# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 182/1074 data_c103 _audit_author_name 'Mayer, P.' _audit_block_code 'Co_BNP_SCN_c103_janiak' _audit_creation_method 'form98_1/compatible with shelxl97-2' _audit_creation_date 02-Sep-98 _chemical_name_systematic ;Di-(2,2'-bis(1,6-naphthyridine))-dithiocyanato-cobalt(II) ; _chemical_compound_source 'crystal provided by C. Janiak, Uni FR' _chemical_name_common 'Co-BNP-KSCN, Nr. 2943' _chemical_formula_moiety '2(C16 N4 H10), 2(S C N), Co' _chemical_formula_sum 'C34 H20 Co N10 S2' _chemical_formula_weight 691.655 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Co' 'Co' .3494 .9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m c a' _symmetry_Int_Tables_number 64 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' 'x, -y+1/2, z+1/2' 'x, y+1/2, -z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, -z' 'x+1/2, -y+1, z+1/2' 'x+1/2, y+1, -z+1/2' '-x, -y, -z' '-x, y, z' '-x, y-1/2, -z-1/2' '-x, -y-1/2, z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, z' '-x+1/2, y, -z-1/2' '-x+1/2, -y, z-1/2' _cell_length_a 21.4385(17) _cell_length_b 15.9180(10) _cell_length_c 8.3683(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2855.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 27.9 _cell_special_details 'Orthorhombic C (as derived from metrics)' _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.60871(17) _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 0.795 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8958 _exptl_absorpt_correction_T_max 0.9657 _exptl_absorpt_process_details 'XRed, Stoe (Darmstadt, Germany)' _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 1 0 0.029 1 -1 0 0.033 1 1 0 0.075 -1 -1 0 0.030 2 0 1 0.262 1 2 -1 0.219 -1 -2 1 0.226 -2 -1 -1 0.236 _diffrn_ambient_temperature 200(2) _diffr_source_type 'Spellman DF4 Series' _diffr_source_power 2.00_kW _diffr_source_voltage 50_kV _diffr_source_current 40_mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation '0.8 mm collimator' _diffrn_measurement_device 'image-plate area detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'area detection' _diffrn_detector_area_resol_mean ? _kl_diffrn_detector_area_phi_start 0.0 _kl_diffrn_detector_area_phi_end 118.0 _kl_diffrn_detector_area_phi_incr 1.0 _kl_diffrn_detector_area_expos_time 8.00_min _kl_diffrn_detector_area_plate_dist 60.0_mm _kl_diffrn_detector_area_eff_mos_spread 0.008 _kl_diffrn_detector_area_profile_funct dynamic _kl_diffrn_detector_area_profile_min 9 _kl_diffrn_detector_area_profile_max 21 _diffrn_special_details ;little formation of ice, no crystal decay in terms of mean intensity per frame ; _diffrn_reflns_number 7660 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.93 _diffrn_measured_fraction_theta_max .961 _diffrn_reflns_theta_full 27.93 _diffrn_measured_fraction_theta_full .961 _refine_diff_density_max .643 _refine_diff_density_min -.414 _refine_diff_density_rms .077 _reflns_number_total 1698 _reflns_number_gt 1334 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Stoe IPDS software (Darmstadt, Germany)' _computing_cell_refinement 'Stoe IPDS software (Darmstadt, Germany)' _computing_data_reduction 'Stoe IPDS software (Darmstadt, Germany)' _computing_structure_solution 'SHELXS-97 (G. M. Sheldrick. University of G\"ottingen, Germany, 1997)' _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ;ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations, Oak Ridge National Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), Germany, 1995). ; _computing_publication_material ;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1698 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0785 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_restrained_S_all 0.948 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_special_details ? 