# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name _publ_author_address A.Lytvynenko 'Institute of Physical Chemistry of NAS of Ukraine, Pr.Nauki 31,Kiev,Ukraine' S.Kolotilov 'Institute of Physical Chemistry of NAS of Ukraine, Pr.Nauki 31,Kiev,Ukraine' O.Cador 'Sci.Chim.de Rennes,UMR UR1-CNRS 6226, Univ.de Rennes 1,35042 Rennes,France' S.Golhen 'Sci.Chim.de Rennes,UMR UR1-CNRS 6226, Univ.de Rennes 1,35042 Rennes,France' L.Ouahab 'Sci.Chim.de Rennes,UMR UR1-CNRS 6226, Univ.de Rennes 1,35042 Rennes,France' ; V.Pavlishchuk ; 'Institute of Physical Chemistry of NAS of Ukraine, Pr.Nauki 31,Kiev,Ukraine' _publ_contact_author_name 'Dr Lahcene Ouahab' _publ_contact_author_email lahcene.ouahab@univ-rennes1.fr _publ_section_title ; Antiferromagnetic ordering in Cobalt(II) and nickel(II) 1D coordination polymers with dithioamide of 1,3-benzenedicarboxylic acid ; _publ_contact_author_address 'Sci.Chim.de Rennes,UMR UR1-CNRS 6226, Univ.de Rennes 1,35042 Rennes,France' _publ_contact_author_fax '+33 (0)2 23 23 68 40' _publ_contact_author_phone '+33 (0)2 23 23 56 59' # Attachment '- Compound1.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 813877' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H8 Cl2 Co N2 S2' _chemical_formula_weight 326.11 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' S S 0.1246 0.1234 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M c2/c 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 10.513(2) _cell_length_b 15.638(1) _cell_length_c 7.496(1) _cell_angle_alpha 90.00 _cell_angle_beta 104.450(5) _cell_angle_gamma 90.00 _cell_volume 1193.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1564 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 28.700 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 2.201 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2988 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 4.05 _diffrn_reflns_theta_max 28.70 _reflns_number_total 1540 _reflns_number_gt 1119 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'Sir 97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0913P)^2^+0.2630P] where P=(Fo^2^+2Fc^2^)/3' _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 1540 _refine_ls_number_parameters 78 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1508 _refine_ls_wR_factor_gt 0.1352 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7621(3) 0.0783(2) 0.5795(5) 0.0329(7) Uani 1 1 d . . . C2 C 0.8858(3) 0.0324(2) 0.6646(4) 0.0312(7) Uani 1 1 d . . . C3 C 1.0000 0.0765(3) 0.7500 0.0329(10) Uani 1 2 d S . . H3 H 1.0000 0.1360 0.7500 0.040 Uiso 1 2 calc SR . . C4 C 0.8871(3) -0.0567(2) 0.6622(4) 0.0344(7) Uani 1 1 d . . . H4 H 0.8123 -0.0866 0.6017 0.041 Uiso 1 1 calc R . . C5 C 1.0000 -0.1012(3) 0.7500 0.0383(11) Uani 1 2 d S . . H5 H 1.0000 -0.1606 0.7500 0.046 Uiso 1 2 calc SR . . N1 N 0.7442(3) 0.1550(2) 0.6396(5) 0.0467(8) Uani 1 1 d . . . S1 S 0.65010(8) 0.02956(6) 0.40817(12) 