# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 loop_ _publ_author_address ; School of Chemistry, The University of Edinburgh, Joseph Black Building The Kings Buildings West mains road Edinburgh, EH9 3JJ, UK. ; _publ_contact_author_address ; School of Chemistry, The University of Edinburgh, Joseph Black Building The Kings Buildings West mains road Edinburgh, EH9 3JJ, UK. ; _publ_contact_author_email neil.robertson@ed.ac.uk _publ_contact_author_fax ? _publ_contact_author_phone '+44 (0)131 6504804' #looking for refcif _publ_contact_author_name 'Neil Robertson' _journal_coeditor_code ? _journal_date_accepted ? _journal_date_from_coeditor ? #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? loop_ _publ_author_footnote ; FIRST AUTHORS FOOTNOTES ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_category FA _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_author_name 'Neil Robertson' data_nr2009 _database_code_depnum_ccdc_archive 'CCDC 882247' #TrackingRef '- Co(L1).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H14 Co N4' _chemical_formula_sum 'C18 H14 Co N4' _chemical_formula_weight 345.26 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' 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' _cell_length_a 14.707(2) _cell_length_b 5.1858(8) _cell_length_c 17.973(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1370.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1461 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 20.66 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 1.256 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8055 _exptl_absorpt_correction_T_max 0.9875 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7681 _diffrn_reflns_av_R_equivalents 0.0964 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 20.82 _reflns_number_total 1432 _reflns_number_gt 1002 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 2008) and local programs' _refine_special_details ; The data set was integrated to a resolution of 1 A, there being no measurable diffraction at higher resolution. Mild similarity restraints were used on the displacement ellipsoids of some atoms. The absolute structure parameter is based on 686 Friedel pairs. When all atoms had been identified there remained a residual peak approximately 1.37 e.A-3 located 1.79 A from N3 and 1.85 A from C9. There is no obvious chemical or crystallographic explanation for this peak. The diffraction pattern has no evidence of untreated twinning, for example, and the position of the peak does not make chemical sense to be modelled as solvent. 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^)+(0.0891P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881; 686 Friedel pairs' _refine_ls_abs_structure_Flack 0.07(9) _refine_ls_number_reflns 1432 _refine_ls_number_parameters 209 _refine_ls_number_restraints 199 _refine_ls_R_factor_all 0.0840 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1457 _refine_ls_wR_factor_gt 0.1272 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 0.995 _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 Co1 Co 0.62462(9) 0.5002(3) 0.6498(2) 0.0271(4) Uani 1 1 d . . . N1 N 0.5334(9) 0.2420(12) 0.6488(10) 0.023(3) Uani 1 1 d U . . N2 N 0.5748(6) 0.590(2) 0.7429(6) 0.028(2) Uani 1 1 d U . . N3 N 0.7094(9) 0.7597(13) 0.6537(9) 0.026(3) Uani 1 1 d U . . N4 N 0.6736(7) 0.414(2) 0.5571(6) 0.029(3) Uani 1 1 d U . . C1 C 0.4796(16) 0.234(2) 0.7108(10) 0.025(3) Uani 1 1 d U . . C2 C 0.4115(7) 0.055(2) 0.7277(6) 0.027(3) Uani 1 1 d U . . H2 H 0.3994 -0.0804 0.6934 0.032 Uiso 1 1 calc R . . C3 C 0.3614(9) 0.069(2) 0.7925(6) 0.029(3) Uani 1 1 d U . . H3 H 0.3133 -0.0505 0.8003 0.035 Uiso 1 1 calc R . . C4 C 0.3806(13) 0.261(2) 0.8489(9) 0.021(3) Uani 1 1 d U . . H4 H 0.3482 0.2696 0.8946 0.025 Uiso 1 1 calc R . . C5 C 0.4514(7) 0.436(2) 0.8308(6) 0.029(3) Uani 1 1 d U . . H5 H 0.4661 0.5669 0.8657 0.035 Uiso 1 1 calc R . . C6 C 0.5013(8) 0.425(2) 0.7638(6) 0.027(3) Uani 1 1 d U . . C7 C 0.6014(14) 0.774(2) 0.7886(11) 0.027(4) Uani 1 1 d U . . H7 H 0.5705 0.7949 0.8346 0.032 Uiso 1 1 calc R . . C8 C 0.6754(9) 0.942(3) 