
O1 Co1 N3 C7 175.7(3) . . . . ?
O1 C6 C1 C5 1.2(5) . . . . ?
O1 C6 C1 C2 -178.7(4) . . . . ?
N3 Co1 O1 C6 2.4(2) . . . . ?
N3 N2 C6 O1 0.4(5) . . . . ?
N3 N2 C6 C1 179.3(3) . . . . ?
N2 N3 C7 C8 0.8(6) . . . . ?
N2 N3 C7 C9 178.5(3) . . . . ?
N2 C6 C1 C5 -177.8(3) . . . . ?
N2 C6 C1 C2 2.4(6) . . . . ?
N4 Co1 N7 N6 86.4(3) . . . . ?
N4 Co1 N7 C20 -98.1(3) . . . . ?
N4 Co1 O1 C6 11.8(6) . . . . ?
N4 Co1 N3 N2 180.0(3) . . . . ?
N4 Co1 N3 C7 -1.9(3) . . . . ?
N4 C9 C7 N3 2.0(5) . . . . ?
N4 C9 C7 C8 179.7(4) . . . . ?
N4 C9 C10 C11 -2.2(7) . . . . ?
N4 C13 C12 C11 -1.3(7) . . . . ?
N6 N7 C20 C22 -178.6(3) . . . . ?
N6 N7 C20 C21 2.4(6) . . . . ?
N8 Co1 N7 N6 179.0(3) . . . . ?
N8 Co1 N7 C20 -5.5(3) . . . . ?
N8 Co1 O1 C6 -97.1(2) . . . . ?
N8 Co1 N3 N2 87.1(3) . . . . ?
N8 Co1 N3 C7 -94.7(3) . . . . ?
N8 C22 C23 C24 0.7(7) . . . . ?
N8 C26 C25 C24 0.0(7) . . . . ?
N5 C17 C16 C15 -1.4(9) . . . . ?
C14 C15 C16 C17 0.4(9) . . . . ?
C20 N7 N6 C19 -177.4(3) . . . . ?
C20 C22 C23 C24 -177.2(4) . . . . ?
C6 C1 C5 N1 177.9(4) . . . . ?
C6 C1 C2 C3 -176.9(4) . . . . ?
C1 C2 C3 C4 -2.0(7) . . . . ?
C5 N1 C4 C3 1.6(6) . . . . ?
C5 C1 C2 C3 3.3(6) . . . . ?
C19 C14 C18 N5 179.1(4) . . . . ?
C19 C14 C15 C16 -178.8(5) . . . . ?
C9 N4 C13 C12 0.2(6) . . . . ?
C7 N3 N2 C6 -176.3(3) . . . . ?
C7 C9 C10 C11 176.5(4) . . . . ?
C22 N8 C26 C25 -1.1(6) . . . . ?
C22 C23 C24 C25 -1.7(8) . . . . ?
C18 N5 C17 C16 1.8(8) . . . . ?
C18 C14 C19 O2 166.9(4) . . . . ?
C18 C14 C19 N6 -14.3(6) . . . . ?
C18 C14 C15 C16 0.3(7) . . . . ?
C2 C1 C5 N1 -2.2(6) . . . . ?
C2 C3 C4 N1 -0.4(7) . . . . ?
C21 C20 C22 N8 175.5(4) . . . . ?
C21 C20 C22 C23 -6.5(7) . . . . ?
C4 N1 C5 C1 -0.2(6) . . . . ?
C13 N4 C9 C7 -177.3(3) . . . . ?
C13 N4 C9 C10 1.6(6) . . . . ?
C26 N8 C22 C20 178.8(4) . . . . ?
C26 N8 C22 C23 0.7(6) . . . . ?
C26 C25 C24 C23 1.4(8) . . . . ?
C15 C14 C19 O2 -14.0(6) . . . . ?
C15 C14 C19 N6 164.7(4) . . . . ?