0.0377(3) Uani 1 1 d . . . Cl1 Cl 0.42778(10) 0.21351(6) 0.44759(13) 0.0492(3) Uani 1 1 d . . . Co1 Co 0.5000 0.12853(4) 0.2500 0.0372(3) Uani 1 2 d S . . H1N H 0.672(4) 0.186(3) 0.605(5) 0.041(10) Uiso 1 1 d . . . H2N H 0.788(5) 0.183(4) 0.746(8) 0.082(17) Uiso 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 C1 0.0267(15) 0.0356(17) 0.0337(16) 0.0018(13) 0.0023(12) -0.0001(12) C2 0.0256(15) 0.0362(17) 0.0284(15) -0.0006(12) 0.0001(12) 0.0001(12) C3 0.030(2) 0.032(2) 0.033(2) 0.000 0.0002(17) 0.000 C4 0.0322(16) 0.0358(17) 0.0316(16) -0.0010(13) 0.0011(13) -0.0039(13) C5 0.038(2) 0.036(3) 0.038(3) 0.000 0.002(2) 0.000 N1 0.0337(16) 0.0418(18) 0.054(2) -0.0078(15) -0.0094(14) 0.0061(13) S1 0.0303(5) 0.0386(5) 0.0371(5) -0.0033(3) -0.0052(3) 0.0023(3) Cl1 0.0506(6) 0.0451(6) 0.0472(6) -0.0040(4) 0.0036(4) 0.0086(4) Co1 0.0318(4) 0.0371(4) 0.0362(4) 0.000 -0.0038(3) 0.000 _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 C1 N1 1.312(5) . ? C1 C2 1.483(4) . ? C1 S1 1.692(3) . ? C2 C4 1.394(5) . ? C2 C3 1.394(4) . ? C3 C2 1.394(4) 2_756 ? C4 C5 1.391(4) . ? C5 C4 1.391(4) 2_756 ? S1 Co1 2.3146(9) . ? Cl1 Co1 2.2577(11) . ? Co1 Cl1 2.2577(11) 2_655 ? Co1 S1 2.3146(9) 2_655 ? 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 N1 C1 C2 118.7(3) . . ? N1 C1 S1 122.7(3) . . ? C2 C1 S1 118.6(2) . . ? C4 C2 C3 119.3(3) . . ? C4 C2 C1 119.3(3) . . ? C3 C2 C1 121.4(3) . . ? C2 C3 C2 120.7(4) . 2_756 ? C5 C4 C2 120.2(3) . . ? C4 C5 C4 120.1(5) 2_756 . ? C1 S1 Co1 110.13(12) . . ? Cl1 Co1 Cl1 107.89(6) . 2_655 ? Cl1 Co1 S1 115.58(4) . 2_655 ? Cl1 Co1 S1 110.82(3) 2_655 2_655 ? Cl1 Co1 S1 110.82(3) . . ? Cl1 Co1 S1 115.58(4) 2_655 . ? S1 Co1 S1 96.07(5) 2_655 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.599 _refine_diff_density_min -0.841 _refine_diff_density_rms 0.130 # Attachment '- Compound2.cif' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 813878' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H8 Br2 Co N2 S2' _chemical_formula_weight 415.03 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' S S 0.1246 0.1234 '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' Br Br -0.2901 2.4595 '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' 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 10.6100(5) _cell_length_b 16.1750(6) _cell_length_c 7.5080(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.83(1) _cell_angle_gamma 90.00 _cell_volume 1245.58(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2546 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.213 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 8.096 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4764 _diffrn_reflns_av_R_equivalents 0.0749 _diffrn_reflns_av_sigmaI/netI 0.0592 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 4.71 _diffrn_reflns_theta_max 27.45 _reflns_number_total 1419 _reflns_number_gt 985 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'Sir 