#============================================================================== data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 11 _journal_issue 4 _journal_year 2020 _journal_page_first 334 _journal_page_last 341 #============================================================================== data_test3 _audit_creation_date 2020-10-15 _audit_creation_method ; Olex2 1.3-beta (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _shelxl_version_number 2013-4 _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. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common AM10 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C25 H22 Br Cu N2 P' _chemical_formula_sum 'C25 H22 Br Cu N2 P' _chemical_formula_weight 524.86 _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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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' 'P' 'P' 0.1023 0.0942 '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 9.471(10) _cell_length_b 11.043(11) _cell_length_c 13.215(18) _cell_angle_alpha 65.853(18) _cell_angle_beta 69.94(2) _cell_angle_gamma 67.350(14) _cell_volume 1135(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 999 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 22.41 _cell_measurement_theta_min 1.73 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 2.806 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 530 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.2 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_unetI/netI 0.1621 _diffrn_reflns_Laue_measured_fraction_full 0.643 _diffrn_reflns_Laue_measured_fraction_max 0.899 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 4059 _diffrn_reflns_point_group_measured_fraction_full 0.643 _diffrn_reflns_point_group_measured_fraction_max 0.899 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 22.409 _diffrn_reflns_theta_min 1.731 _diffrn_ambient_temperature 296.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.643 _diffrn_measured_fraction_theta_max 0.899 _diffrn_measurement_device_type 'Bruker D8 Venture' _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 1231 _reflns_number_total 2639 _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 1.3-beta (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-beta (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2013/4 (Sheldrick, 2015)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _refine_diff_density_max 0.977 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.129 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 259 _refine_ls_number_reflns 2639 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1688 _refine_ls_R_factor_gt 0.0700 _refine_ls_restrained_S_all 0.945 _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^)+(0.1159P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1685 _refine_ls_wR_factor_ref 0.2207 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C25) = Uanis(N2) = Uanis(C) 3.a Secondary CH2 refined with riding coordinates: C(HA,HB) 3.b Aromatic/amide H refined with riding coordinates: C5(H5), C2(H2), C1(H1), C4(H4), C8(H8), C7(H7), C9(H9), C10(H10), C11(H11), C17(H17), C13(H13), C15(H15), C14(H14), C16(H16), C20(H20), C23(H23), C19(H19), C21(H21), C22(H22), C25(H25) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _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 Br1 Br 0.43015(18) 0.35247(18) -0.00486(13) 0.0669(7) Uani 1 1 d . . . . . Cu2 Cu 0.5025(2) 0.4238(2) 0.12272(15) 0.0640(7) Uani 1 1 d . . . . . P1 P 0.3020(4) 0.4525(4) 0.2665(3) 0.0534(12) Uani 1 1 d . . . . . N1 N 0.7159(14) 0.2869(14) 0.1467(10) 0.063(4) Uani 1 1 d . . . . . C5 C 0.8016(18) 0.2007(19) 0.0896(13) 0.073(5) Uani 1 1 d . . . . . H5 H 0.7540 0.1879 0.0452 0.087 Uiso 1 1 calc R U . . . C2 C 0.9508(17) 0.2402(17) 0.2060(13) 0.064(5) Uani 1 1 d . . . . . H2 H 0.9987 0.2553 0.2488 0.077 Uiso 1 1 calc R U . . . C3 C 1.0342(17) 0.1508(16) 0.1451(13) 0.055(4) Uani 1 1 d . . . . . C1 C 0.795(2) 0.3079(17) 0.2037(13) 0.075(5) Uani 1 1 d . . . . . H1 H 0.7412 0.3714 0.2432 0.090 Uiso 1 1 calc R U . . . C4 C 0.9571(19) 0.1270(17) 0.0897(14) 0.072(5) Uani 1 1 d . . . . . H4 H 1.0079 0.0616 0.0519 0.087 Uiso 1 1 calc R U . . . C6 C 0.3216(15) 0.5239(15) 0.3600(13) 0.050(4) Uani 1 1 d . . . . . C8 C 0.2923(17) 0.5464(19) 0.5409(13) 0.068(5) Uani 1 1 d . . . . . H8 H 0.2680 0.5117 0.6199 0.081 Uiso 1 1 calc R U . . . C7 C 0.2818(16) 0.4804(17) 0.4779(14) 0.061(4) Uani 1 1 d . . . . . H7 H 0.2461 0.4022 0.5157 0.073 Uiso 1 1 calc R U . . . C9 C 0.3380(19) 0.662(2) 0.4880(16) 0.080(5) Uani 1 1 d . . . . . H9 H 0.3416 0.7096 0.5306 0.096 Uiso 1 1 calc R U . . . C10 C 0.3792(17) 0.7104(17) 0.3722(15) 0.077(5) Uani 1 1 d . . . . . H10 H 0.4154 0.7883 0.3368 0.092 Uiso 1 1 calc R U . . . C11 C 0.3679(18) 0.6449(17) 0.3064(13) 0.067(5) Uani 1 1 d . . . . . H11 H 0.3908 0.6814 0.2275 0.081 Uiso 1 1 calc R U . . . C12 C 0.263(2) 0.2913(17) 0.3578(13) 0.063(5) Uani 1 1 d . . . . . C17 C 0.1130(17) 0.2854(18) 0.4314(14) 0.068(5) Uani 1 1 d . . . . . H17 H 0.0325 0.3666 0.4331 0.082 Uiso 1 1 calc R U . . . C13 C 0.3755(18) 0.1700(18) 0.3608(13) 0.069(5) Uani 1 1 d . . . . . H13 H 0.4742 0.1731 0.3143 0.082 Uiso 1 1 calc R U . . . C15 C 0.206(2) 0.041(2) 0.4990(14) 0.083(6) Uani 1 1 d . . . . . H15 H 0.1889 -0.0443 0.5467 0.100 Uiso 1 1 calc R U . . . C14 C 0.355(2) 0.0437(19) 0.4269(16) 0.090(6) Uani 1 1 d . . . . . H14 H 0.4354 -0.0374 0.4246 0.109 Uiso 1 1 calc R U . . . C16 C 0.088(2) 0.158(2) 0.5003(15) 0.087(6) Uani 1 1 d . . . . . H16 H -0.0102 0.1535 0.5474 0.105 Uiso 1 1 