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.5000 0.0000 0.0000 0.01029(13) Uani 1 4 d S . . S S 0.5000 -0.15307(6) 0.47598(9) 0.0337(2) Uani 1 2 d S . . N N 0.5000 -0.10009(14) 0.1580(3) 0.0181(5) Uani 1 2 d S . . C C 0.5000 -0.12144(17) 0.2911(3) 0.0183(5) Uani 1 2 d S . . N1 N 0.28077(6) 0.15213(10) 0.43102(19) 0.0156(3) Uani 1 1 d . . . C2 C 0.27550(7) 0.23418(11) 0.4466(2) 0.0148(3) Uani 1 1 d . . . C3 C 0.31477(7) 0.29331(12) 0.3686(2) 0.0187(4) Uani 1 1 d . . . H3 H 0.3068(10) 0.3525(16) 0.379(3) 0.021(6) Uiso 1 1 d . . . C4 C 0.36180(7) 0.26439(12) 0.2726(2) 0.0182(4) Uani 1 1 d . . . H4 H 0.3896(10) 0.3028(17) 0.221(3) 0.023(6) Uiso 1 1 d . . . C5 C 0.41661(7) 0.14068(12) 0.1575(2) 0.0152(4) Uani 1 1 d . . . H5 H 0.4447(8) 0.1776(13) 0.101(2) 0.007(4) Uiso 1 1 d . . . N6 N 0.42371(6) 0.05947(10) 0.13865(18) 0.0147(3) Uani 1 1 d . . . C7 C 0.38164(7) 0.00765(13) 0.2137(2) 0.0174(4) Uani 1 1 d . . . H7 H 0.3876(10) -0.0480(18) 0.194(3) 0.026(6) Uiso 1 1 d . . . C8 C 0.33412(8) 0.03573(12) 0.3076(2) 0.0184(4) Uani 1 1 d . . . H8 H 0.3053(9) -0.0039(16) 0.353(3) 0.016(5) Uiso 1 1 d . . . C9 C 0.32722(7) 0.12253(11) 0.3333(2) 0.0145(3) Uani 1 1 d . . . C10 C 0.36925(7) 0.17704(11) 0.2542(2) 0.0138(3) Uani 1 1 d . . . 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 Co 0.00832(18) 0.0113(2) 0.0112(2) -0.00319(18) 0.000 0.000 S 0.0368(4) 0.0464(5) 0.0180(4) 0.0042(3) 0.000 0.000 N 0.0151(9) 0.0186(11) 0.0205(13) 0.0023(9) 0.000 0.000 C 0.0111(9) 0.0215(13) 0.0222(15) -0.0016(10) 0.000 0.000 N1 0.0138(6) 0.0176(7) 0.0153(8) -0.0029(6) 0.0028(5) 0.0017(5) C2 0.0106(6) 0.0198(9) 0.0141(9) -0.0040(7) 0.0002(6) 0.0008(6) C3 0.0164(7) 0.0162(10) 0.0233(10) -0.0047(7) 0.0048(6) 0.0003(6) C4 0.0156(7) 0.0167(10) 0.0223(10) -0.0031(7) 0.0059(6) -0.0021(6) C5 0.0114(7) 0.0191(9) 0.0150(10) -0.0024(7) 0.0016(6) 0.0000(6) N6 0.0111(5) 0.0189(7) 0.0142(8) -0.0048(6) 0.0012(5) 0.0011(5) C7 0.0160(7) 0.0140(10) 0.0223(10) -0.0030(7) 0.0022(6) 0.0014(6) C8 0.0168(7) 0.0178(9) 0.0207(10) -0.0005(7) 0.0041(7) -0.0012(6) C9 0.0120(6) 0.0181(9) 0.0135(9) -0.0025(6) -0.0001(5) 0.0007(6) C10 0.0113(6) 0.0164(9) 0.0135(8) -0.0024(6) -0.0001(5) 0.0003(6) 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 Co N 2.071(2) 9_655 ? Co N 2.071(2) . ? Co N6 2.2175(13) . ? Co N6 2.2175(13) 2 ? Co N6 2.2175(13) 10_655 ? Co N6 2.2175(13) 9_655 ? S C 1.627(3) . ? N C 1.165(4) . ? N1 C2 1.317(2) . ? N1 C9 1.372(2) . ? C2 C3 1.422(2) . ? C2 C2 1.499(3) 13_556 ? C3 C4 1.369(2) . ? C4 C10 1.408(2) . ? C5 N6 1.311(2) . ? C5 C10 1.422(2) . ? N6 C7 1.374(2) . ? C7 C8 1.362(2) . ? C8 C9 1.406(3) . ? C9 C10 1.415(2) . ? 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 N Co N 180.0 9_655 . ? N Co N6 90.33(6) 9_655 . ? N Co N6 89.67(6) . . ? N Co N6 89.67(6) 9_655 2 ? N Co N6 90.33(6) . 2 ? N6 Co N6 84.96(7) . 2 ? N Co N6 90.33(6) 9_655 10_655 ? N Co N6 89.67(6) . 10_655 ? N6 Co N6 95.04(7) . 10_655 ? N6 Co N6 180.0 2 10_655 ? N Co N6 89.67(6) 9_655 9_655 ? N Co N6 90.33(6) . 9_655 ? N6 Co N6 180.00(4) . 9_655 ? N6 Co N6 95.04(7) 2 9_655 ? N6 Co N6 84.96(7) 10_655 9_655 ? C N Co 146.7(2) . . ? N C S 178.9(3) . . ? C2 N1 C9 117.51(15) . . ? N1 C2 C3 124.04(15) . . ? N1 C2 C2 117.06(19) . 13_556 ? C3 C2 C2 118.9(2) . 13_556 ? C4 C3 C2 118.89(17) . . ? C3 C4 C10 118.67(16) . . ? N6 C5 C10 123.56(16) . . ? C5 N6 C7 117.43(14) . . ? C5 N6 Co 124.72(11) . . ? C7 N6 Co 117.84(12) . . ? C8 C7 N6 123.89(18) . . ? C7 C8 C9 119.29(17) . . ? N1 C9 C8 120.32(15) . . ? N1 C9 C10 122.02(16) . . ? C8 C9 C10 117.65(15) . . ? C4 C10 C9 118.83(15) . . ? C4 C10 C5 123.04(16) . . ? C9 C10 C5 118.12(16) . . ? _geom_special_details ? #=END data_c105 _audit_author_name 'Mayer, P.' _audit_block_code Zn_bnp_SCN_c105_jan _audit_creation_method 'form98_1/compatible with shelxl97-2' _audit_creation_date 04-Sep-98 _chemical_name_systematic ;Bis-(2,2'-di(1,6-naphthyridine))-dithhiocyanato-zinc(II) ; _chemical_compound_source 'crystal provided by C. Janiak, Uni FR' _chemical_name_common 'Zn-BNP-KSCN, Nr. 0751' _chemical_formula_moiety '2(C16 N4 H10), 2(S C N), Zn' _chemical_formula_sum 'C34 H20 N10 S2 Zn' _chemical_formula_weight 698.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Zn' 'Zn' .2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m c a' _symmetry_Int_Tables_number 64 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' 'x, -y+1/2, z+1/2' 'x, y+1/2, -z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, -z' 'x+1/2, -y+1, z+1/2' 'x+1/2, y+1, -z+1/2' '-x, -y, -z' '-x, y, z' '-x, y-1/2, -z-1/2' '-x, -y-1/2, z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, z' '-x+1/2, y, -z-1/2' '-x+1/2, -y, z-1/2' _cell_length_a 21.5003(19) _cell_length_b 15.9253(10) _cell_length_c 8.3967(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2875.