0.7709(7) 0.032(3) Uani 1 1 d U . . H8 H 0.6911 1.0700 0.8065 0.038 Uiso 1 1 calc R . . C9 C 0.7257(9) 0.932(2) 0.7062(6) 0.031(3) Uani 1 1 d U . . H9 H 0.7735 1.0532 0.6992 0.037 Uiso 1 1 calc R . . C10 C 0.7691(15) 0.766(2) 0.5854(9) 0.022(3) Uani 1 1 d U . . C11 C 0.8379(7) 0.946(2) 0.5713(6) 0.027(3) Uani 1 1 d U . . H11 H 0.8503 1.0810 0.6056 0.033 Uiso 1 1 calc R . . C12 C 0.8867(10) 0.922(2) 0.5069(7) 0.033(3) Uani 1 1 d U . . H12 H 0.9341 1.0393 0.4948 0.040 Uiso 1 1 calc R . . C13 C 0.8653(14) 0.729(2) 0.4621(10) 0.034(4) Uani 1 1 d U . . H13 H 0.9009 0.7148 0.4182 0.041 Uiso 1 1 calc R . . C14 C 0.7995(8) 0.548(2) 0.4705(6) 0.032(3) Uani 1 1 d U . . H14 H 0.7893 0.4154 0.4352 0.039 Uiso 1 1 calc R . . C15 C 0.7486(8) 0.574(2) 0.5346(6) 0.027(3) Uani 1 1 d U . . C16 C 0.6425(13) 0.227(2) 0.5141(11) 0.028(4) Uani 1 1 d U . . H16 H 0.6739 0.2016 0.4686 0.034 Uiso 1 1 calc R . . C17 C 0.5724(8) 0.071(3) 0.5269(7) 0.033(3) Uani 1 1 d U . . H17 H 0.5556 -0.0483 0.4892 0.039 Uiso 1 1 calc R . . C18 C 0.5224(8) 0.074(2) 0.5932(6) 0.028(3) Uani 1 1 d U . . H18 H 0.4768 -0.0546 0.5991 0.034 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 Co1 0.0236(6) 0.0374(7) 0.0203(7) -0.0015(6) 0.0003(6) 0.0007(6) N1 0.027(6) 0.028(7) 0.015(5) 0.007(4) -0.009(5) 0.005(3) N2 0.013(6) 0.053(7) 0.018(6) 0.004(5) -0.006(4) 0.003(4) N3 0.021(6) 0.043(8) 0.013(6) 0.002(4) 0.006(5) 0.008(3) N4 0.035(7) 0.023(6) 0.028(6) -0.003(5) 0.005(5) 0.001(4) C1 0.022(7) 0.033(7) 0.021(6) 0.003(4) -0.008(5) 0.008(4) C2 0.018(6) 0.036(6) 0.026(5) -0.005(5) -0.003(4) 0.001(4) C3 0.015(7) 0.046(7) 0.027(5) -0.002(5) -0.011(5) -0.001(5) C4 0.026(7) 0.032(7) 0.005(5) 0.008(4) -0.003(6) 0.001(4) C5 0.032(6) 0.040(7) 0.016(5) 0.002(4) -0.002(5) -0.003(4) C6 0.022(6) 0.036(7) 0.022(6) 0.003(4) 0.000(5) -0.002(4) C7 0.028(8) 0.035(8) 0.017(7) -0.002(5) 0.006(6) 0.008(5) C8 0.037(7) 0.032(7) 0.027(6) -0.008(5) -0.001(5) 0.002(5) C9 0.031(7) 0.034(8) 0.028(6) -0.001(5) 0.005(5) 0.001(6) C10 0.018(6) 0.035(7) 0.012(5) 0.011(4) -0.001(5) 0.001(4) C11 0.023(6) 0.035(6) 0.024(5) 0.005(4) -0.002(4) -0.004(4) C12 0.029(8) 0.042(7) 0.028(6) 0.013(5) 0.003(5) -0.009(6) C13 0.023(9) 0.054(10) 0.025(9) 0.002(5) 0.013(7) -0.001(6) C14 0.021(6) 0.049(8) 0.028(6) -0.002(5) -0.003(5) -0.001(5) C15 0.018(6) 0.041(7) 0.024(6) 0.000(5) -0.002(5) -0.005(5) C16 0.016(8) 0.053(10) 0.015(8) -0.011(6) -0.006(6) -0.004(5) C17 0.012(7) 0.055(9) 0.031(7) -0.006(6) -0.005(5) -0.001(5) C18 0.026(6) 0.031(7) 0.026(6) 0.001(4) -0.005(5) 0.005(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 Co1 N1 1.896(11) . ? Co1 N2 1.886(10) . ? Co1 N3 1.836(11) . ? Co1 N4 1.870(10) . ? N1 C1 1.37(2) . ? N1 C18 1.337(17) . ? N2 C6 1.428(15) . ? N2 C7 1.316(19) . ? N3 C9 1.323(17) . ? N3 C10 1.51(2) . ? N4 C15 1.438(15) . ? N4 C16 1.318(18) . ? C1 C2 1.40(2) . ? C1 C6 1.412(19) . ? C2 H2 0.950 . ? C2 C3 1.380(16) . ? C3 H3 0.950 . ? C3 C4 1.451(18) . ? C4 H4 0.950 . ? C4 C5 1.418(19) . ? C5 H5 0.950 . ? C5 C6 1.410(15) . ? C7 H7 0.950 . ? C7 C8 1.43(2) . ? C8 H8 0.950 . ? C8 C9 1.380(17) . ? C9 H9 0.950 . ? C10 C11 1.40(2) . ? C10 C15 1.386(18) . ? C11 H11 0.950 . ? C11 C12 1.369(16) . ? C12 H12 0.950 . ? C12 C13 1.323(19) . ? C13 H13 0.950 . ? C13 C14 1.354(19) . ? C14 H14 0.950 . ? C14 C15 1.380(15) . ? C16 H16 0.950 . ? C16 C17 1.33(2) . ? C17 H17 0.950 . ? C17 C18 1.400(17) . ? C18 H18 0.950 . ? 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 Co1 N2 84.7(7) . . ? N1 Co1 N3 177.2(9) . . ? N1 Co1 N4 95.4(7) . . ? N2 Co1 N3 92.8(6) . . ? N2 Co1 N4 179.5(6) . . ? N3 Co1 N4 87.0(6) . . ? Co1 N1 C1 115.1(11) . . ? Co1 N1 C18 123.6(13) . . ? C1 N1 C18 121.3(12) . . ? Co1 N2 C6 112.3(8) . . ? Co1 N2 C7 128.1(11) . . ? C6 N2 C7 119.6(12) . . ? Co1 N3 C9 130.2(13) . . ? Co1 N3 C10 112.4(10) . . ? C9 N3 C10 117.4(12) . . ? Co1 N4 C15 114.0(8) . . ? Co1 N4 C16 124.3(11) . . ? C15 N4 C16 121.6(13) . . ? N1 C1 C2 127.7(13) . . ? N1 C1 C6 113.4(15) . . ? C2 C1 C6 118.8(17) . . ? C1 C2 H2 119.0 . . ? C1 C2 C3 122.0(12) . . ? H2 C2 C3 119.0 . . ? C2 C3 H3 119.3 . . ? C2 C3 C4 121.5(13) . . ? H3 C3 C4 119.3 . . ? C3 