C15 C14 C18 N5 0.0(6) . . . . ?
C12 C11 C10 C9 1.0(8) . . . . ?
C17 N5 C18 C14 -1.1(7) . . . . ?
C10 C9 C7 N3 -176.8(4) . . . . ?
C10 C9 C7 C8 0.9(6) . . . . ?
C10 C11 C12 C13 0.7(8) . . . . ?
_shelx_res_file
;
TITL MII-C3DS002-Per-Cr3 in P1
mii-c3ds002-per-cr3.res
created by SHELXL-2018/3 at 21:08:56 on 14-Jan-2021
CELL 0.71073 8.88 10.529 18.43 99.407 102.174 100.652
ZERR 2 0.005 0.005 0.005 0.005 0.005 0.005
LATT 1
SFAC C H N O Cl Co
UNIT 48 48 16 20 4 2
EQIV $1 -1+X,+Y,+Z
EQIV $2 -X,1-Y,1-Z
EQIV $3 1-X,1-Y,1-Z
EQIV $4 1+X,1+Y,+Z
EQIV $5 -X,1-Y,2-Z
L.S. 10
PLAN 25
HTAB C8 N6_$1
HTAB C8 O3_$2
HTAB C12 O6_$3
HTAB C17 N1_$4
HTAB C17 O10_$4
HTAB C4 O2_$5
HTAB C26 N3
HTAB C26 O6_$1
HTAB C5 O11
HTAB C3 O11_$1
MPLA N4 N8 O1 O2
MPLA O2 N7 N8 N3
MPLA O1 N7 N4 N3
CONF
MORE -1
BOND $H
HTAB
fmap 2
acta
MERG 2
OMIT -2 -4 9
OMIT -3 3 4
OMIT -4 3 6
OMIT 4 -3 1
OMIT 1 0 8
OMIT 1 4 8
OMIT -2 -4 5
OMIT 4 -7 4
OMIT 0 -1 3
OMIT -1 -1 3
OMIT -2 2 1
OMIT 1 -2 1
OMIT -2 1 1
OMIT 4 -3 13
OMIT 2 0 2
OMIT 3 -3 1
OMIT -5 3 12
OMIT 0 -4 6
OMIT 1 -4 8
OMIT -2 -1 4
REM
REM
REM
WGHT 0.084500 1.655200
FVAR 0.96600 0.71203
CO1 6 0.110853 0.449494 0.743809 11.00000 0.02321 0.03171 =
0.03095 0.00640 0.00883 0.00572
CL1 5 0.438379 0.257794 0.528793 11.00000 0.04547 0.08395 =
0.05061 0.00773 0.00852 0.01738
CL2 5 0.086559 -0.007676 0.833886 11.00000 0.09216 0.07140 =
0.07685 0.03859 0.03388 0.03669
N7 3 0.301707 0.398678 0.750352 11.00000 0.02478 0.03775 =
0.03300 0.00719 0.01125 0.00699
O2 4 0.243756 0.612167 0.803685 11.00000 0.02741 0.03447 =
0.04006 0.00495 0.00923 0.00714
O1 4 0.079361 0.389047 0.831545 11.00000 0.02747 0.04175 =
0.03466 0.01403 0.01120 0.01149
N3 3 -0.076924 0.501012 0.746087 11.00000 0.02558 0.03260 =
0.03022 0.00880 0.01097 0.00564
N2 3 -0.146532 0.469110 0.802739 11.00000 0.02560 0.04423 =
0.03359 0.01294 0.01411 0.01043
AFIX 43
H2 2 -0.234589 0.484835 0.809807 11.00000 -1.20000
AFIX 0
N4 3 0.098780 0.531429 0.657693 11.00000 0.03207 0.03748 =
0.03305 0.00973 0.01172 0.00609
N6 3 0.435142 0.492913 0.791593 11.00000 0.02187 0.03841 =
0.04386 0.00502 0.00783 0.00426
AFIX 43
H6 2 0.530808 0.482919 0.800719 11.00000 -1.20000
AFIX 0
N8 3 0.027813 0.274329 0.683331 11.00000 0.02937 0.03415 =
0.03499 0.00561 0.00730 0.00512
N5 3 0.776499 0.822839 0.916680 11.00000 0.03724 0.04759 =
0.03867 0.00492 0.00203 0.00159