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(3) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 28.0 _cell_special_details 'Orthorhombic C (as derived from metrics)' _exptl_crystal_description prismatic _exptl_crystal_colour brownish _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.6129(2) _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 1.047 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7811 _exptl_absorpt_correction_T_max 0.8793 _exptl_absorpt_process_details 'XRed, rev. 1.06, Stoe (Darmstadt, Germany)' _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 0 0 0.0640 1 0 0 0.0620 0 -1 -1 0.1040 0 1 -1 0.1090 0 0 1 0.2090 0 1 0 0.0850 0 -1 0 0.0760 _diffrn_ambient_temperature 200(3) _diffr_source_type 'Spellman DF4 Series' _diffr_source_power 2.00_kW _diffr_source_voltage 50_kV _diffr_source_current 40_mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation '0.5 mm collimator' _diffrn_measurement_device 'image-plate area detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'area detection' _diffrn_detector_area_resol_mean ? _kl_diffrn_detector_area_phi_start 0.0 _kl_diffrn_detector_area_phi_end 144.0 _kl_diffrn_detector_area_phi_incr 1.0 _kl_diffrn_detector_area_expos_time 8.00_min _kl_diffrn_detector_area_plate_dist 60.0_mm _kl_diffrn_detector_area_eff_mos_spread 0.006 _kl_diffrn_detector_area_profile_funct dynamic _kl_diffrn_detector_area_profile_min 9 _kl_diffrn_detector_area_profile_max 21 _diffrn_special_details 'no crystal decay in terms of mean intensity per image' _diffrn_reflns_number 9429 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 27.92 _diffrn_measured_fraction_theta_max .993 _diffrn_reflns_theta_full 27.92 _diffrn_measured_fraction_theta_full .993 _refine_diff_density_max .525 _refine_diff_density_min -.424 _refine_diff_density_rms .070 _reflns_number_total 1762 _reflns_number_gt 1555 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Stoe IPDS software (Darmstadt, Germany)' _computing_cell_refinement 'Stoe IPDS software (Darmstadt, Germany)' _computing_data_reduction 'Stoe IPDS software (Darmstadt, Germany)' _computing_structure_solution 'SHELXS-97 (G. M. Sheldrick. University of G\"ottingen, Germany, 1997)' _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ;ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations, Oak Ridge National Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), Germany, 1995). ; _computing_publication_material ;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1762 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0759 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_special_details ? 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn 0.5000 0.0000 0.0000 0.01061(11) Uani 1 4 d S . . S S 0.5000 -0.15291(5) 0.47393(7) 0.03041(16) Uani 1 2 d S . . N N 0.5000 -0.10213(11) 0.1552(2) 0.0173(3) Uani 1 2 d S . . C C 0.5000 -0.12266(12) 0.2891(2) 0.0156(4) Uani 1 2 d S . . N1 N 0.28080(5) 0.15217(8) 0.43110(14) 0.0144(2) Uani 1 1 d . . . C2 C 0.27551(5) 0.23444(8) 0.44666(15) 0.0135(3) Uani 1 1 d . . . C3 C 0.31477(6) 0.29347(9) 0.36943(16) 0.0168(3) Uani 1 1 d . . . H3 H 0.3067(8) 0.3524(13) 0.382(2) 0.022(4) Uiso 1 1 d . . . C4 C 0.36164(6) 0.26458(8) 0.27419(16) 0.0165(3) Uani 1 1 d . . . H4 H 0.3876(9) 0.3034(14) 0.221(2) 0.025(5) Uiso 1 1 d . . . C5 C 0.41641(5) 0.14109(8) 0.15938(15) 0.0137(3) Uani 1 1 d . . . H5 H 0.4443(8) 0.1786(10) 0.106(2) 0.013(4) Uiso 1 1 d . . . N6 N 0.42353(5) 0.05951(7) 0.14120(13) 0.0138(2) Uani 1 1 d . . . C7 C 0.38171(6) 0.00786(8) 0.21557(18) 0.0165(3) Uani 1 1 d . . . H7 H 0.3880(8) -0.0493(13) 0.199(2) 0.017(4) Uiso 1 1 d . . . C8 C 0.33399(6) 0.03565(9) 0.30883(16) 0.0163(3) Uani 1 1 d . . . H8 H 0.3063(9) -0.0020(10) 0.357(2) 0.018(5) Uiso 1 1 d . . . C9 C 0.32711(5) 0.12296(8) 0.33429(15) 0.0129(3) Uani 1 1 d . . . C10 C 0.36921(6) 0.17710(8) 0.25569(16) 0.0126(3) Uani 1 1 d . . . 