2004' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0655P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1419 _refine_ls_number_parameters 70 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1305 _refine_ls_wR_factor_gt 0.1144 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.2633(5) 0.0772(3) 0.4244(8) 0.0373(12) Uani 1 1 d . . . C2 C -0.3867(5) 0.0334(3) 0.3367(7) 0.0329(11) Uani 1 1 d . . . C3 C -0.5000 0.0755(5) 0.2500 0.0354(16) Uani 1 2 d S . . H3 H -0.5000 0.1330 0.2500 0.042 Uiso 1 2 calc SR . . C4 C -0.3886(6) -0.0539(3) 0.3380(8) 0.0395(13) Uani 1 1 d . . . H1 H -0.3144 -0.0832 0.3984 0.047 Uiso 1 1 calc R . . C5 C -0.5000 -0.0957(5) 0.2500 0.0422(19) Uani 1 2 d S . . H6 H -0.5000 -0.1532 0.2500 0.051 Uiso 1 2 calc SR . . N1 N -0.2467(5) 0.1521(3) 0.3668(8) 0.0559(15) Uani 1 1 d . . . H1A H -0.3064 0.1744 0.2806 0.067 Uiso 1 1 calc R . . H1B H -0.1762 0.1788 0.4152 0.067 Uiso 1 1 calc R . . S1 S -0.15133(15) 0.02954(9) 0.5927(2) 0.0410(4) Uani 1 1 d . . . Co1 Co 0.0000 0.12444(7) 0.7500 0.0390(3) Uani 1 2 d S . . Br1 Br 0.07834(7) 0.21143(4) 0.54389(9) 0.0505(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 C1 0.035(3) 0.036(3) 0.039(3) -0.001(2) 0.006(2) -0.001(2) C2 0.026(3) 0.036(3) 0.032(3) 0.000(2) 0.000(2) -0.001(2) C3 0.030(4) 0.037(4) 0.035(4) 0.000 0.000(3) 0.000 C4 0.039(3) 0.036(3) 0.040(3) 0.003(2) 0.003(2) 0.004(2) C5 0.043(5) 0.036(4) 0.041(5) 0.000 -0.001(4) 0.000 N1 0.043(3) 0.045(3) 0.063(4) 0.014(3) -0.016(3) -0.008(3) S1 0.0345(7) 0.0394(7) 0.0418(8) 0.0035(6) -0.0036(6) -0.0020(6) Co1 0.0352(6) 0.0372(6) 0.0388(6) 0.000 -0.0007(5) 0.000 Br1 0.0533(5) 0.0445(4) 0.0512(4) 0.0030(3) 0.0091(3) -0.0079(3) _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 C1 N1 1.313(7) . ? C1 C2 1.486(7) . ? C1 S1 1.683(6) . ? C2 C3 1.391(6) . ? C2 C4 1.412(8) . ? C3 C2 1.391(6) 2_455 ? C4 C5 1.375(7) . ? C5 C4 1.375(7) 2_455 ? S1 Co1 2.3146(16) . ? Co1 S1 2.3146(16) 2_556 ? Co1 Br1 2.3925(9) . ? Co1 Br1 2.3925(9) 2_556 ? 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 N1 C1 C2 118.1(5) . . ? N1 C1 S1 122.8(5) . . ? C2 C1 S1 119.1(4) . . ? C3 C2 C4 118.8(5) . . ? C3 C2 C1 122.1(5) . . ? C4 C2 C1 119.1(5) . . ? C2 C3 C2 121.3(7) 2_455 . ? C5 C4 C2 120.0(6) . . ? C4 C5 C4 121.1(8) . 2_455 ? C1 S1 Co1 110.1(2) . . ? S1 Co1 S1 96.92(8) . 2_556 ? S1 Co1 Br1 111.75(4) . . ? S1 Co1 Br1 114.17(4) 2_556 . ? S1 Co1 Br1 114.17(4) . 2_556 ? S1 Co1 Br1 111.75(4) 2_556 2_556 ? Br1 Co1 Br1 107.95(5) . 2_556 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.658 _refine_diff_density_min -0.969 _refine_diff_density_rms 0.155 # Attachment '- Compound3.cif' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 813879' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H16 Br2 N4 Ni S4' _chemical_formula_weight 611.10 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.912(1) _cell_length_b 10.124(2) _cell_length_c 13.225(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.737(1) _cell_angle_gamma 90.00 _cell_volume 1029.