calc R U . . . C20 C -0.0847(19) 0.609(2) 0.1344(14) 0.076(6) Uani 1 1 d . . . . . H20 H -0.1242 0.5854 0.0917 0.092 Uiso 1 1 calc R U . . . C18 C 0.1142(18) 0.5621(18) 0.2316(13) 0.063(5) Uani 1 1 d . . . . . C23 C 0.0183(19) 0.6695(19) 0.2752(14) 0.078(6) Uani 1 1 d . . . . . H23 H 0.0491 0.6891 0.3251 0.093 Uiso 1 1 calc R U . . . C19 C 0.0648(18) 0.5314(18) 0.1583(14) 0.076(5) Uani 1 1 d . . . . . H19 H 0.1289 0.4620 0.1264 0.091 Uiso 1 1 calc R U . . . C21 C -0.168(2) 0.715(2) 0.1727(18) 0.092(7) Uani 1 1 d . . . . . H21 H -0.2623 0.7694 0.1504 0.110 Uiso 1 1 calc R U . . . C22 C -0.122(2) 0.746(2) 0.2437(16) 0.103(7) Uani 1 1 d . . . . . H22 H -0.1863 0.8200 0.2708 0.124 Uiso 1 1 calc R U . . . C25 C 1.2047(16) 0.0891(15) 0.1376(13) 0.065(3) Uani 1 1 d . . . . . H25 H 1.2498 0.0980 0.1856 0.077 Uiso 1 1 calc R U . . . N2 N 1.2906(13) 0.0249(13) 0.0684(10) 0.065(3) Uani 1 1 d . . . . . C C 1.4573(15) -0.0215(16) 0.0600(11) 0.065(3) Uani 1 1 d . . . . . HA H 1.4909 -0.1216 0.0919 0.077 Uiso 1 1 calc R U . . . HB H 1.4821 0.0171 0.1037 0.077 Uiso 1 1 calc R U . . . 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 Br1 0.0562(11) 0.0870(14) 0.0693(12) -0.0320(10) -0.0052(8) -0.0325(10) Cu2 0.0426(12) 0.0861(17) 0.0654(14) -0.0316(12) -0.0024(9) -0.0209(11) P1 0.036(2) 0.070(3) 0.058(3) -0.024(2) -0.0058(19) -0.020(2) N1 0.048(8) 0.090(11) 0.044(8) -0.023(8) 0.010(7) -0.029(8) C5 0.036(10) 0.131(17) 0.061(11) -0.051(12) 0.015(8) -0.035(11) C2 0.037(10) 0.095(14) 0.086(12) -0.062(11) -0.011(9) -0.011(10) C3 0.055(10) 0.068(12) 0.059(10) -0.021(9) -0.010(8) -0.034(10) C1 0.084(14) 0.089(14) 0.067(12) -0.033(10) -0.013(10) -0.035(12) C4 0.057(12) 0.067(12) 0.106(14) -0.045(11) -0.011(10) -0.019(10) C6 0.029(8) 0.052(11) 0.063(12) -0.017(9) -0.003(7) -0.012(8) C8 0.055(11) 0.099(16) 0.048(11) -0.038(12) 0.007(8) -0.023(11) C7 0.046(10) 0.090(14) 0.055(12) -0.029(10) 0.002(8) -0.032(9) C9 0.076(13) 0.101(17) 0.080(15) -0.050(13) -0.013(11) -0.025(12) C10 0.068(12) 0.096(15) 0.063(13) -0.027(12) 0.009(9) -0.039(11) C11 0.084(12) 0.075(14) 0.052(11) -0.023(10) -0.020(9) -0.025(11) C12 0.075(13) 0.059(13) 0.075(12) -0.038(10) -0.034(10) -0.006(11) C17 0.037(10) 0.070(14) 0.089(13) -0.029(11) -0.001(9) -0.013(9) C13 0.053(11) 0.055(13) 0.082(13) -0.015(11) -0.001(9) -0.019(11) C15 0.097(15) 0.077(16) 0.083(14) -0.026(12) 0.006(12) -0.053(14) C14 0.063(13) 0.066(14) 0.111(16) -0.014(12) -0.005(11) -0.013(11) C16 0.076(14) 0.078(15) 0.100(15) -0.025(13) -0.003(11) -0.032(13) C20 0.031(11) 0.121(17) 0.078(13) -0.028(12) -0.013(9) -0.026(11) C18 0.047(10) 0.089(14) 0.053(11) -0.030(10) 0.007(8) -0.028(10) C23 0.036(10) 0.106(16) 0.072(12) -0.023(12) -0.007(9) -0.011(11) C19 0.050(12) 0.105(15) 0.079(12) -0.029(11) -0.003(9) -0.040(11) C21 0.042(12) 