N1 3 -0.027577 0.269489 1.017004 11.00000 0.04692 0.04245 =
0.03524 0.01145 0.00737 0.00465
C14 1 0.512047 0.721502 0.854263 11.00000 0.03015 0.03804 =
0.03776 0.00637 0.00916 0.00307
C20 1 0.301740 0.279042 0.721611 11.00000 0.03188 0.03663 =
0.03698 0.00752 0.01485 0.00973
C6 1 -0.053579 0.410284 0.843917 11.00000 0.02729 0.03376 =
0.03311 0.00837 0.00957 0.00475
C1 1 -0.099696 0.366544 0.909850 11.00000 0.03295 0.03040 =
0.03129 0.00541 0.01009 0.00557
C5 1 0.001349 0.308104 0.955481 11.00000 0.03550 0.04312 =
0.03982 0.01207 0.00780 0.00813
C19 1 0.388827 0.600187 0.814173 11.00000 0.02934 0.03744 =
0.03193 0.00786 0.00962 0.00558
C8 1 -0.275800 0.618613 0.694244 11.00000 0.04539 0.06280 =
0.04864 0.02438 0.01891 0.02667
AFIX 137
H8A 2 -0.337720 0.576668 0.724253 11.00000 -1.50000
H8B 2 -0.336944 0.600838 0.642613 11.00000 -1.50000
H8C 2 -0.246307 0.712313 0.714053 11.00000 -1.50000
AFIX 0
C9 1 -0.027928 0.587232 0.645372 11.00000 0.03568 0.03463 =
0.03238 0.00780 0.01161 0.00721
C7 1 -0.131732 0.566297 0.697035 11.00000 0.03011 0.03723 =
0.03369 0.01102 0.00878 0.00943
C11 1 0.058395 0.677814 0.547217 11.00000 0.07249 0.06231 =
0.05798 0.03412 0.03197 0.01946
AFIX 43
H11 2 0.045358 0.727162 0.509789 11.00000 -1.20000
AFIX 0
C22 1 0.142096 0.204809 0.679571 11.00000 0.03507 0.03384 =
0.03600 0.00491 0.01147 0.00598
C18 1 0.666549 0.714574 0.881886 11.00000 0.03554 0.04132 =
0.03619 0.00896 0.00560 0.00377
C2 1 -0.238907 0.379818 0.929484 11.00000 0.04007 0.04658 =
0.04184 0.01505 0.01542 0.01463
C3 1 -0.267320 0.341962 0.993829 11.00000 0.05085 0.05488 =
0.05654 0.01943 0.03067 0.01660
C21 1 0.443705 0.222582 0.730700 11.00000 0.03766 0.05077 =
0.05577 0.00562 0.00842 0.02154
O3 4 0.417316 0.241219 0.450009 11.00000 0.09855 0.18535 =
0.06403 0.03892 0.02355 0.05185
C4 1 -0.159932 0.287558 1.036699 11.00000 0.05284 0.04631 =
0.04258 0.01380 0.01971 0.00962
C13 1 0.204678 0.548835 0.616050 11.00000 0.03893 0.05227 =
0.04414 0.01320 0.02035 0.01063
O6 4 0.579218 0.330156 0.572075 11.00000 0.08057 0.18161 =
0.12493 0.04365 -0.02871 -0.02292
C23 1 0.104302 0.078386 0.637297 11.00000 0.04764 0.03878 =
0.06118 0.00474 0.01457 0.01375
C26 1 -0.122015 0.217706 0.646105 11.00000 0.03396 0.04192 =
0.04789 0.00469 0.00477 0.00373
C15 1 0.474133 0.844054 0.863633 11.00000 0.03903 0.04080 =