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2572 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.878 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.972 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 5.242 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4591 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.0728 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.89 _reflns_number_total 2450 _reflns_number_gt 1489 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'Sir 2004' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0765P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2450 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1030 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1432 _refine_ls_wR_factor_gt 0.1208 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1631(8) -0.2293(6) -0.1034(5) 0.0410(13) Uani 1 1 d . . . C2 C 0.0931(7) -0.3657(6) -0.1205(4) 0.0396(13) Uani 1 1 d . . . C3 C -0.0836(8) -0.3920(7) -0.1400(5) 0.0486(15) Uani 1 1 d . . . H3 H -0.1624 -0.3227 -0.1457 0.058 Uiso 1 1 calc R . . C4 C 0.2092(8) -0.4704(6) -0.1171(5) 0.0403(14) Uani 1 1 d . . . H4 H 0.3276 -0.4537 -0.1069 0.048 Uiso 1 1 calc R . . C5 C 1.1438(8) -0.4785(7) 0.1513(6) 0.0532(17) Uani 1 1 d . . . H5 H 1.2626 -0.4619 0.1635 0.064 Uiso 1 1 calc R . . C6 C 1.0287(7) -0.3744(7) 0.1445(5) 0.0474(15) Uani 1 1 d . . . H6 H 1.0693 -0.2879 0.1503 0.057 Uiso 1 1 calc R . . C7 C 0.8525(7) -0.4000(6) 0.1291(4) 0.0403(13) Uani 1 1 d . . . C8 C 0.7248(8) -0.2887(6) 0.1212(5) 0.0443(14) Uani 1 1 d . . . N1 N 0.5956(7) -0.3071(6) 0.1683(5) 0.0565(15) Uani 1 1 d . . . H1A H 0.5889 -0.3796 0.2010 0.068 Uiso 1 1 calc R . . H1B H 0.5188 -0.2463 0.1662 0.068 Uiso 1 1 calc R . . N2 N 0.0515(7) -0.1369(6) -0.0899(5) 0.0614(16) Uani 1 1 d . . . H2A H -0.0545 -0.1577 -0.0913 0.074 Uiso 1 1 calc R . . H2B H 0.0851 -0.0562 -0.0797 0.074 Uiso 1 1 calc R . . S1 S 0.7455(2) -0.15444(16) 0.05256(14) 0.0465(4) Uani 1 1 d . . . S2 S 0.3700(2) -0.19420(17) -0.10347(13) 0.0480(4) Uani 1 1 d . . . Ni1 Ni 0.5000 0.0000 0.0000 0.0377(3) Uani 1 2 d S . . Br1 Br 0.65766(8) 0.04829(6) -0.14600(5) 0.0448(2) 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 C1 0.046(3) 0.033(3) 0.048(3) 0.000(3) 0.017(2) 0.000(3) C2 0.044(3) 0.034(3) 0.042(3) 0.001(3) 0.013(2) 0.003(3) C3 0.048(3) 0.037(4) 0.059(4) -0.001(3) 0.010(3) 0.000(3) C4 0.041(3) 0.036(4) 0.047(3) 0.001(3) 0.017(2) -0.005(3) C5 0.035(3) 0.051(5) 0.072(5) -0.004(4) 0.010(3) -0.002(3) C6 0.044(3) 0.039(4) 0.059(4) 0.001(3) 0.012(3) -0.009(3) C7 0.045(3) 0.033(3) 0.045(3) -0.001(3) 0.014(3) 0.002(3) C8 0.048(3) 0.032(3) 0.054(4) -0.002(3) 0.013(3) -0.001(3) N1 0.058(3) 0.041(3) 0.080(4) 0.012(3) 0.035(3) 0.010(3) N2 0.050(3) 0.044(3) 0.095(5) -0.017(3) 0.027(3) -0.003(3) S1 0.0506(9) 0.0308(9) 0.0631(10) 0.0073(7) 0.0236(7) 0.0025(7) S2 