0.093(18) 0.093(17) -0.004(13) -0.018(11) 0.005(12) C22 0.090(18) 0.117(19) 0.076(15) -0.021(13) -0.015(12) -0.016(15) C25 0.038(5) 0.077(7) 0.071(6) -0.022(5) -0.006(4) -0.015(5) N2 0.038(5) 0.077(7) 0.071(6) -0.022(5) -0.006(4) -0.015(5) C 0.038(5) 0.077(7) 0.071(6) -0.022(5) -0.006(4) -0.015(5) _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 Br1 Cu2 2.495(3) . ? Br1 Cu2 2.514(3) 2_665 ? Cu2 Br1 2.514(3) 2_665 ? Cu2 Cu2 2.989(5) 2_665 ? Cu2 P1 2.207(5) . ? Cu2 N1 2.041(12) . ? P1 C6 1.802(15) . ? P1 C12 1.790(16) . ? P1 C18 1.814(16) . ? N1 C5 1.306(17) . ? N1 C1 1.360(17) . ? C5 H5 0.9300 . ? C5 C4 1.381(19) . ? C2 H2 0.9300 . ? C2 C3 1.363(18) . ? C2 C1 1.378(19) . ? C3 C4 1.347(19) . ? C3 C25 1.476(18) . ? C1 H1 0.9300 . ? C4 H4 0.9300 . ? C6 C7 1.388(18) . ? C6 C11 1.394(18) . ? C8 H8 0.9300 . ? C8 C7 1.357(19) . ? C8 C9 1.34(2) . ? C7 H7 0.9300 . ? C9 H9 0.9300 . ? C9 C10 1.36(2) . ? C10 H10 0.9300 . ? C10 C11 1.39(2) . ? C11 H11 0.9300 . ? C12 C17 1.429(19) . ? C12 C13 1.347(18) . ? C17 H17 0.9300 . ? C17 C16 1.39(2) . ? C13 H13 0.9300 . ? C13 C14 1.358(19) . ? C15 H15 0.9300 . ? C15 C14 1.41(2) . ? C15 C16 1.35(2) . ? C14 H14 0.9300 . ? C16 H16 0.9300 . ? C20 H20 0.9300 . ? C20 C19 1.41(2) . ? C20 C21 1.32(2) . ? C18 C23 1.39(2) . ? C18 C19 1.41(2) . ? C23 H23 0.9300 . ? C23 C22 1.38(2) . ? C19 H19 0.9300 . ? C21 H21 0.9300 . ? C21 C22 1.36(2) . ? C22 H22 0.9300 . ? C25 H25 0.9300 . ? C25 N2 1.257(16) . ? N2 C 1.439(16) . ? C C 1.48(2) 2_855 ? C HA 0.9700 . ? C HB 0.9700 . ? 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 Cu2 Br1 Cu2 73.25(11) . 2_665 ? Br1 Cu2 Br1 106.75(11) . 2_665 ? Br1 Cu2 Cu2 53.08(7) 2_665 2_665 ? Br1 Cu2 Cu2 53.67(10) . 2_665 ? P1 Cu2 Br1 109.53(15) . . ? P1 Cu2 Br1 110.78(14) . 2_665 ? P1 Cu2 Cu2 125.28(16) . 2_665 ? N1 Cu2 Br1 104.1(4) . . ? N1 Cu2 Br1 102.5(3) . 2_665 ? N1 Cu2 Cu2 112.7(3) . 2_665 ? N1 Cu2 P1 122.0(4) . . ? C6 P1 Cu2 116.6(5) . . ? C6 P1 C18 102.7(7) . . ? C12 P1 Cu2 111.2(6) . . ? C12 P1 C6 104.6(7) . . ? C12 P1 C18 103.4(7) . . ? C18 P1 Cu2 116.8(5) . . ? C5 N1 Cu2 125.2(12) . . ? C5 N1 C1 114.3(14) . . ? C1 N1 Cu2 118.3(12) . . ? N1 C5 H5 117.3 . . ? N1 C5 C4 125.4(16) . . ? C4 C5 H5 117.3 . . ? C3 C2 H2 120.2 . . ? C3 C2 C1 119.5(14) . . ? C1 C2 H2 120.2 . . ? C2 C3 C25 119.7(14) . . ? C4 C3 C2 117.8(15) . . ? C4 C3 C25 122.4(16) . . ? N1 C1 C2 123.4(16) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C5 C4 H4 120.4 . . ? C3 C4 C5 119.2(16) . . ? C3 C4 H4 120.4 . . ? C7 C6 P1 127.6(12) . . ? C7 C6 C11 116.7(14) . . ? C11 C6 P1 115.4(12) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C9 C8 C7 119.2(15) . . ? C6 C7 H7 118.4 . . ? C8 C7 C6 123.2(15) . . ? C8 C7 H7 118.4 . . ? C8 C9 H9 119.7 . . ? C8 C9 C10 120.6(17) . . ? C10 C9 H9 119.7 . . ? C9 C10 H10 119.5 . . ? C9 C10 C11 120.9(16) . . ? C11 C10 H10 119.5 . . ? C6 C11 H11 120.4 . . ? C10 C11 C6 119.2(14) . . ? C10 C11 H11 120.4 . . ? C17 C12 P1 121.7(14) . . ? C13 C12 P1 121.1(14) . . ? C13 C12 C17 117.2(15) . . ? C12 C17 H17 120.1 . . ? C16 C17 C12 119.8(15) . . ? C16 C17 H17 120.1 . . ? C12 C13 H13 117.7 . . ? C12 C13 C14 124.6(15) . . ? C14 C13 H13 117.7 . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C16 C15 C14 121.4(17) . . ? C13 C14 C15 117.2(16) . . ? C13 C14 H14 121.4 . . ? C15 C14 H14 121.4 . . ? C17 C16 H16 120.1 . . ? C15 C16 C17 119.8(16) . . ? C15 C16 H16 120.1 . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C21 C20 C19 119.9(18) . . ? C23 C18 P1 123.8(13) . . ? C23 C18 C19 119.8(15) . . ? C19 C18 P1 116.4(14) . . ? C18 C23 H23 120.3 . . ? C22 C23 C18 119.4(18) . . ? C22 C23 H23 120.3 . . ? C20 C19 H19 120.9 . . ? C18 C19 C20 118.2(16) . . ? C18 C19 H19 120.9 . . ? C20 C21 H21 118.7 . . ? C20 C21 C22 122.6(18) . . ? C22 C21 H21 118.7 . . ? C23 C22 H22 120.1 . . ? C21 C22 C23 120(2) . . ? C21 C22 H22 120.1 . . ? C3 C25 H25 119.0 . . ? N2 C25 C3 122.0(15) . . ? N2 C25 H25 119.0 . . ? C25 N2 C 118.2(13) . . ? N2 C C 110.8(15) . 2_855 ? N2 C HA 109.5 . . ? N2 C HB 109.5 . . ? C C HA 109.5 2_855 . ? C C HB 109.5 2_855 . ? HA C HB 108.1 . . ? 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 Cu2 P1 C6 C7 -136.1(11) . . . . ? Cu2 P1 C6 C11 50.7(12) . . . . ? Cu2 P1 C12 C17 -157.8(11) . . . . ? Cu2 P1 C12 C13 23.0(14) . . . . ? Cu2 P1 C18 C23 -130.4(12) . . . . ? Cu2 P1 C18 C19 51.2(13) . . . . ? Cu2 N1 C5 C4 167.0(12) . . . . ? Cu2 N1 C1 C2 -166.9(12) . . . . ? P1 C6 C7 C8 -175.9(12) . . . . ? P1 C6 C11 C10 177.2(12) . . . . ? P1 C12 C17 C16 179.7(12) . . . . ? P1 C12 C13 C14 -179.4(14) . . . . ? P1 C18 C23 C22 -179.7(13) . . . . ? P1 C18 C19 C20 176.3(11) . . . . ? N1 C5 C4 C3 -5(3) . . . . ? C5 N1 C1 C2 -3(2) . . . . ? C2 C3 C4 C5 5(2) . . . . ? C2 C3 C25 N2 -168.2(15) . . . . ? C3 C2 C1 N1 3(2) . . . . ? C3 C25 N2 C 174.7(12) . . . . ? C1 N1 C5 C4 4(2) . . . . ? C1 C2 C3 C4 -4(2) . . . . ? C1 C2 C3 C25 173.7(14) . . . . ? C4 C3 C25 N2 9(2) . . . . ? C6 P1 C12 C17 75.5(13) . . . . ? C6 P1 C12 C13 -103.7(13) . . . . ? C6 P1 C18 C23 -1.6(15) . . . . ? C6 P1 C18 C19 -179.9(12) . . . . ? C8 C9 C10 C11 3(3) . . . . ? C7 C6 C11 C10 3(2) . . . . ? C7 C8 C9 C10 -2(3) . . . . ? C9 C8 C7 C6 2(2) . . . . ? C9 C10 C11 C6 -3(2) . . . . ? C11 C6 C7 C8 -3(2) . . . . ? C12 P1 C6 C7 -12.8(14) . . . . ? C12 P1 C6 C11 174.0(11) . . . . ? C12 P1 C18 C23 107.0(14) . . . . ? C12 P1 C18 C19 -71.3(13) . . . . ? C12 C17 C16 C15 1(3) . . . . ? C12 C13 C14 C15 -2(3) . . . . ? C17 C12 C13 C14 1(2) . . . . ? C13 C12 C17 C16 -1(2) . . . . ? C14 C15 C16 C17 -1(3) . . . . ? C16 C15 C14 C13 2(3) . . . . ? C20 C21 C22 C23 2(3) . . . . ? C18 P1 C6 C7 94.9(13) . . . . ? C18 P1 C6 C11 -78.3(12) . . . . ? C18 P1 C12 C17 -31.7(14) . . . . ? C18 P1 C12 C13 149.1(13) . . . . ? C18 C23 C22 C21 2(3) . . . . ? C23 C18 C19 C20 -2(2) . . . . ? C19 C20 C21 C22 -6(3) . . . . ? C19 C18 C23 C22 -1(2) . . . . ? C21 C20 C19 C18 6(2) . . . . ? C25 C3 C4 C5 -172.4(14) . . . . ? C25 N2 C C -129.4(18) . . . 