0.06639 0.00654 0.00731 0.00805
C12 1 0.187463 0.623044 0.560883 11.00000 0.06272 0.06346 =
0.05334 0.02228 0.03658 0.01224
AFIX 43
H12 2 0.263077 0.635824 0.533115 11.00000 -1.20000
AFIX 0
C25 1 -0.164067 0.091618 0.602931 11.00000 0.04292 0.04570 =
0.06120 0.00076 0.00297 -0.00351
AFIX 43
H25 2 -0.269145 0.054185 0.577498 11.00000 -1.20000
AFIX 0
C17 1 0.743201 0.942784 0.925363 11.00000 0.05218 0.04607 =
0.06452 0.00085 -0.00182 -0.00730
AFIX 43
H17 2 0.823010 1.017800 0.948761 11.00000 -1.20000
AFIX 0
C24 1 -0.051147 0.021735 0.597565 11.00000 0.05683 0.03594 =
0.06248 -0.00413 0.00929 0.00156
AFIX 43
H24 2 -0.077814 -0.063124 0.567585 11.00000 -1.20000
AFIX 0
C10 1 -0.052658 0.659100 0.589626 11.00000 0.05841 0.05474 =
0.04391 0.02252 0.02005 0.02068
O4 4 0.303609 0.277337 0.549924 11.00000 0.08883 0.18977 =
0.09279 0.06071 0.04552 0.07200
O7 4 0.060323 -0.139329 0.802539 11.00000 0.22440 0.10659 =
0.17639 -0.03483 -0.01764 0.08385
C16 1 0.592583 0.953899 0.899826 11.00000 0.06075 0.03687 =
0.08340 -0.00083 0.00296 0.00757
O9 4 -0.035087 0.048723 0.804110 11.00000 0.15412 0.16126 =
0.12089 0.06967 0.04117 0.10520
O10 4 0.090451 -0.001015 0.911731 11.00000 0.12003 0.17636 =
0.08204 0.05644 0.02568 0.01163
O5 4 0.445852 0.127105 0.545490 11.00000 0.20917 0.10043 =
0.11907 0.02181 0.01172 0.07732
O8 4 0.230267 0.059015 0.827900 11.00000 0.11854 0.23193 =
0.26412 0.16610 0.10256 0.04687
H2A 2 -0.299852 0.402658 0.902547 11.00000 0.03014
H13 2 0.283070 0.515231 0.627573 11.00000 0.01952
H18 2 0.694207 0.632256 0.882032 11.00000 0.04352
H16 2 0.572400 1.036501 0.901629 11.00000 0.06762
H21A 2 0.468678 0.200218 0.774878 11.00000 0.09787
H23 2 0.169711 0.041718 0.639671 11.00000 0.04107
H4 2 -0.179843 0.255411 1.083349 11.00000 0.05271
H26 2 -0.189152 0.268599 0.649956 11.00000 0.03906
H15 2 0.384482 0.856963 0.846882 11.00000 0.04097
H21B 2 0.547358 0.292315 0.748946 11.00000 0.08305
H5 2 0.101679 0.305445 0.945626 11.00000 0.07200
H3 2 -0.351642 0.350479 1.008049 11.00000 0.06854
H21C 2 0.453992 0.177161 0.697921 11.00000 0.10241
H10 2 -0.117932 0.706994 0.583952 11.00000 0.08860
AFIX 6
O11 4 0.367228 0.319714 0.930300 21.00000 0.06686 0.24249 =
0.14555 0.08502 0.03033 0.04055
H11A 2 0.379306 0.376725 0.903000 21.00000 -1.50000
H11B 2 0.281901 0.264542 0.905779 21.00000 -1.50000
AFIX 6
PART -1