0.0468(9) 0.0363(9) 0.0651(10) -0.0109(8) 0.0215(7) -0.0032(7) Ni1 0.0446(6) 0.0277(6) 0.0445(6) -0.0003(5) 0.0177(5) -0.0006(4) Br1 0.0542(4) 0.0372(4) 0.0489(4) 0.0026(3) 0.0240(3) 0.0027(3) _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 C1 N2 1.328(8) . ? C1 C2 1.485(9) . ? C1 S2 1.675(6) . ? C2 C3 1.386(8) . ? C2 C4 1.396(8) . ? C3 C5 1.390(9) 3_645 ? C4 C7 1.396(9) 3_645 ? C5 C6 1.382(9) . ? C5 C3 1.390(9) 3_645 ? C6 C7 1.385(8) . ? C7 C4 1.396(9) 3_645 ? C7 C8 1.500(8) . ? C8 N1 1.332(8) . ? C8 S1 1.664(6) . ? S1 Ni1 2.4617(16) . ? S2 Ni1 2.4754(17) . ? Ni1 S1 2.4617(16) 3_655 ? Ni1 S2 2.4754(17) 3_655 ? Ni1 Br1 2.5820(6) . ? Ni1 Br1 2.5820(6) 3_655 ? 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 N2 C1 C2 116.1(5) . . ? N2 C1 S2 122.1(5) . . ? C2 C1 S2 121.8(4) . . ? C3 C2 C4 119.1(6) . . ? C3 C2 C1 122.0(5) . . ? C4 C2 C1 118.8(5) . . ? C2 C3 C5 120.4(6) . 3_645 ? C2 C4 C7 120.0(5) . 3_645 ? C6 C5 C3 120.5(6) . 3_645 ? C5 C6 C7 119.5(6) . . ? C6 C7 C4 120.3(6) . 3_645 ? C6 C7 C8 120.5(6) . . ? C4 C7 C8 119.1(5) 3_645 . ? N1 C8 C7 116.2(5) . . ? N1 C8 S1 123.7(5) . . ? C7 C8 S1 120.0(5) . . ? C8 S1 Ni1 120.0(2) . . ? C1 S2 Ni1 116.5(2) . . ? S1 Ni1 S1 180.00 . 3_655 ? S1 Ni1 S2 81.27(6) . . ? S1 Ni1 S2 98.73(6) 3_655 . ? S1 Ni1 S2 98.73(6) . 3_655 ? S1 Ni1 S2 81.27(6) 3_655 3_655 ? S2 Ni1 S2 180.00 . 3_655 ? S1 Ni1 Br1 80.94(4) . . ? S1 Ni1 Br1 99.06(4) 3_655 . ? S2 Ni1 Br1 87.03(4) . . ? S2 Ni1 Br1 92.97(4) 3_655 . ? S1 Ni1 Br1 99.06(4) . 3_655 ? S1 Ni1 Br1 80.94(4) 3_655 3_655 ? S2 Ni1 Br1 92.97(4) . 3_655 ? S2 Ni1 Br1 87.03(4) 3_655 3_655 ? Br1 Ni1 Br1 180.00 . 3_655 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.616 _refine_diff_density_min -0.896 _refine_diff_density_rms 0.161 # Attachment 'Ligand.cif' data_m-dtab _database_code_depnum_ccdc_archive 'CCDC 813880' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H8 N2 S2' _chemical_formula_weight 196.28 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 4.27790(10) _cell_length_b 14.0489(6) _cell_length_c 14.9941(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.425(3) _cell_angle_gamma 90.00 _cell_volume 897.11(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2784 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.508 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.9 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 408 _exptl_absorpt_coefficient_mu 0.535 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5287 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 30.50 _reflns_number_total 2730 _reflns_number_gt 1512 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution Sir-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1045P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2730 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1207 _refine_ls_R_factor_gt 0.0602 _refine_ls_wR_factor_ref 0.1849 _refine_ls_wR_factor_gt 0.1488 