2_855 ? _shelx_res_file ; TITL test3 in P-1 CELL 0.71073 9.4711 11.0435 13.2147 65.853 69.941 67.35 ZERR 2 0.0098 0.0114 0.018 0.018 0.021 0.014 LATT 1 SFAC C H Br Cu N P UNIT 50 44 2 2 4 2 EADP C25 N2 C L.S. 20 PLAN 4 TEMP 23 CONF BOND MORE -1 BOND $H fmap 2 ACTA REM REM REM WGHT 0.115900 FVAR 0.16315 BR1 3 0.430155 0.352467 -0.004861 11.00000 0.05624 0.08699 = 0.06929 -0.03203 -0.00518 -0.03246 CU2 4 0.502450 0.423809 0.122721 11.00000 0.04262 0.08609 = 0.06536 -0.03158 -0.00244 -0.02092 P1 6 0.302043 0.452466 0.266533 11.00000 0.03633 0.07039 = 0.05830 -0.02400 -0.00584 -0.02039 N1 5 0.715874 0.286900 0.146680 11.00000 0.04754 0.09017 = 0.04393 -0.02337 0.01031 -0.02880 C5 1 0.801628 0.200702 0.089600 11.00000 0.03645 0.13050 = 0.06111 -0.05052 0.01504 -0.03486 AFIX 43 H5 2 0.754038 0.187922 0.045229 11.00000 -1.20000 AFIX 0 C2 1 0.950811 0.240179 0.206022 11.00000 0.03677 0.09522 = 0.08589 -0.06238 -0.01105 -0.01139 AFIX 43 H2 2 0.998668 0.255276 0.248849 11.00000 -1.20000 AFIX 0 C3 1 1.034245 0.150850 0.145087 11.00000 0.05488 0.06757 = 0.05896 -0.02106 -0.01015 -0.03401 C1 1 0.795035 0.307941 0.203691 11.00000 0.08436 0.08919 = 0.06677 -0.03339 -0.01335 -0.03508 AFIX 43 H1 2 0.741244 0.371393 0.243191 11.00000 -1.20000 AFIX 0 C4 1 0.957110 0.126951 0.089656 11.00000 0.05746 0.06692 = 0.10561 -0.04475 -0.01058 -0.01905 AFIX 43 H4 2 1.007916 0.061571 0.051861 11.00000 -1.20000 AFIX 0 C6 1 0.321600 0.523914 0.359967 11.00000 0.02917 0.05199 = 0.06333 -0.01711 -0.00342 -0.01245 C8 1 0.292260 0.546360 0.540883 11.00000 0.05539 0.09932 = 0.04840 -0.03805 0.00665 -0.02267 AFIX 43 H8 2 0.267996 0.511704 0.619859 11.00000 -1.20000 AFIX 0 C7 1 0.281755 0.480397 0.477940 11.00000 0.04619 0.08994 = 0.05505 -0.02921 0.00177 -0.03208 AFIX 43 H7 2 0.246119 0.402208 0.515675 11.00000 -1.20000 AFIX 0 C9 1 0.337973 0.661956 0.487983 11.00000 0.07561 0.10114 = 0.08027 -0.05005 -0.01332 -0.02463 AFIX 43 H9 2 0.341640 0.709643 0.530554 11.00000 -1.20000 AFIX 0 C10 1 0.379216 0.710376 0.372166 11.00000 0.06833 0.09617 = 0.06267 -0.02661 0.00930 -0.03939 AFIX 43 H10 2 0.415441 0.788292 0.336807 11.00000 -1.20000 AFIX 0 C11 1 0.367851 0.644929 0.306368 11.00000 0.08428 0.07528 = 0.05157 -0.02320 -0.02034 -0.02464 AFIX 43 H11 2 0.390825 0.681404 0.227472 11.00000 -1.20000 AFIX 0 C12 1 0.263106 0.291268 0.357766 11.00000 0.07503 0.05945 = 0.07458 -0.03794 -0.03427 -0.00642 C17 1 0.113042 0.285373 0.431373 11.00000 