O12 4 -0.389061 -0.081773 0.716587 0.23725 0.26051 0.11416 =
0.13004 0.01054 0.12618 0.04748
H12A 2 -0.478852 -0.083773 0.726236 1.02682 -1.50000
H12B 2 -0.329411 -0.011385 0.745660 1.07387 -1.50000
AFIX 0
HKLF 4
REM MII-C3DS002-Per-Cr3 in P1
REM wR2 = 0.1870, GooF = S = 1.081, Restrained GooF = 1.081 for all data
REM R1 = 0.0663 for 5762 Fo > 4sig(Fo) and 0.0917 for all 7648 data
REM 509 parameters refined using 0 restraints
END
WGHT 0.0845 1.6552
REM Instructions for potential hydrogen bonds
HTAB C8 N6_$1
HTAB C8 O3_$2
HTAB C12 O6_$3
HTAB C17 N1_$4
HTAB C17 O10_$4
HTAB C4 O2_$5
HTAB C26 N3
HTAB C26 O6_$1
HTAB C5 O11
HTAB C3 O11_$1
REM Highest difference peak 0.967, deepest hole -0.637, 1-sigma level 0.087
Q1 1 0.4539 0.4154 0.5094 11.00000 0.05 0.97
Q2 1 0.3868 -0.0599 0.5926 11.00000 0.05 0.67
Q3 1 0.0749 -0.2839 0.7430 11.00000 0.05 0.52
Q4 1 0.5569 0.2226 0.5563 11.00000 0.05 0.51
Q5 1 0.1943 0.0468 0.8766 11.00000 0.05 0.50
Q6 1 0.1467 0.1832 0.7408 11.00000 0.05 0.49
Q7 1 0.1087 0.1136 0.8182 11.00000 0.05 0.49
Q8 1 0.2880 0.0660 0.8932 11.00000 0.05 0.43
Q9 1 0.0774 -0.0988 0.8667 11.00000 0.05 0.43
Q10 1 0.5100 0.3579 0.6115 11.00000 0.05 0.41
Q11 1 0.6103 0.3480 0.5683 11.00000 0.05 0.41
Q12 1 0.8804 0.8001 0.9380 11.00000 0.05 0.39
Q13 1 0.4988 0.1810 0.4924 11.00000 0.05 0.39
Q14 1 -0.0473 0.0762 0.7986 11.00000 0.05 0.38
Q15 1 0.1603 -0.0633 0.7665 11.00000 0.05 0.37
Q16 1 0.4209 0.3212 0.5054 11.00000 0.05 0.37
Q17 1 0.0791 0.2406 0.6816 11.00000 0.05 0.36
Q18 1 0.4244 0.1378 0.7482 11.00000 0.05 0.34
Q19 1 0.3134 0.1845 0.5366 11.00000 0.05 0.34
Q20 1 -0.0818 0.5823 0.6675 11.00000 0.05 0.30
Q21 1 0.2477 0.0956 0.8254 11.00000 0.05 0.29
Q22 1 -0.3879 0.1104 0.7677 11.00000 0.05 0.29
Q23 1 0.0069 -0.0221 0.7445 11.00000 0.05 0.27
Q24 1 0.7456 0.8594 0.9365 11.00000 0.05 0.27
Q25 1 0.3636 0.2423 0.7286 11.00000 0.05 0.27
;
_shelx_res_checksum 78946
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11 -2 -15 11.4067 11.7847 3
11 -2 -14 48.3796 18.8464 3
11 -1 5 32.7841 18.1052 2
0 0 0 0.00 0.00 0
TITL MII-C3DS002-Per-Cr3 in P1
REM P1 (#1 in standard setting)
CELL 0.71073 8.879692 10.529010 18.430183 99.4068 102.1744 100.6519
ZERR 7.00 0.000317 0.000484 0.001054 0.0043 0.0038 0.0034
LATT -1
SFAC C H N O
UNIT 77.00 70.00 7.00 7.00
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