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.26905(19) 0.35534(6) 1.00191(5) 0.0587(3) Uani 1 1 d . . . S2 S 0.90835(16) 0.51583(5) 0.63582(5) 0.0478(2) Uani 1 1 d . . . N1 N 0.1121(5) 0.47841(17) 0.87309(15) 0.0479(6) Uani 1 1 d . . . H1A H 0.1110 0.4982 0.8188 0.057 Uiso 1 1 calc R . . H1B H 0.0249 0.5119 0.9119 0.057 Uiso 1 1 calc R . . N2 N 0.7712(7) 0.36497(19) 0.53606(17) 0.0637(7) Uani 1 1 d . . . H2A H 0.7017 0.3079 0.5278 0.076 Uiso 1 1 calc R . . H2B H 0.8398 0.3959 0.4924 0.076 Uiso 1 1 calc R . . C6 C 0.3922(5) 0.34397(17) 0.82485(16) 0.0384(5) Uani 1 1 d . . . C3 C 0.6731(6) 0.24877(17) 0.68971(18) 0.0438(6) Uani 1 1 d . . . H3 H 0.7663 0.2166 0.6449 0.053 Uiso 1 1 calc R . . C2 C 0.6512(5) 0.34759(17) 0.68773(16) 0.0380(5) Uani 1 1 d . . . C8 C 0.2476(5) 0.39673(19) 0.89688(16) 0.0411(6) Uani 1 1 d . . . C5 C 0.4174(6) 0.24538(18) 0.82583(19) 0.0456(6) Uani 1 1 d . . . H5 H 0.3410 0.2107 0.8719 0.055 Uiso 1 1 calc R . . C1 C 0.7727(6) 0.40508(19) 0.61574(17) 0.0417(6) Uani 1 1 d . . . C7 C 0.5107(5) 0.39426(18) 0.75566(16) 0.0394(6) Uani 1 1 d . . . H7 H 0.4961 0.4603 0.7547 0.047 Uiso 1 1 calc R . . C4 C 0.5556(6) 0.1986(2) 0.75861(19) 0.0501(7) Uani 1 1 d . . . H4 H 0.5699 0.1326 0.7597 0.060 Uiso 1 1 calc R . . 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 S1 0.0759(5) 0.0654(6) 0.0369(4) 0.0082(3) 0.0170(3) 0.0115(4) S2 0.0651(5) 0.0383(4) 0.0422(4) 0.0027(3) 0.0159(3) -0.0038(3) N1 0.0634(14) 0.0465(14) 0.0357(12) 0.0004(10) 0.0144(10) 0.0060(10) N2 0.103(2) 0.0525(15) 0.0388(14) -0.0037(12) 0.0247(13) -0.0148(13) C6 0.0429(12) 0.0394(13) 0.0328(12) 0.0016(10) 0.0039(9) -0.0024(9) C3 0.0543(14) 0.0366(13) 0.0410(14) -0.0035(11) 0.0069(11) 0.0030(10) C2 0.0422(12) 0.0395(13) 0.0326(12) 0.0010(10) 0.0051(9) -0.0003(9) C8 0.0434(13) 0.0441(14) 0.0366(13) 0.0000(11) 0.0081(10) -0.0045(10) C5 0.0578(15) 0.0366(13) 0.0426(15) 0.0049(11) 0.0057(11) -0.0063(10) C1 0.0493(13) 0.0394(13) 0.0380(14) -0.0002(11) 0.0126(10) 0.0030(10) C7 0.0459(13) 0.0345(13) 0.0383(13) 0.0010(10) 0.0072(10) -0.0009(9) C4 0.0684(17) 0.0314(14) 0.0513(17) 0.0018(12) 0.0104(13) -0.0010(11) _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 S2 C1 1.678(3) . ? S1 C8 1.673(3) . ? N1 C8 1.319(3) . ? N2 C1 1.320(3) . ? C6 C5 1.389(3) . ? C6 C7 1.390(3) . ? C6 C8 1.491(3) . ? C3 C4 1.383(4) . ? C3 C2 1.392(3) . ? C2 C7 1.394(3) . ? C2 C1 1.481(3) . ? C5 C4 1.382(4) . ? 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 C5 C6 C7 118.8(2) . . ? C5 C6 C8 121.7(2) . . ? C7 C6 C8 119.6(2) . . ? C4 C3 C2 119.7(2) . . ? C3 C2 C7 119.1(2) . . ? C3 C2 C1 122.1(2) . . ? C7 C2 C1 118.8(2) . . ? N1 C8 C6 116.0(2) . . ? N1 C8 S1 122.7(2) . . ? C6 C8 S1 121.3(2) . . ? C4 C5 C6 120.3(2) . . ? N2 C1 C2 117.0(2) . . ? N2 C1 S2 122.0(2) . . ? C2 C1 S2 120.94(19) . . ? C6 C7 C2 121.3(2) . . ? C5 C4 C3 120.9(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.495 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.083