0.03692 0.07008 = 0.08928 -0.02921 -0.00138 -0.01289 AFIX 43 H17 2 0.032512 0.366617 0.433073 11.00000 -1.20000 AFIX 0 C13 1 0.375494 0.170020 0.360781 11.00000 0.05324 0.05460 = 0.08232 -0.01469 -0.00117 -0.01899 AFIX 43 H13 2 0.474162 0.173058 0.314344 11.00000 -1.20000 AFIX 0 C15 1 0.206070 0.040539 0.498970 11.00000 0.09668 0.07704 = 0.08272 -0.02576 0.00553 -0.05301 AFIX 43 H15 2 0.188915 -0.044271 0.546674 11.00000 -1.20000 AFIX 0 C14 1 0.354787 0.043676 0.426882 11.00000 0.06312 0.06553 = 0.11088 -0.01417 -0.00550 -0.01290 AFIX 43 H14 2 0.435434 -0.037360 0.424632 11.00000 -1.20000 AFIX 0 C16 1 0.087827 0.157972 0.500349 11.00000 0.07586 0.07766 = 0.10026 -0.02528 -0.00269 -0.03184 AFIX 43 H16 2 -0.010207 0.153532 0.547360 11.00000 -1.20000 AFIX 0 C20 1 -0.084664 0.608792 0.134381 11.00000 0.03080 0.12085 = 0.07774 -0.02767 -0.01291 -0.02555 AFIX 43 H20 2 -0.124234 0.585380 0.091674 11.00000 -1.20000 AFIX 0 C18 1 0.114202 0.562148 0.231632 11.00000 0.04712 0.08947 = 0.05337 -0.02971 0.00705 -0.02845 C23 1 0.018350 0.669484 0.275186 11.00000 0.03643 0.10608 = 0.07243 -0.02337 -0.00744 -0.01079 AFIX 43 H23 2 0.049113 0.689112 0.325122 11.00000 -1.20000 AFIX 0 C19 1 0.064782 0.531426 0.158308 11.00000 0.04979 0.10530 = 0.07912 -0.02885 -0.00300 -0.03970 AFIX 43 H19 2 0.128916 0.461954 0.126437 11.00000 -1.20000 AFIX 0 C21 1 -0.168365 0.714518 0.172680 11.00000 0.04167 0.09324 = 0.09297 -0.00383 -0.01823 0.00526 AFIX 43 H21 2 -0.262334 0.769436 0.150359 11.00000 -1.20000 AFIX 0 C22 1 -0.122493 0.746424 0.243709 11.00000 0.09032 0.11655 = 0.07560 -0.02083 -0.01508 -0.01572 AFIX 43 H22 2 -0.186294 0.820013 0.270779 11.00000 -1.20000 AFIX 0 C25 1 1.204677 0.089122 0.137627 11.00000 0.03758 0.07695 = 0.07086 -0.02189 -0.00577 -0.01520 AFIX 43 H25 2 1.249841 0.098041 0.185636 11.00000 -1.20000 AFIX 0 N2 5 1.290608 0.024874 0.068357 11.00000 0.03758 0.07695 = 0.07086 -0.02189 -0.00577 -0.01520 C 1 1.457309 -0.021512 0.060040 11.00000 0.03758 0.07695 = 0.07086 -0.02189 -0.00577 -0.01520 AFIX 23 HA 2 1.490937 -0.121617 0.091930 11.00000 -1.20000 HB 2 1.482116 0.017105 0.103677 11.00000 -1.20000 AFIX 0 HKLF 4 REM test3 in P-1 REM R1 = 0.0700 for 1231 Fo > 4sig(Fo) and 0.1688 for all 2639 data REM 259 parameters refined using 0 restraints END WGHT 0.1158 0.0000 REM Highest difference peak 0.977, deepest hole -0.576, 1-sigma level 0.129 Q1 1 0.4670 0.2190 0.0381 11.00000 0.05 0.98 Q2 1 0.4771 0.5466 0.0867 11.00000 0.05 0.88 Q3 1 0.3914 0.4749 -0.0350 11.00000 0.05 0.81 Q4 1 0.4531 0.3071 -0.0946 11.00000 0.05 0.71 ; _shelx_res_checksum 34233 _shelx_hkl_file ; 1 0 0 205.06 8.11 -1 0 0 209.75 8.11 -1 0 0 212.75 8.70 -2 0 0 44.75 2.33 2 0 0 49.16 2.23 3 0 0 0.31 0.40 3 0 0 0.52 0.92 4 0 0 47.93 2.82 5 0 0 28.46 2.44 5 0 0 40.15 2.71 6 0 0 -2.17 