C4 H4 122.5 . . ? C3 C4 C5 114.9(14) . . ? H4 C4 C5 122.5 . . ? C4 C5 H5 118.2 . . ? C4 C5 C6 123.6(12) . . ? H5 C5 C6 118.2 . . ? N2 C6 C1 114.4(13) . . ? N2 C6 C5 126.5(11) . . ? C1 C6 C5 119.0(13) . . ? N2 C7 H7 119.0 . . ? N2 C7 C8 122.0(16) . . ? H7 C7 C8 119.0 . . ? C7 C8 H8 117.5 . . ? C7 C8 C9 124.9(13) . . ? H8 C8 C9 117.5 . . ? N3 C9 C8 121.9(13) . . ? N3 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? N3 C10 C11 125.6(12) . . ? N3 C10 C15 113.2(13) . . ? C11 C10 C15 121.2(16) . . ? C10 C11 H11 120.9 . . ? C10 C11 C12 118.2(13) . . ? H11 C11 C12 120.9 . . ? C11 C12 H12 121.4 . . ? C11 C12 C13 117.2(14) . . ? H12 C12 C13 121.4 . . ? C12 C13 H13 115.6 . . ? C12 C13 C14 128.7(17) . . ? H13 C13 C14 115.6 . . ? C13 C14 H14 122.7 . . ? C13 C14 C15 114.5(12) . . ? H14 C14 C15 122.7 . . ? N4 C15 C10 113.4(12) . . ? N4 C15 C14 126.6(11) . . ? C10 C15 C14 120.0(13) . . ? N4 C16 H16 116.1 . . ? N4 C16 C17 127.9(18) . . ? H16 C16 C17 116.1 . . ? C16 C17 H17 118.4 . . ? C16 C17 C18 123.2(14) . . ? H17 C17 C18 118.4 . . ? N1 C18 C17 125.4(13) . . ? N1 C18 H18 117.3 . . ? C17 C18 H18 117.3 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 20.82 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.370 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.098 _vrf_THETM01_nr2009 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: The data set was integrated to a resolution of 1 A, there being no measurable diffraction at higher resolution. ; _vrf_REFNR01_nr2009 ; PROBLEM: Ratio of reflections to parameters is < 8 for a RESPONSE: The data set was integrated to a resolution of 1 A, there being no measurable diffraction at higher resolution. ; _vrf_REFLT03_nr2009 ; PROBLEM: Please check that the estimate of the number of Friedel pairs is RESPONSE: 686 Friedel pairs ; _vrf_PLAT003_nr2009 ; PROBLEM: Number of Uiso or Uij Restrained Atom Sites .... 22 RESPONSE: See _refine_special_details. ; _vrf_PLAT860_nr2009 ; PROBLEM: Note: Number of Least-Squares Restraints ....... 199 RESPONSE: See _refine_special_details. ; # Attachment '- Co(L1).Cl.cif' data_NR1003 _database_code_depnum_ccdc_archive 'CCDC 882248' _audit_creation_date 11-04-27 _audit_creation_method CRYSTALS_ver_14.11 _oxford_structure_analysis_title 'NR1003 in P-1' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_exptl_refinement ; Check-cif alerts Hydrogen atoms on the toluene solvent were added geometrically while all other hydrogen atoms were found in a difference map. All hydrogen atoms were constrained to ride on their parent atoms. 232_ALERT_2_B Hirshfeld Test Diff (M-X) Co2 -- Cl26 .. 11.91 su 232_ALERT_2_B Hirshfeld Test Diff (M-X) Co1 -- Cl1 .. 11.06 su 232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 -- N2 .. 5.70 su 232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 -- N4 .. 5.04 su Anisotropic displacement parameters for Co atoms are expected to be smaller because Co atoms reside at the centre of the coordination complex while Cl atoms are monodentate ligands with greater freedom of vibration. 411_ALERT_2_C Short Inter H...H Contact H111 .. H381 .. 2.13 Ang. 432_ALERT_2_C Short Inter X...Y Contact C5 .. C5 .. 3.18 Ang. Intermolecular pi stacking between aromatic rings results in short C5 - C5 contact, while H111 - H381 short contact probably arises from the large degree of disorder in the toluene solvent. 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 152 910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 3 911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 48 341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang .. 7 960_ALERT_3_G Number of Intensities with I .LT. - 2*sig(I) .. 1 Experiment conducted in a high pressure cell leading to reduced data set due to low sampling of reciprocal space. 243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors of C37 243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors of C42 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors of C41 302_ALERT_4_G Note: Anion/Solvent Disorder ................... 30.00 Perc. Toluene solvent is highly disordered and lies on an inversion centre, leading to large anisotropic displacement parameters. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 75 Thermal similarity, distance, and bond angle restraints applied between carbon atoms on toluene molecules. 929_ALERT_5_G No Weight Pars,Obs and Calc R1,wR2,S not checked ! ShelX weighting scheme not used. No action taken. 931_ALERT_5_G Check Twin Law ( 0 0 1)[ ] Estimated BASF 0.25 Twin law checked using ROTAX. No action taken. 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? No action taken. ; _publ_section_exptl_prep ; ? ; #end of refcif _cell_length_a 9.3850(9) _cell_length_b 13.3040(12) _cell_length_c 15.3654(11) _cell_angle_alpha 74.895(7) _cell_angle_beta 81.155(7) _cell_angle_gamma 75.541(8) _cell_volume 1785.5(3) _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Co -2.3653 3.6143 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C42 Cl2 Co2 N6 # Dc = 1.45 Fooo = 876.00 Mu = 89.72 M = 777.27 # Found Formula = C43 H36 Cl2 Co2 N8 # Dc = 1.59 FOOO = 876.00 Mu = 90.23 M = 853.58 _chemical_formula_sum 'C43 H36 Cl2 Co2 N8' _chemical_formula_moiety '2(C18 H14 Cl Co N4), C7 H8' _chemical_compound_source ? _chemical_formula_weight 853.58 _cell_measurement_reflns_used 11308 _cell_measurement_theta_min 3 _cell_measurement_theta_max 73 _cell_measurement_temperature 100 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_min 0.060 _exptl_crystal_size_mid 0.110 _exptl_crystal_size_max 0.250 _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 9.023 # Sheldrick geometric approximatio 0.37 0.58 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.32 _exptl_absorpt_correction_T_max 0.58 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_device Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 100 _diffrn_reflns_number 34656 _reflns_number_total 6975 _diffrn_reflns_av_R_equivalents 0.101 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 6975 # Theoretical number of reflections is about 14231 _diffrn_reflns_theta_min 2.992 _diffrn_reflns_theta_max 72.955 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 68.578 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min -15 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 1.65 _oxford_diffrn_Wilson_scale 0.10 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap,geom _refine_diff_density_min -1.13 _refine_diff_density_max 1.17 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 5964 _refine_ls_number_restraints 75 _refine_ls_number_parameters 524 _oxford_refine_ls_R_factor_ref 0.0833 _refine_ls_wR_factor_ref 0.0728 _refine_ls_goodness_of_fit_ref 1.1254 _refine_ls_shift/su_max 0.0023949 _refine_ls_shift/su_mean 0.0000942 # The values computed from all data _oxford_reflns_number_all 6934 _refine_ls_R_factor_all 0.0967 _refine_ls_wR_factor_all 0.0767 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5964 _refine_ls_R_factor_gt 0.0833 _refine_ls_wR_factor_gt 0.0728 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 43.6 42.2 43.2 22.4 3.99 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined data collection reference User defined data reduction User defined cell refinement Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Co1 Co 0.36170(6) 0.34216(4) 0.51537(4) 0.0125 1.0000 Uani . . . . . . Co2 Co 0.12333(6) 0.12903(5) 0.01985(4) 0.0142 1.0000 Uani . . . . . . Cl1 Cl 0.19525(10) 0.26984(7) 0.61570(6) 0.0247 1.0000 Uani . . . . . . Cl26 Cl 0.25131(10) 0.15942(7) 0.11748(6) 0.0265 1.0000 Uani . . . . . . N1 N 0.3101(3) 0.3129(2) 0.4120(2) 0.0184 1.0000 Uani . . . . . . N2 N 0.5090(3) 0.2158(2) 0.5177(2) 0.0205 1.0000 Uani . . . . . . N3 N 0.4480(3) 0.3865(2) 0.5985(2) 0.0191 1.0000 Uani . . . . . . N4 N 0.2484(3) 0.4829(2) 0.4941(2) 0.0187 1.0000 Uani . . . . . . N5 N 0.0158(3) 0.0393(3) 0.1056(2) 0.0212 1.0000 Uani . . . . . . N6 N 0.2523(3) -0.0014(3) 0.0056(2) 0.0202 1.0000 Uani . . . . . . N7 N 0.2051(3) 0.2126(2) -0.0870(2) 0.0205 1.0000 Uani . . . . . . N8 N -0.0292(3) 0.2529(2) 0.0168(2) 0.0204 1.0000 Uani . . . . . . C1 C 0.3939(4) 0.2173(3) 0.3915(2) 0.0213 1.0000 Uani . . . . . . C2 C 0.3811(5) 0.1761(3) 0.3192(3) 0.0258 1.0000 Uani . . . . . . C3 C 0.4776(5) 0.0834(3) 0.3047(3) 0.0308 1.0000 Uani . . . . . . C4 C 0.5903(5) 0.0322(3) 0.3615(3) 0.0274 1.0000 Uani . . . . . . C5 C 0.6039(4) 0.0711(3) 0.4338(3) 0.0236 1.0000 Uani . . . . . . C6 C 0.5054(4) 0.1646(3) 0.4492(2) 0.0210 1.0000 Uani . . . . . . C7 C 0.6029(4) 0.1711(3) 0.5809(3) 0.0231 1.0000 Uani . . . . . . C8 C 0.6212(4) 0.2202(3) 0.6460(3) 0.0261 1.0000 Uani . . . . . . C9 C 0.5513(4) 0.3240(3) 0.6509(3) 0.0243 1.0000 Uani . . . . . . C10 C 0.3837(4) 0.4910(3) 0.6083(2) 0.0227 1.0000 Uani . . . . . . C11 C 0.4209(4) 0.5428(3) 0.6661(3) 0.0265 1.0000 Uani . . . . . . C12 C 0.3431(5) 0.6448(3) 0.6693(3) 0.0316 1.0000 Uani . . . . . . C13 C 0.2269(5) 0.6953(3) 0.6161(3) 0.0300 1.0000 Uani . . . . . . C14 C 0.1891(4) 0.6455(3) 0.5574(3) 0.0284 1.0000 Uani . . . . . . C15 C 0.2682(4) 0.5425(3) 0.5519(2) 0.0202 1.0000 Uani . . . . . . C16 C 0.1441(4) 0.5241(3) 0.4352(2) 0.0222 1.0000 Uani . . . . . . C17 C 0.1191(4) 0.4708(3) 0.3745(3) 0.0244 1.0000 Uani . . . . . . C18 C 0.2012(4) 0.3726(3) 0.3626(2) 0.0222 1.0000 Uani . . . . . . C19 C 0.0883(4) -0.0684(3) 0.1259(2) 0.0240 1.0000 Uani . . . . . . C20 C 0.0414(4) -0.1514(3) 0.1917(3) 0.0258 1.0000 Uani . . . . . . C21 C 0.1254(5) -0.2545(4) 0.2016(3) 0.0323 1.0000 Uani . . . . . . C22 C 0.2576(5) -0.2759(3) 0.1472(3) 0.0313 1.0000 Uani . . . . . . C23 C 0.3060(5) -0.1949(3) 0.0821(3) 0.0275 1.0000 Uani . . . . . . C24 C 0.2225(4) -0.0910(3) 0.0704(2) 0.0232 1.0000 Uani . . . . . . C25 C 0.3720(4) -0.0102(3) -0.0532(3) 0.0261 1.0000 Uani . . . . . . C26 C 0.4087(4) 0.0753(3) -0.1205(2) 0.0250 1.0000 Uani . . . . . . C27 C 0.3281(4) 0.1781(3) -0.1363(2) 0.0252 1.0000 Uani . . . . . . C28 C 0.1300(4) 0.3210(3) -0.1063(2) 0.0239 1.0000 Uani . . . . . . C29 C 0.1714(5) 0.4033(3) -0.1751(3) 0.0304 1.0000 Uani . . . . . . C30 C 0.0878(5) 0.5053(4) -0.1848(3) 0.0324 1.0000 Uani . . . . . . C31 C -0.0401(5) 0.5278(3) -0.1277(3) 0.0338 1.0000 Uani . . . . . . C32 C -0.0830(5) 0.4475(3) -0.0600(3) 0.0300 1.0000 Uani . . . . . . C33 C 0.0012(4) 0.3427(3) -0.0479(2) 0.0213 1.0000 Uani . . . . . . C34 C -0.1513(4) 0.2613(3) 0.0736(3) 0.0290 1.0000 Uani . . . . . . C35 C -0.1911(4) 0.1751(4) 0.1386(3) 0.0309 1.0000 Uani . . . . . . C36 C -0.1125(4) 0.0706(3) 0.1520(3) 0.0254 1.0000 Uani . . . . . . C37 C 0.4441(7) 0.3789(4) 0.0993(4) 0.0945 1.0000 Uani D U . . . . C38 C 0.5120(11) 0.4507(7) 0.1137(6) 0.0602 0.5000 Uani D U . . 2 . C39 C 0.5469(6) 0.5329(4) 0.0505(3) 0.0655 1.0000 Uani D U . . . . C40 C 0.5820(11) 0.6159(6) -0.0141(5) 0.0543 0.5000 Uani D U . . 1 . C41 C 0.4787(9) 0.4621(5) 0.03475(17) 0.0545 0.5000 Uani D U . . 1 . C42 C 0.9490(6) -0.0267(5) 0.6398(4) 0.0688 1.0000 Uani D U . . . . C43 C 1.0008(9) 0.0597(5) 0.5924(3) 0.0459 0.5000 Uani D U . . 3 . C44 C 1.0369(5) 0.0766(3) 0.5021(3) 0.0456 1.0000 Uani D U . . . . C45 C 1.0709(10) 0.0926(8) 0.4117(3) 0.0535 0.5000 Uani D U . . 4 . C46 C 0.9801(9) -0.0078(5) 0.5490(4) 0.0387 0.5000 Uani D U . . 4 . H21 H 0.3044 0.2115 0.2799 0.0317 1.0000 Uiso R . . . . . H31 H 0.4673 0.0546 0.2572 0.0371 1.0000 Uiso R . . . . . H41 H 0.6564 -0.0294 0.3502 0.0340 1.0000 Uiso R . . . . . H51 H 0.6773 0.0351 0.4719 0.0302 1.0000 Uiso R . . . . . H71 H 0.6608 0.1032 0.5809 0.0277 1.0000 Uiso R . . . . . H81 H 0.6860 0.1813 0.6895 0.0310 1.0000 Uiso R . . . . . H91 H 0.5772 0.3520 0.6944 0.0300 1.0000 Uiso R . . . . . H111 H 0.4992 0.5094 0.7024 0.0321 1.0000 Uiso R . . . . . H121 H 0.3669 0.6802 0.7076 0.0371 1.0000 Uiso R . . . . . H131 H 0.1739 0.7639 0.6194 0.0357 1.0000 Uiso R . . . . . H141 H 0.1105 0.6801 0.5210 0.0323 1.0000 Uiso R . . . . . H161 H 0.0873 0.5926 0.4355 0.0269 1.0000 Uiso R . . . . . H171 H 0.0402 0.5039 0.3388 0.0294 1.0000 Uiso R . . . . . H181 H 0.1789 0.3452 0.3167 0.0262 1.0000 Uiso R . . . . . H201 H -0.0459 -0.1353 0.2289 0.0323 1.0000 Uiso R . . . . . H211 H 0.0937 -0.3113 0.2446 0.0392 1.0000 Uiso R . . . . . H221 H 0.3124 -0.3466 0.1547 0.0389 1.0000 Uiso R . . . . . H231 H 0.3949 -0.2105 0.0465 0.0343 1.0000 Uiso R . . . . . H251 H 0.4345 -0.0770 -0.0487 0.0315 1.0000 Uiso R . . . . . H261 H 0.4961 0.0611 -0.1582 0.0305 1.0000 Uiso R . . . . . H271 H 0.3612 0.2281 -0.1859 0.0298 1.0000 Uiso R . . . . . H291 H 0.2557 0.3894 -0.2148 0.0368 1.0000 Uiso R . . . . . H301 H 0.1147 0.5608 -0.2313 0.0382 1.0000 Uiso R . . . . . H311 H -0.0959 0.5976 -0.1345 0.0402 1.0000 Uiso R . . . . . H321 H -0.1684 0.4626 -0.0216 0.0351 1.0000 Uiso R . . . . . H341 H -0.2140 0.3288 0.0692 0.0353 1.0000 Uiso R . . . . . H351 H -0.2778 0.1911 0.1763 0.0380 1.0000 Uiso R . . . . . H361 H -0.1520 0.0182 0.1954 0.0315 1.0000 Uiso R . . . . . H371 H 0.3976 0.3392 0.0736 0.1120 0.5000 Uiso R . . . 