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 Zn 0.00932(16) 0.01097(17) 0.01154(17) -0.00203(10) 0.000 0.000 S 0.0347(3) 0.0413(4) 0.0152(3) 0.0038(2) 0.000 0.000 N 0.0146(7) 0.0188(8) 0.0185(8) 0.0022(7) 0.000 0.000 C 0.0111(7) 0.0155(8) 0.0202(9) -0.0015(7) 0.000 0.000 N1 0.0134(5) 0.0156(5) 0.0140(5) -0.0028(4) 0.0029(4) 0.0010(4) C2 0.0102(5) 0.0179(6) 0.0125(6) -0.0040(5) 0.0011(4) 0.0006(4) C3 0.0149(6) 0.0136(6) 0.0219(6) -0.0044(5) 0.0043(5) -0.0002(5) C4 0.0144(6) 0.0144(6) 0.0207(6) -0.0020(5) 0.0050(5) -0.0022(5) C5 0.0102(5) 0.0165(6) 0.0142(6) -0.0012(5) 0.0015(4) -0.0003(4) N6 0.0116(5) 0.0155(5) 0.0142(5) -0.0032(4) 0.0011(4) 0.0007(4) C7 0.0157(6) 0.0129(6) 0.0210(7) -0.0025(5) 0.0023(5) 0.0009(5) C8 0.0158(6) 0.0144(6) 0.0187(6) -0.0004(5) 0.0041(5) -0.0010(5) C9 0.0108(5) 0.0158(6) 0.0121(6) -0.0018(5) 0.0009(4) 0.0009(4) C10 0.0100(5) 0.0149(6) 0.0128(5) -0.0027(5) 0.0007(4) 0.0004(4) 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 Zn N 2.0840(17) 9_655 ? Zn N 2.0840(17) . ? Zn N6 2.2376(10) 2 ? Zn N6 2.2376(10) . ? Zn N6 2.2376(10) 9_655 ? Zn N6 2.2376(10) 10_655 ? S C 1.625(2) . ? N C 1.171(3) . ? N1 C2 1.3216(17) . ? N1 C9 1.3668(16) . ? C2 C3 1.4200(18) . ? C2 C2 1.500(2) 13_556 ? C3 C4 1.3663(17) . ? C4 C10 1.4112(18) . ? C5 N6 1.3170(18) . ? C5 C10 1.4187(17) . ? N6 C7 1.3692(17) . ? C7 C8 1.3644(18) . ? C8 C9 1.4145(19) . ? C9 C10 1.4138(18) . ? 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 N Zn N 180.0 9_655 . ? N Zn N6 89.96(4) 9_655 2 ? N Zn N6 90.04(4) . 2 ? N Zn N6 90.04(4) 9_655 . ? N Zn N6 89.96(4) . . ? N6 Zn N6 85.43(5) 2 . ? N Zn N6 89.96(4) 9_655 9_655 ? N Zn N6 90.04(4) . 9_655 ? N6 Zn N6 94.58(5) 2 9_655 ? N6 Zn N6 179.999(1) . 9_655 ? N Zn N6 90.04(4) 9_655 10_655 ? N Zn N6 89.96(4) . 10_655 ? N6 Zn N6 180.0 2 10_655 ? N6 Zn N6 94.57(5) . 10_655 ? N6 Zn N6 85.42(5) 9_655 10_655 ? C N Zn 144.91(16) . . ? N C S 178.97(18) . . ? C2 N1 C9 117.32(11) . . ? N1 C2 C3 124.05(11) . . ? N1 C2 C2 116.70(14) . 13_556 ? C3 C2 C2 119.25(15) . 13_556 ? C4 C3 C2 118.87(12) . . ? C3 C4 C10 118.81(12) . . ? N6 C5 C10 123.24(12) . . ? C5 N6 C7 117.60(11) . . ? C5 N6 Zn 124.38(8) . . ? C7 N6 Zn 118.02(8) . . ? C8 C7 N6 124.10(12) . . ? C7 C8 C9 118.97(12) . . ? N1 C9 C10 122.44(12) . . ? N1 C9 C8 120.05(12) . . ? C10 C9 C8 117.51(11) . . ? C4 C10 C9 118.48(12) . . ? C4 C10 C5 122.98(12) . . ? C9 C10 C5 118.52(11) . . ? _geom_special_details ? #=END data_c106 _audit_author_name 'Mayer, P.' _audit_block_code Cd_bnp_SCN_c106_janiak _audit_creation_method 'form98_1/compatible with shelxl97-2' _audit_creation_date 05-Sep-98 _chemical_name_systematic ;Bis-(2,2'-di(1,6-naphthyridine))-dithiocyanato-cadmium(II) ; _chemical_compound_source 'crystal provided by C. Janiak, Uni FR' _chemical_name_common Cd_BNP_KSCN_2941 _chemical_formula_moiety '2(C16 N4 H10), 2(S C N), Cd' _chemical_formula_sum 'C34 H20 Cd N10 S2' _chemical_formula_weight 745.133 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cd' 'Cd' -.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m c a' _symmetry_Int_Tables_number 64 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' 'x, -y+1/2, z+1/2' 'x, y+1/2, -z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, -z' 'x+1/2, -y+1, z+1/2' 'x+1/2, y+1, -z+1/2' '-x, -y, -z' '-x, y, z' '-x, y-1/2, -z-1/2' '-x, -y-1/2, z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, z' '-x+1/2, y, -z-1/2' '-x+1/2, -y, z-1/2' _cell_length_a 21.9537(13) _cell_length_b 16.0270(11) _cell_length_c 8.5477(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3007.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(3) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.9 _cell_special_details 'Orthorhombic C (as derived from metrics)' _exptl_crystal_description prismatic _exptl_crystal_colour brownish _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.64567(16) _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.910 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6776 _exptl_absorpt_correction_T_max 0.9117 _exptl_absorpt_process_details 'XRed, rev. 1.06, Stoe (Darmstadt, Germany)' _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 -1 0 0.0630 -1 1 0 0.0610 -1 -1 0 0.0990 1 1 0 0.1140 -2 -2 -1 0.2340 0 2 -1 0.2050 1 -1 1 0.2580 _diffrn_ambient_temperature 200(3) _diffr_source_type 'Spellman DF4 Series' _diffr_source_power 2.00_kW _diffr_source_voltage 50_kV _diffr_source_current 40_mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation '0.8 mm collimator' _diffrn_measurement_device 'image-plate area detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'area