2.12 6 0 0 1.55 2.06 7 0 0 0.45 2.53 7 0 0 -0.95 2.47 8 0 0 -1.34 3.10 8 0 0 0.40 2.93 9 0 0 -1.08 3.79 9 1 1 -4.77 2.85 8 1 1 0.41 3.02 8 1 1 0.88 2.83 7 1 1 9.85 2.89 7 1 1 12.09 2.69 6 1 1 -2.67 1.74 6 1 1 0.31 2.13 5 1 1 3.70 1.51 5 1 1 -1.59 1.89 4 1 1 26.98 2.21 4 1 1 27.51 1.88 3 1 1 17.02 1.54 3 1 1 18.48 1.29 2 1 1 3.70 0.60 -2 -1 -1 4.22 0.59 2 1 1 3.13 0.87 1 1 1 220.80 9.31 -1 -1 -1 225.37 9.30 0 1 1 128.01 5.13 0 -1 -1 134.91 5.16 -1 1 1 63.67 2.72 1 -1 -1 59.76 2.74 2 -1 -1 361.17 14.92 2 -1 -1 341.98 14.09 -2 1 1 375.95 14.91 3 -1 -1 234.93 9.97 3 -1 -1 229.43 9.56 4 -1 -1 212.59 9.53 4 -1 -1 235.98 9.92 5 -1 -1 19.71 2.45 5 -1 -1 21.13 2.63 6 -1 -1 -0.52 1.99 6 -1 -1 -2.10 2.23 7 -1 -1 2.69 2.90 8 -1 -1 -4.81 3.39 9 2 2 10.47 3.80 8 2 2 34.25 4.25 8 2 2 31.60 3.47 7 2 2 19.42 2.73 7 2 2 17.17 3.27 6 2 2 27.73 2.87 6 2 2 31.42 2.43 5 2 2 1.03 1.36 5 2 2 1.05 1.76 4 2 2 8.44 1.75 4 2 2 8.60 1.22 3 2 2 38.34 1.85 3 2 2 35.73 2.34 -3 -2 -2 36.26 1.82 2 2 2 11.64 1.21 1 2 2 423.17 17.41 1 2 2 436.61 16.22 1 2 2 408.36 16.17 0 -2 -2 25.64 1.42 0 2 2 23.83 1.35 1 -2 -2 23.59 1.53 2 -2 -2 59.97 3.11 3 -2 -2 130.30 5.90 3 -2 -2 123.51 5.71 4 -2 -2 91.14 4.82 4 -2 -2 91.78 4.55 5 -2 -2 21.08 2.18 5 -2 -2 22.36 2.61 6 -2 -2 19.31 3.33 7 -2 -2 9.63 3.56 8 -2 -2 8.00 4.21 9 3 3 26.35 4.35 8 3 3 28.79 4.17 7 3 3 40.29 3.71 7 3 3 41.41 3.06 6 3 3 19.70 2.12 6 3 3 24.42 3.10 5 3 3 13.01 2.24 5 3 3 11.46 1.56 4 3 3 4.48 0.95 -4 -3 -3 2.80 0.82 4 3 3 5.54 1.68 3 3 3 -0.43 1.26 2 3 3 45.54 2.45 2 3 3 41.73 1.98 -1 -3 -3 15.62 1.03 -1 -3 -3 14.61 1.20 -1 -3 -3 11.90 1.23 0 -3 -3 18.41 1.49 1 -3 -3 8.21 1.41 2 -3 -3 -0.58 1.35 3 -3 -3 5.51 1.78 4 -3 -3 9.12 2.36 5 -3 -3 6.82 2.64 6 -3 -3 47.52 4.32 7 -3 -3 22.51 4.47 9 4 4 1.04 3.49 8 4 4 -1.28 3.15 7 4 4 27.01 3.64 6 4 4 35.80 3.25 6 4 4 27.47 2.25 5 4 4 62.59 4.05 4 4 4 58.48 3.72 3 4 4 71.44 3.88 3 4 4 70.91 3.13 2 4 4 2.87 0.91 -1 -4 -4 23.61 1.66 -1 -4 -4 23.58 1.67 0 -4 -4 1.78 1.30 1 -4 -4 20.87 2.43 2 -4 -4 3.20 1.75 3 -4 -4 3.30 2.22 4 -4 -4 -2.69 2.23 5 -4 -4 -0.62 2.93 6 -4 -4 5.05 3.75 9 5 5 0.50 3.47 8 5 5 23.49 3.96 7 5 5 -0.86 2.52 6 5 5 10.74 2.75 5 5 5 17.31 2.74 4 5 5 18.67 2.49 3 5 5 4.25 1.14 -2 -5 -5 9.86 1.86 2 5 5 12.24 1.53 -1 -5 -5 31.89 2.17 -1 -5 -5 32.69 2.30 0 -5 -5 31.86 2.70 1 -5 -5 0.90 2.16 2 -5 -5 28.10 3.63 3 -5 -5 13.10 3.20 4 -5 -5 -3.07 2.88 5 -5 -5 -3.88 3.51 8 6 6 3.82 3.25 7 6 6 -0.37 2.72 6 6 6 2.47 2.66 4 6 6 -0.55 1.29 -3 -6 -6 15.70 2.23 3 6 6 12.84 1.48 2 6 6 29.53 2.26 -2 -6 -6 29.87 2.33 -1 -6 -6 19.52 2.24 0 -6 -6 -0.12 2.30 1 -6 -6 -0.38 2.46 2 -6 -6 -3.32 2.52 3 -6 -6 -1.70 3.08 4 -6 -6 -1.41 3.64 -5 -7 -7 41.19 3.57 4 7 7 22.28 2.17 -4 -7 -7 25.43 2.73 -3 -7 -7 2.34 1.92 3 7 7 0.16 1.58 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