1 . H372 H 0.5312 0.3341 0.1241 0.1120 0.5000 Uiso R . . . 1 . H373 H 0.3783 0.4054 0.1458 0.1120 0.5000 Uiso R . . . 1 . H374 H 0.4137 0.3270 0.1494 0.1133 0.5000 Uiso . . . . 2 . H381 H 0.5386 0.4412 0.1730 0.0755 0.5000 Uiso R . . . 2 . H391 H 0.5871 0.5850 0.0646 0.0786 0.5000 Uiso R . . . . . H392 H 0.5717 0.5241 0.1101 0.0786 0.5000 Uiso R . . . . . H401 H 0.6221 0.6682 -0.0003 0.0637 0.5000 Uiso R . . . 1 . H421 H 0.9100 -0.0887 0.6612 0.0824 0.5000 Uiso . . . . 4 . H422 H 1.0364 -0.0358 0.6680 0.0824 0.5000 Uiso . . . . 4 . H423 H 0.8778 0.0330 0.6553 0.0824 0.5000 Uiso . . . . 4 . H424 H 0.9273 -0.0412 0.7037 0.0831 0.5000 Uiso R . . . 3 . H431 H 1.0128 0.1098 0.6233 0.0570 0.5000 Uiso R . . . 3 . H441 H 1.0531 0.1257 0.5327 0.0548 0.5000 Uiso R . . . . . H442 H 1.0751 0.1378 0.4720 0.0548 0.5000 Uiso R . . . . . H451 H 1.1111 0.1528 0.3816 0.0669 0.5000 Uiso R . . . 4 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0109(3) 0.0131(3) 0.0149(3) -0.0052(2) -0.0046(2) -0.0010(2) Co2 0.0133(3) 0.0206(3) 0.0118(3) -0.0077(2) -0.0025(2) -0.0042(2) Cl1 0.0228(4) 0.0216(4) 0.0271(4) -0.0032(3) -0.0008(3) -0.0038(3) Cl26 0.0254(4) 0.0331(5) 0.0266(4) -0.0157(4) -0.0089(3) -0.0033(3) N1 0.0165(14) 0.0194(14) 0.0210(14) -0.0056(12) -0.0051(11) -0.0041(11) N2 0.0185(15) 0.0238(15) 0.0194(14) -0.0067(12) -0.0037(12) -0.0019(12) N3 0.0169(14) 0.0216(14) 0.0213(14) -0.0071(12) -0.0061(11) -0.0036(11) N4 0.0201(15) 0.0171(13) 0.0197(14) -0.0028(11) -0.0042(11) -0.0058(11) N5 0.0196(15) 0.0304(16) 0.0170(14) -0.0097(12) -0.0025(11) -0.0065(12) N6 0.0182(15) 0.0270(16) 0.0194(14) -0.0108(12) -0.0021(11) -0.0063(12) N7 0.0202(15) 0.0256(15) 0.0193(14) -0.0084(12) -0.0044(12) -0.0066(12) N8 0.0198(15) 0.0235(15) 0.0191(14) -0.0084(12) -0.0050(12) -0.0016(12) C1 0.0250(18) 0.0224(17) 0.0175(16) -0.0041(14) 0.0010(14) -0.0094(14) C2 0.036(2) 0.0245(18) 0.0201(17) -0.0051(15) -0.0059(15) -0.0099(16) C3 0.047(2) 0.030(2) 0.0212(18) -0.0108(16) -0.0002(17) -0.0144(18) C4 0.036(2) 0.0231(19) 0.0253(18) -0.0097(16) 0.0012(16) -0.0078(16) C5 0.0276(19) 0.0195(17) 0.0234(17) -0.0054(14) 0.0031(14) -0.0075(14) C6 0.0214(17) 0.0174(16) 0.0247(17) -0.0044(14) -0.0005(14) -0.0064(13) C7 0.0210(18) 0.0205(17) 0.0250(17) -0.0048(14) -0.0050(14) 0.0018(14) C8 0.0262(19) 0.029(2) 0.0236(18) -0.0069(15) -0.0105(15) -0.0011(15) C9 0.0227(18) 0.0295(19) 0.0235(17) -0.0098(15) -0.0055(14) -0.0051(15) C10 0.0216(18) 0.0239(18) 0.0223(17) -0.0048(15) 0.0008(14) -0.0069(14) C11 0.0246(19) 0.030(2) 0.0282(19) -0.0113(16) 0.0027(15) -0.0102(16) C12 0.040(2) 0.029(2) 0.035(2) -0.0180(18) 0.0000(18) -0.0149(17) C13 0.027(2) 0.0190(18) 0.042(2) -0.0099(17) 0.0091(17) -0.0059(15) C14 0.0246(19) 0.0226(19) 0.036(2) -0.0096(16) 0.0032(16) -0.0030(15) C15 0.0176(16) 0.0196(17) 0.0260(17) -0.0082(14) -0.0004(14) -0.0066(13) C16 0.0205(17) 0.0222(17) 0.0234(17) -0.0040(14) -0.0059(14) -0.0025(14) C17 0.0198(17) 0.0256(18) 0.0275(18) 0.0001(15) -0.0137(14) -0.0041(14) C18 0.0193(17) 0.0258(18) 0.0240(17) -0.0025(15) -0.0086(14) -0.0090(14) C19 0.0249(18) 0.035(2) 0.0185(16) -0.0097(15) -0.0065(14) -0.0110(15) C20 0.031(2) 0.029(2) 0.0214(17) -0.0033(15) -0.0104(15) -0.0123(16) C21 0.042(2) 0.036(2) 0.0244(19) -0.0052(17) -0.0139(17) -0.0135(18) C22 0.049(3) 0.0254(19) 0.0233(18) -0.0088(16) -0.0153(18) -0.0051(17) C23 0.031(2) 0.029(2) 0.0272(19) -0.0146(16) -0.0084(16) -0.0036(16) C24 0.0242(18) 0.031(2) 0.0193(16) -0.0116(15) -0.0084(14) -0.0054(15) C25 0.0270(19) 0.0287(19) 0.0281(19) -0.0170(16) -0.0074(15) -0.0025(15) C26 