detection' _diffrn_detector_area_resol_mean ? _kl_diffrn_detector_area_phi_start 0.0 _kl_diffrn_detector_area_phi_end 283.2 _kl_diffrn_detector_area_phi_incr 0.8 _kl_diffrn_detector_area_expos_time 2.00_min _kl_diffrn_detector_area_plate_dist 60.0_mm _kl_diffrn_detector_area_eff_mos_spread 0.005 _kl_diffrn_detector_area_profile_funct dynamic _kl_diffrn_detector_area_profile_min 11 _kl_diffrn_detector_area_profile_max 23 _diffrn_special_details 'no crystal decay in terms of mean intensity per image' _diffrn_reflns_number 19631 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0145 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.92 _diffrn_measured_fraction_theta_max .994 _diffrn_reflns_theta_full 27.92 _diffrn_measured_fraction_theta_full .994 _refine_diff_density_max .627 _refine_diff_density_min -.582 _refine_diff_density_rms .075 _reflns_number_total 1841 _reflns_number_gt 1679 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Stoe IPDS software (Darmstadt, Germany)' _computing_cell_refinement 'Stoe IPDS software (Darmstadt, Germany)' _computing_data_reduction 'Stoe IPDS software (Darmstadt, Germany)' _computing_structure_solution 'SHELXS-97 (G. M. Sheldrick. University of G\"ottingen, Germany, 1997)' _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ;ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations, Oak Ridge National Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), Germany, 1995). ; _computing_publication_material ;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1841 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0262 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0616 _refine_ls_wR_factor_gt 0.0606 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_special_details ? 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd 0.5000 0.0000 0.0000 0.01244(9) Uani 1 4 d S . . S S 0.5000 -0.15897(6) 0.47724(8) 0.0420(2) Uani 1 2 d S . . N N 0.5000 -0.11244(13) 0.1631(2) 0.0264(4) Uani 1 2 d S . . C C 0.5000 -0.13015(14) 0.2948(3) 0.0219(4) Uani 1 2 d S . . N1 N 0.28011(6) 0.15320(8) 0.43134(15) 0.0184(3) Uani 1 1 d . . . C2 C 0.27520(6) 0.23489(9) 0.44788(18) 0.0169(3) Uani 1 1 d . . . C3 C 0.31376(7) 0.29342(10) 0.37328(19) 0.0223(3) Uani 1 1 d . . . H3 H 0.3069(10) 0.3512(13) 0.389(2) 0.029(5) Uiso 1 1 d . . . C4 C 0.35973(7) 0.26533(10) 0.2800(2) 0.0221(3) Uani 1 1 d . . . H4 H 0.3863(11) 0.3024(16) 0.229(3) 0.040(6) Uiso 1 1 d . . . C5 C 0.41337(7) 0.14316(9) 0.16587(17) 0.0182(3) Uani 1 1 d . . . H5 H 0.4407(9) 0.1779(11) 0.113(2) 0.016(4) Uiso 1 1 d . . . N6 N 0.41998(6) 0.06229(8) 0.14750(14) 0.0187(3) Uani 1 1 d . . . C7 C 0.37934(8) 0.01072(10) 0.2206(2) 0.0228(3) Uani 1 1 d . . . H7 H 0.3855(9) -0.0458(14) 0.203(2) 0.022(5) Uiso 1 1 d . . . C8 C 0.33253(7) 0.03797(10) 0.31140(19) 0.0219(3) Uani 1 1 d . . . H8 H 0.3053(10) 0.0007(11) 0.363(3) 0.025(6) Uiso 1 1 d . . . C9 C 0.32570(6) 0.12472(9) 0.33633(17) 0.0166(3) Uani 1 1 d . . . C10 C 0.36690(7) 0.17863(9) 0.25984(18) 0.0168(3) Uani 1 1 d . . . 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 Cd 0.00920(12) 0.01392(12) 0.01418(12) -0.00516(7) 0.000 0.000 S 0.0512(5) 0.0522(5) 0.0226(3) 0.0026(3) 0.000 0.000 N 0.0244(10) 0.0255(10) 0.0292(10) 0.0050(8) 0.000 0.000 C 0.0155(9) 0.0205(10) 0.0296(12) -0.0011(9) 0.000 0.000 N1 0.0156(6) 0.0196(6) 0.0199(6) -0.0043(5) 0.0045(5) 0.0009(5) C2 0.0117(6) 0.0214(7) 0.0177(6) -0.0056(6) 0.0022(5) 0.0011(5) C3 0.0192(7) 0.0171(7) 0.0304(8) -0.0068(6) 0.0074(6) -0.0004(6) C4 0.0179(7) 0.0186(7) 0.0296(8) -0.0036(6) 0.0083(6) -0.0022(6) C5 0.0135(6) 0.0209(7) 0.0201(7) -0.0040(6) 0.0032(5) 0.0005(6) N6 0.0151(6) 0.0205(6) 0.0204(6) -0.0067(5) 0.0038(5) 0.0018(5) C7 0.0219(8) 0.0169(7) 0.0295(9) -0.0047(6) 0.0053(7) 0.0011(6) C8 0.0211(7) 0.0179(7) 0.0267(7) -0.0014(6) 0.0079(6) -0.0012(6) C9 0.0136(6) 0.0185(7) 0.0176(6) -0.0036(5) 0.0017(5) 0.0011(5) C10 0.0135(6) 0.0187(7) 0.0181(6) -0.0038(5) 0.0023(5) 0.0005(5) 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 Cd N 2.278(2) 9_655 ? Cd N 2.278(2) . ? Cd N6 2.3816(12) 2 ? Cd N6 2.3817(12) . ? Cd N6 2.3817(12) 10_655 ? Cd N6 2.3817(12) 9_655 ? S C 1.626(2) . ? N C 1.161(3) . ? N1 C2 1.3213(19) . ? N1 C9 1.3674(18) . ? C2 C3 1.415(2) . ? C2 C2 1.501(3) 13_556 ? C3 C4 1.363(2) . ? C4 C10 1.409(2) . ? C5 N6 1.3137(19) . ? C5 C10 1.418(2) . ? N6 C7 1.367(2) . ? C7 C8 1.360(2) . ? C8 C9 1.414(2) . ? C9 C10 1.411(2) . ? 