0.0252(18) 0.034(2) 0.0194(17) -0.0150(16) 0.0053(14) -0.0089(15) C27 0.0252(19) 0.035(2) 0.0185(17) -0.0109(15) 0.0028(14) -0.0109(16) C28 0.0257(19) 0.031(2) 0.0170(16) -0.0094(15) -0.0066(14) -0.0041(15) C29 0.031(2) 0.037(2) 0.0211(18) -0.0018(16) -0.0052(16) -0.0062(17) C30 0.034(2) 0.039(2) 0.0219(18) 0.0004(17) -0.0088(16) -0.0084(18) C31 0.039(2) 0.028(2) 0.031(2) -0.0022(17) -0.0145(18) -0.0005(17) C32 0.028(2) 0.034(2) 0.0269(19) -0.0085(17) -0.0085(16) 0.0007(16) C33 0.0231(18) 0.0234(18) 0.0200(16) -0.0107(14) -0.0083(14) -0.0001(14) C34 0.024(2) 0.032(2) 0.033(2) -0.0137(17) 0.0001(16) -0.0053(16) C35 0.0185(18) 0.040(2) 0.031(2) -0.0116(18) 0.0084(15) -0.0031(16) C36 0.0202(18) 0.036(2) 0.0220(18) -0.0100(16) 0.0010(14) -0.0084(15) C37 0.040(3) 0.063(4) 0.147(7) 0.011(4) -0.007(4) 0.012(3) C38 0.052(5) 0.045(5) 0.067(6) -0.017(5) -0.001(5) 0.020(4) C39 0.042(3) 0.044(3) 0.110(5) -0.028(3) -0.024(3) 0.013(2) C40 0.039(5) 0.043(5) 0.069(6) -0.010(5) 0.010(5) 0.000(4) C41 0.032(4) 0.029(4) 0.091(6) -0.004(4) -0.003(4) 0.002(3) C42 0.039(3) 0.060(3) 0.105(5) -0.020(3) -0.029(3) 0.010(3) C43 0.035(4) 0.045(5) 0.064(5) -0.036(4) -0.024(4) 0.015(4) C44 0.030(2) 0.030(2) 0.085(4) -0.022(2) -0.032(2) 0.0043(17) C45 0.024(4) 0.044(4) 0.082(6) 0.004(4) -0.019(4) 0.000(3) C46 0.028(4) 0.031(4) 0.060(5) -0.014(4) -0.020(4) 0.002(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 3.633(11) loop_ _oxford_twin_element_scale_factors 0.755(2) 0.245(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 . Cl1 . 2.2314(11) yes Co1 . N1 . 1.887(3) yes Co1 . N2 . 1.888(3) yes Co1 . N3 . 1.893(3) yes Co1 . N4 . 1.881(3) yes Co2 . Cl26 . 2.2292(10) yes Co2 . N5 . 1.885(3) yes Co2 . N6 . 1.895(3) yes Co2 . N7 . 1.899(3) yes Co2 . N8 . 1.890(3) yes N1 . C1 . 1.403(5) yes N1 . C18 . 1.330(5) yes N2 . C6 . 1.402(5) yes N2 . C7 . 1.332(5) yes N3 . C9 . 1.330(5) yes N3 . C10 . 1.408(5) yes N4 . C15 . 1.395(5) yes N4 . C16 . 1.350(5) yes N5 . C19 . 1.399(5) yes N5 . C36 . 1.331(5) yes N6 . C24 . 1.398(5) yes N6 . C25 . 1.330(5) yes N7 . C27 . 1.328(5) yes N7 . C28 . 1.414(5) yes N8 . C33 . 1.399(5) yes N8 . C34 . 1.330(5) yes C1 . C2 . 1.394(5) yes C1 . C6 . 1.403(5) yes C2 . C3 . 1.384(6) yes C2 . H21 . 0.960 no C3 . C4 . 1.399(6) yes C3 . H31 . 0.935 no C4 . C5 . 1.377(5) yes C4 . H41 . 0.935 no C5 . C6 . 1.403(5) yes C5 . H51 . 0.928 no C7 . C8 . 1.382(5) yes C7 . H71 . 0.930 no C8 . C9 . 1.389(5) yes C8 . H81 . 0.934 no C9 . H91 . 0.932 no C10 . C11 . 1.385(5) yes C10 . C15 . 1.416(5) yes C11 . C12 . 1.381(6) yes C11 . H111 . 0.939 no C12 . C13 . 1.390(6) yes C12 . H121 . 0.925 no C13 . C14 . 1.380(6) yes C13 . H131 . 0.935 no C14 . C15 . 1.403(5) yes C14 . H141 . 0.944 no C16 . C17 . 1.388(5) yes C16 . H161 . 0.934 no C17 . C18 . 1.382(5) yes C17 . H171 . 0.937 no C18 . H181 . 0.945 no C19 . C20 . 1.401(6) yes C19 . C24 . 1.420(5) yes C20 . C21 . 1.384(6) yes C20 . H201 . 0.936 no C21 . C22 . 1.395(7) yes C21 . H211 . 0.942 no C22 . C23 . 1.382(6) yes C22 . H221 . 0.940 no C23 . C24 . 1.390(5) yes C23 . H231 . 0.933 no C25 . C26 . 1.399(6) yes C25 . H251 . 0.927 no C26 . C27 . 1.367(6) yes C26 . H261 . 0.937 no C27 . H271 . 0.940 no C28 . C29 . 1.396(6) yes C28 . C33 . 1.407(5) yes C29 . C30 . 1.371(6) yes C29 . H291 . 0.933 no C30 . C31 . 1.391(7) yes C30 . H301 . 0.938 no C31 . C32 . 1.376(6) yes C31 . H311 . 0.934 no C32 . C33 . 1.400(5) yes C32 . H321 . 0.931 no C34 . C35 . 1.397(6) yes C34 . H341 . 0.936 no C35 . C36 . 1.380(6) yes C35 . H351 . 0.936 no C36 . H361 . 0.937 no C37 . C40 2_665 1.3503(7) yes C37 . C41 . 1.3504(10) yes C37 . H371 . 0.950 no C37 . H372 . 0.950 no C37 . H373 . 0.950 no C38 . C39 . 1.332(9) yes C38 . H381 . 0.950 no C39 . C41 2_665 1.3501(7) yes C39 . C40 . 1.3500(10) yes C39 . C41 . 1.3497(10) yes C39 . H391 . 0.950 no C39 . H392 . 0.950 no C40 . C41 2_665 1.423(8) yes C40 . H401 . 0.950 no C41 . C41 2_665 1.3503(7) yes C42 . C43 . 1.3504(10) yes C42 . H424 . 0.950 no C43 . C44 . 1.3495(10) yes C43 . H431 . 0.950 no C44 . H441 . 0.950 no C44 . H442 . 0.950 no C45 . C46 2_756 1.300(10) yes C45 . H451 . 