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 N Cd N 180.0 9_655 . ? N Cd N6 90.43(5) 9_655 2 ? N Cd N6 89.57(5) . 2 ? N Cd N6 89.57(5) 9_655 . ? N Cd N6 90.43(5) . . ? N6 Cd N6 84.95(6) 2 . ? N Cd N6 89.57(5) 9_655 10_655 ? N Cd N6 90.43(5) . 10_655 ? N6 Cd N6 180.0 2 10_655 ? N6 Cd N6 95.05(6) . 10_655 ? N Cd N6 90.43(5) 9_655 9_655 ? N Cd N6 89.57(5) . 9_655 ? N6 Cd N6 95.05(6) 2 9_655 ? N6 Cd N6 180.0 . 9_655 ? N6 Cd N6 84.95(6) 10_655 9_655 ? C N Cd 141.88(19) . . ? N C S 177.6(2) . . ? C2 N1 C9 117.01(13) . . ? N1 C2 C3 124.04(13) . . ? N1 C2 C2 116.32(16) . 13_556 ? C3 C2 C2 119.65(16) . 13_556 ? C4 C3 C2 119.18(14) . . ? C3 C4 C10 118.70(14) . . ? N6 C5 C10 122.88(14) . . ? C5 N6 C7 118.02(13) . . ? C5 N6 Cd 123.94(10) . . ? C7 N6 Cd 118.02(10) . . ? C8 C7 N6 124.04(14) . . ? C7 C8 C9 118.80(14) . . ? N1 C9 C10 122.67(13) . . ? N1 C9 C8 119.68(13) . . ? C10 C9 C8 117.65(13) . . ? C4 C10 C9 118.39(14) . . ? C4 C10 C5 123.04(14) . . ? C9 C10 C5 118.57(13) . . ? _geom_special_details ? #=END data_c104 _audit_author_name 'Mayer, P.' _audit_block_code Cu_bnp_BF4_c104_jan _audit_creation_method 'form98_1/compatible with shelxl97-2' _audit_creation_date 03-Sep-98 _chemical_name_systematic ;2,2'-Di(1,6-naphthyridine)-acetonitrile-copper(I)tetrafluoroborate dichloromethane (2:1) ; _chemical_compound_source 'crystal provided by C. Janiak, Uni FR' _chemical_name_common 'Cu-BNP-CH3CN-BF4, Nr. 0946' _chemical_formula_moiety 'B F4, 0.5(C H2 Cl2), Cu, C16 N4 H10, C2 H3 N' _chemical_formula_sum 'C18.50 H14 B Cl Cu F4 N5' _chemical_formula_weight 492.146 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' .3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' .0013 .0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.4063(16) _cell_length_b 8.1045(4) _cell_length_c 22.5896(18) _cell_angle_alpha 90.00 _cell_angle_beta 100.771(9) _cell_angle_gamma 90.00 _cell_volume 4029.8(5) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 25.9 _cell_special_details 'Monoclinic C (as derived from metrics)' _exptl_crystal_description block _exptl_crystal_colour 'red, blue, dichroitic' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.6224(2) _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 1.269 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7563 _exptl_absorpt_correction_T_max 0.8648 _exptl_absorpt_process_details 'X-RED, Revision 1.06, May 1996' _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.069 -1 0 0 0.052 -1 -1 3 0.133 0 -2 -3 0.100 -1 2 -4 0.078 -1 1 4 0.096 _diffrn_ambient_temperature 200(2) _diffr_source_type 'Spellman DF4 Series' _diffr_source_power 2.00_kW _diffr_source_voltage 50_kV _diffr_source_current 40_mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation '0.5 mm collimator' _diffrn_measurement_device 'image-plate area detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'area detection' _diffrn_detector_area_resol_mean ? _kl_diffrn_detector_area_phi_start 0.0 _kl_diffrn_detector_area_phi_end 136.0 _kl_diffrn_detector_area_phi_incr 0.8 _kl_diffrn_detector_area_expos_time 4.00_min _kl_diffrn_detector_area_plate_dist 70.0_mm _kl_diffrn_detector_area_eff_mos_spread 0.005 _kl_diffrn_detector_area_profile_funct dynamic _kl_diffrn_detector_area_profile_min 11 _kl_diffrn_detector_area_profile_max 19 _diffrn_special_details 'no crystal decay in terms of mean intensity per image' _diffrn_reflns_number 10377 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.81 _diffrn_measured_fraction_theta_max .977 _diffrn_reflns_theta_full 25.81 _diffrn_measured_fraction_theta_full .977 _refine_diff_density_max .631 _refine_diff_density_min -.441 _refine_diff_density_rms .069 _reflns_number_total 3792 _reflns_number_gt 2754 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Stoe IPDS software' _computing_cell_refinement 'Stoe IPDS software' _computing_data_reduction 'Stoe IPDS software' _computing_structure_solution 'SHELXS-97 (G. M. Sheldrick. University of G\"ottingen, Germany, 1997)' _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ;ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations, Oak Ridge National Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), Germany, 1995). ; _computing_publication_material ;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3792 _refine_ls_number_parameters 357 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0844 _refine_ls_wR_factor_gt 0.0797 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.910 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_special_details ; Hydrogen atoms of: bnp: refall, CH3CN: riding with U(H)=1.5*U(C), HFIX 137, CH2Cl2: riding with U(H)=1.2*U(C), DFIX 0.97 \%A, Disorder: the fluorine atoms of the BF4 moiety are disordered, two tetrahedra were found (F1...F4, F5...F8), the occupancy factors are 0.59 and 0.41, resp., the fluorines have been refined anisotropically, thus the disordered entity is not analyzed carefully but is smoothed out! ; 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.197452(12) 0.61533(4) 0.108476(13) 0.02887(11) Uani 1 1 d . . . N1 N 0.27243(8) 0.7580(3) 0.14427(9) 0.0242(5) Uani 1 1 d . . . C2 C 0.32123(10) 0.7210(3) 0.12163(11) 0.0251(5) Uani 1 1 d . . . C3 C 0.38065(11) 0.7605(4) 0.15093(12) 0.0328(6) Uani 1 1 d . . . H3 H 0.4126(13) 0.733(4) 0.1333(13) 0.029(7) Uiso 1 1 d . . . C4 C 0.38926(11) 0.8357(4) 0.20579(12) 0.0335(7) Uani 1 1 d . . . H4 H 0.4276(14) 0.864(4) 0.2248(14) 0.043(8) Uiso 1 1 d . . . C5 C 0.34254(11) 0.9417(4) 0.28950(12) 0.0301(6) Uani 1 1 d . . . H5 H 0.3795(13) 0.964(4) 0.3114(13) 0.033(7) Uiso 1 1 d . . . N6 N 0.29515(9) 0.9712(3) 0.31464(9) 0.0283(5) Uani 1 1 d . . . C7 C 0.23878(11) 0.9326(4) 0.28210(12) 0.0285(6) Uani 1 1 d . . . H7 H 0.2029(13) 0.948(4) 0.3015(13) 0.037(8) Uiso 1 1 d . . . C8 C 0.22964(10) 0.8676(4) 0.22593(12) 0.0284(6) Uani 1 1 d . . . H8 H 0.1881(12) 0.840(4) 0.2038(13) 0.032(7) Uiso 1 1 d . . . C9 C 0.28015(10) 0.8327(3) 0.19931(11) 0.0246(6) Uani 1 1 d . . . C10 C 0.33856(10) 0.8723(4) 0.23201(11) 0.0270(5) Uani 1 1 d . . . N1' N 0.25255(8) 0.5676(3) 0.04866(9) 0.0246(5) Uani 1 1 d . . . C2' C 0.30877(10) 0.6270(4) 0.06395(10) 0.0256(5) Uani 1 1 d . . . C3' C 0.35374(12) 0.6016(4) 0.02870(12) 0.0322(6) Uani 1 1 d . . . H3' H 0.3899(13) 0.647(4) 0.0413(13) 0.036(8) Uiso 1 1 d . . . C4' C 0.33992(12) 0.5141(4) -0.02320(12) 0.0346(7) Uani 1 1 d . . . H4' H 0.3698(12) 0.496(4) -0.0461(13) 0.030(7) Uiso 1 1 d . . . C5' C 0.26168(13) 0.3602(4) -0.09507(12) 0.0353(6) Uani 1 1 d . . . H5' H 0.2927(12) 0.338(4) -0.1189(13) 0.032(7) Uiso 1 1 d . . . N6' N 0.20667(11) 0.3042(3) -0.11279(10) 0.0398(6) Uani 1 1 d . . . C7' C 0.16590(13) 0.3354(4) -0.07639(13) 0.0392(7) Uani 1 1 d . . . H7' H 0.1257(15) 0.291(4) -0.0913(16) 0.053(10) Uiso 1 1 d . . . C8' C 0.17876(12) 0.4191(4) -0.02340(12) 0.0340(7) Uani 1 1 d . . . H8' H 0.1504(13) 0.438(4) -0.0011(14) 0.034(8) Uiso 1 1 d . . . C9' C 0.23801(11) 0.4816(3) -0.00441(11) 0.0261(5) Uani 1 1 d . . . C10' C 0.28071(11) 0.4513(4) -0.04111(11) 0.0286(6) Uani 1 1 d . . . N11 N 0.11240(9) 0.6657(3) 0.08813(10) 0.0351(6) Uani 1 1 d . . . C21 C 0.06156(12) 0.6798(4) 0.07999(14) 0.0399(7) Uani 1 1 d . . . C31 C -0.00422(14) 0.6954(6) 0.0709(2) 0.0688(12) Uani 1 1 d . . . H31A H -0.0219 0.5902 0.0804 0.103 Uiso 1 1 calc R . . H31B H -0.0201 0.7246 0.0288 0.103 Uiso 1 1 calc R . . H31C H -0.0149 0.7819 0.0974 0.103 Uiso 1 1 calc R . . Cl Cl 0.56539(7) 0.3105(2) 0.27675(7) 0.1148(5) Uani 1 1 d . . . C C 0.5000 0.4275(9) 0.2500 0.0791(18) Uani 1 2 d SD . . H H 0.5090(19) 0.490(5) 0.2162(14) 0.095 Uiso 1 1 d D . . B B 0.45886(19) 0.7044(7) 0.3880(2) 0.0634(13) Uani 1 1 d . . . F1 F 0.4755(5) 0.809(2) 0.3474(7) 0.075(3) Uani 0.591(8) 1 d P . . F2 F 0.4229(4) 0.7785(12) 0.4200(4) 0.097(3) Uani 0.591(8) 1 d P . . F3 F 0.5013(3) 0.6157(11) 0.4198(4) 0.112(4) Uani 0.591(8) 1 d P . . F4 F 0.4150(3) 0.5882(8) 0.3550(3) 0.117(3) Uani 0.591(8) 1 d P . . F5 F 0.5093(3) 0.7863(16) 0.4364(3) 0.104(4) Uani 0.409(8) 1 d P . . F6 F 0.4822(8) 0.5591(16) 0.3911(8) 0.157(7) Uani 0.409(8) 1 d P . . F7 F 0.4731(10) 0.778(4) 0.3387(11) 0.106(9) Uani 0.409(8) 1 d P . . F8 F 0.4114(4) 0.7495(19) 0.4066(7) 0.131(8) Uani 0.409(8) 1 d P . . 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 Cu 0.02219(15) 0.0426(2) 0.02250(16) 0.00134(16) 0.00588(10) -0.00151(15) N1 0.0246(9) 0.0288(12) 0.0201(10) 0.0014(9) 0.0062(8) -0.0004(9) C2 0.0253(12) 0.0280(15) 0.0233(12) 0.0028(11) 0.0076(9) 0.0011(10) C3 0.0225(12) 0.0481(19) 0.0297(14) -0.0043(13) 0.0098(10) 0.0004(12) C4 0.0233(12) 0.047(2) 0.0295(14) -0.0041(13) 0.0040(10) 0.0004(11) C5 0.0218(12) 0.0399(17) 0.0274(13) 0.0006(12) 0.0015(10) 0.0029(11) N6 0.0283(10) 0.0340(14) 0.0231(10) -0.0018(10) 0.0064(8) 0.0035(9) C7 0.0235(12) 0.0342(17) 0.0298(13) -0.0020(11) 0.0100(10) -0.0015(10) C8 0.0218(11) 0.0345(16) 0.0299(13) -0.0036(12) 0.0076(9) 0.0002(11) C9 0.0245(11) 0.0293(15) 0.0207(12) 0.0018(10) 0.0060(9) 0.0014(10) C10 0.0245(11) 0.0327(16) 0.0243(12) -0.0004(12) 0.0058(9) 0.0020(11) N1' 0.0254(10) 0.0296(13) 0.0193(10) 0.0024(9) 0.0052(8) 0.0029(8) C2' 0.0270(11) 0.0307(15) 0.0198(11) 0.0026(11) 0.0060(9) 0.0019(11) C3' 0.0294(13) 0.0392(17) 0.0307(14) -0.0021(13) 0.0129(10) -0.0052(12) C4' 0.0366(14) 0.0418(19) 0.0300(14) -0.0023(13) 0.0179(12) 0.0003(13) C5' 0.0456(15) 0.0350(19) 0.0268(13) -0.0003(12) 0.0108(11) 0.0037(13) N6' 0.0455(14) 0.0445(16) 0.0274(12) -0.0051(11) 0.0021(10) 0.0030(11) C7' 0.0364(14) 0.046(2) 0.0326(15) -0.0052(13) -0.0011(12) 0.0006(13) C8' 0.0285(12) 0.046(2) 0.0266(13) -0.0015(12) 0.0027(11) 0.0017(12) C9' 0.0309(12) 0.0253(15) 0.0219(12) 0.0047(11) 0.0043(9) 0.0042(10) C10' 0.0358(13) 0.0274(15) 0.0232(12) 0.0027(11) 0.0068(10) 0.0014(11) N11 0.0276(11) 0.0447(16) 0.0339(12) 0.0057(11) 0.0078(9) 0.0011(10) C21 0.0319(15) 0.049(2) 0.0389(16) 0.0023(14) 0.0079(12) -0.0002(13) C31 0.0284(15) 0.090(3) 0.086(3) -0.004(2) 0.0072(16) 0.0068(17) Cl 0.1055(9) 0.1279(14) 0.1148(11) 0.0379(10) 0.0304(8) 0.0341(9) C 0.083(4) 0.083(5) 0.069(4) 0.000 0.010(3) 0.000 B 0.055(2) 0.073(4) 0.067(3) 0.024(3) 0.024(2) 0.022(2) F1 0.033(3) 0.095(4) 0.101(9) 0.045(5) 0.024(4) 0.008(3) F2 0.137(7) 0.080(4) 0.087(4) -0.012(4) 0.056(4) 0.019(4) F3 0.055(3) 0.127(9) 0.152(7) 0.083(7) 0.012(3) 0.034(4) F4 0.130(5) 0.127(5) 0.097(4) -0.029(4) 0.031(4) -0.068(4) F5 0.077(4) 0.169(11) 0.068(4) -0.015(5) 0.015(3) 0.005(5) F6 0.218(18) 0.051(5) 0.196(15) -0.012(7) 0.023(12) 0.022(8) F7 0.065(7) 0.20(2) 0.048(5) 0.046(9) 0.010(4) 0.033(9) F8 0.025(3) 0.196(15) 0.186(13) 0.148(12) 0.051(5) 0.039(5) 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 Cu N11 1.919(2) . ? Cu N1' 2.031(2) . ? Cu N6 2.074(2) 4_545 ? Cu N1 2.075(2) . ? N1 C2 1.325(3) . ? N1 C9 1.364(3) . ? C2 C3 1.409(3) . ? C2 C2' 1.490(4) . ? C3 C4 1.362(4) . ? C4 C10 1.408(4) . ? C5 N6 1.316(3) . ? C5 C10 1.403(4) . ? N6 C7 1.373(3) . ? N6 Cu 2.074(2) 4 ? C7 C8 1.354(4) . ? C8 C9 1.406(3) . ? C9 C10 1.414(3) . ? N1' C2' 1.333(3) . ? N1' C9' 1.372(3) . ? C2' C3' 1.411(3) . ? C3' C4' 1.356(4) . ? C4' C10' 1.408(4) . ? C5' N6' 1.304(4) . ? C5' C10' 1.421(4) . ? N6' C7' 1.362(4) . ? C7' C8' 1.359(4) . ? C8' C9' 1.411(4) . ? C9' C10' 1.400(4) . ? N11 C21 1.125(3) . ? C21 C31 1.455(4) . ? Cl C 1.755(4) . ? C Cl 1.755(4) 2_655 ? B F8 1.268(10) . ? B F6 1.285(14) . ? B F3 1.296(7) . ? B F2 1.324(8) . ? B F1 1.351(13) . ? B F7 1.35(2) . ? B F4 1.461(7) . ? B F5 1.567(10) . ? 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 N11 Cu N1' 125.53(9) . . ? N11 Cu N6 103.94(9) . 4_545 ? N1' Cu N6 119.11(9) . 4_545 ? N11 Cu N1 132.09(10) . . ? N1' Cu N1 79.45(8) . . ? N6 Cu N1 93.17(8) 4_545 . ? C2 N1 C9 118.6(2) . . ? C2 N1 Cu 112.95(17) . . ? C9 N1 Cu 123.91(16) . . ? N1 C2 C3 122.9(2) . . ? N1 C2 C2' 114.8(2) . . ? C3 C2 C2' 122.2(2) . . ? C4 C3 C2 119.3(2) . . ? C3 C4 C10 119.3(2) . . ? N6 C5 C10 123.7(2) . . ? C5 N6 C7 117.6(2) . . ? C5 N6 Cu 121.24(18) . 4 ? C7 N6 Cu 119.87(17) . 4 ? C8 C7 N6 123.6(2) . . ? C7 C8 C9 119.1(2) . . ? N1 C9 C8 120.2(2) . . ? N1 C9 C10 121.6(2) . . ? C8 C9 C10 118.1(2) . . ? C5 C10 C4 123.9(2) . . ? C5 C10 C9 117.9(2) . . ? C4 C10 C9 118.2(2) . . ? C2' N1' C9' 117.9(2) . . ? C2' N1' Cu 114.93(16) . . ? C9' N1' Cu 127.13(16) . . ? N1' C2' C3' 122.8(2) . . ? N1' C2' C2 115.2(2) . . ? C3' C2' C2 122.1(2) . . ? C4' C3' C2' 119.5(2) . . ? C3' C4' C10' 119.2(2) . . ? N6' C5' C10' 124.0(3) . . ? C5' N6' C7' 116.9(2) . . ? C8' C7' N6' 124.7(3) . . ? C7' C8' C9' 118.7(3) . . ? N1' C9' C10' 122.0(2) . . ? N1' C9' C8' 120.3(2) . . ? C10' C9' C8' 117.7(2) . . ? C9' C10' C4' 118.5(2) . . ? C9' C10' C5' 118.1(2) . . ? C4' C10' C5' 123.4(2) . . ? C21 N11 Cu 172.0(3) . . ? N11 C21 C31 178.5(4) . . ? Cl C Cl 114.6(5) 2_655 . ? _geom_special_details ?