0.950 no C46 . C46 2_756 1.467(10) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Co1 . N1 . 97.37(10) yes Cl1 . Co1 . N2 . 97.21(10) yes N1 . Co1 . N2 . 84.37(13) yes Cl1 . Co1 . N3 . 96.62(10) yes N1 . Co1 . N3 . 166.02(13) yes N2 . Co1 . N3 . 93.87(13) yes Cl1 . Co1 . N4 . 96.27(10) yes N1 . Co1 . N4 . 94.45(13) yes N2 . Co1 . N4 . 166.51(13) yes N3 . Co1 . N4 . 84.03(13) yes Cl26 . Co2 . N5 . 96.77(9) yes Cl26 . Co2 . N6 . 95.92(9) yes N5 . Co2 . N6 . 83.74(13) yes Cl26 . Co2 . N7 . 97.41(9) yes N5 . Co2 . N7 . 165.82(13) yes N6 . Co2 . N7 . 94.61(13) yes Cl26 . Co2 . N8 . 96.46(9) yes N5 . Co2 . N8 . 94.47(14) yes N6 . Co2 . N8 . 167.62(13) yes N7 . Co2 . N8 . 84.12(13) yes Co1 . N1 . C1 . 114.1(2) yes Co1 . N1 . C18 . 125.3(3) yes C1 . N1 . C18 . 120.6(3) yes Co1 . N2 . C6 . 113.9(2) yes Co1 . N2 . C7 . 125.4(3) yes C6 . N2 . C7 . 120.5(3) yes Co1 . N3 . C9 . 124.8(3) yes Co1 . N3 . C10 . 114.4(2) yes C9 . N3 . C10 . 120.5(3) yes Co1 . N4 . C15 . 114.4(2) yes Co1 . N4 . C16 . 125.3(3) yes C15 . N4 . C16 . 119.9(3) yes Co2 . N5 . C19 . 114.5(2) yes Co2 . N5 . C36 . 126.1(3) yes C19 . N5 . C36 . 119.2(3) yes Co2 . N6 . C24 . 114.2(2) yes Co2 . N6 . C25 . 125.1(3) yes C24 . N6 . C25 . 120.4(3) yes Co2 . N7 . C27 . 125.1(3) yes Co2 . N7 . C28 . 113.5(2) yes C27 . N7 . C28 . 121.2(3) yes Co2 . N8 . C33 . 114.0(2) yes Co2 . N8 . C34 . 125.5(3) yes C33 . N8 . C34 . 120.3(3) yes N1 . C1 . C2 . 126.7(3) yes N1 . C1 . C6 . 113.5(3) yes C2 . C1 . C6 . 119.6(3) yes C1 . C2 . C3 . 120.1(4) yes C1 . C2 . H21 . 119.9 no C3 . C2 . H21 . 120.0 no C2 . C3 . C4 . 120.0(3) yes C2 . C3 . H31 . 120.1 no C4 . C3 . H31 . 119.9 no C3 . C4 . C5 . 120.7(4) yes C3 . C4 . H41 . 119.3 no C5 . C4 . H41 . 119.9 no C4 . C5 . C6 . 119.4(4) yes C4 . C5 . H51 . 119.7 no C6 . C5 . H51 . 120.9 no C5 . C6 . C1 . 120.1(3) yes C5 . C6 . N2 . 125.9(3) yes C1 . C6 . N2 . 114.0(3) yes N2 . C7 . C8 . 123.8(3) yes N2 . C7 . H71 . 118.4 no C8 . C7 . H71 . 117.8 no C7 . C8 . C9 . 124.7(3) yes C7 . C8 . H81 . 117.8 no C9 . C8 . H81 . 117.6 no C8 . C9 . N3 . 124.6(3) yes C8 . C9 . H91 . 118.2 no N3 . C9 . H91 . 117.2 no N3 . C10 . C11 . 127.0(3) yes N3 . C10 . C15 . 112.6(3) yes C11 . C10 . C15 . 120.5(3) yes C10 . C11 . C12 . 119.5(4) yes C10 . C11 . H111 . 120.5 no C12 . C11 . H111 . 120.0 no C11 . C12 . C13 . 120.7(4) yes C11 . C12 . H121 . 120.3 no C13 . C12 . H121 . 119.0 no C12 . C13 . C14 . 120.7(4) yes C12 . C13 . H131 . 120.1 no C14 . C13 . H131 . 119.2 no C13 . C14 . C15 . 119.7(4) yes C13 . C14 . H141 . 120.6 no C15 . C14 . H141 . 119.7 no C10 . C15 . C14 . 119.0(3) yes C10 . C15 . N4 . 114.0(3) yes C14 . C15 . N4 . 127.0(3) yes N4 . C16 . C17 . 123.5(3) yes N4 . C16 . H161 . 117.4 no C17 . C16 . H161 . 119.1 no C16 . C17 . C18 . 125.1(3) yes C16 . C17 . H171 . 117.3 no C18 . C17 . H171 . 117.6 no C17 . C18 . N1 . 124.5(3) yes C17 . C18 . H181 . 118.4 no N1 . C18 . H181 . 117.1 no N5 . C19 . C20 . 127.2(3) yes N5 . C19 . C24 . 113.3(3) yes C20 . C19 . C24 . 119.5(4) yes C19 . C20 . C21 . 119.7(4) yes C19 . C20 . H201 . 118.8 no C21 . C20 . H201 . 121.5 no C20 . C21 . C22 . 120.3(4) yes C20 . C21 . H211 . 120.5 no C22 . C21 . H211 . 119.2 no C21 . C22 . C23 . 120.7(4) yes C21 . C22 . H221 . 118.9 no C23 . C22 . H221 . 120.4 no C22 . C23 . C24 . 119.9(4) yes C22 . C23 . H231 . 119.7 no C24 . C23 . H231 . 120.5 no C19 . C24 . N6 . 113.2(3) yes C19 . C24 . C23 . 119.8(4) yes N6 . C24 . C23 . 127.0(3) yes N6 . C25 . C26 . 123.8(4) yes N6 . C25 . H251 . 117.6 no C26 . C25 . H251 . 118.6 no C25 . C26 . C27 . 125.7(3) yes C25 . C26 . H261 . 117.3 no C27 . C26 . H261 . 117.0 no C26 . C27 . N7 . 124.6(4) yes C26 . C27 . H271 . 118.0 no N7 . C27 . H271 . 117.5 no N7 . C28 . C29 . 126.8(4) yes N7 . C28 . C33 . 113.3(3) yes C29 . C28 . C33 . 119.9(4) yes C28 . C29 . C30 . 120.1(4) yes C28 . C29 . H291 . 120.4 no C30 . C29 . H291 . 119.5 no C29 . C30 . C31 . 120.6(4) yes C29 . C30 . H301 . 120.4 no C31 . C30 . H301 . 118.9 no C30 . C31 . C32 . 120.0(4) yes C30 . C31 . H311 . 120.1 no C32 . C31 . H311 . 119.9 no C31 . C32 . C33 . 120.6(4) yes C31 . C32 . H321 . 120.0 no C33 . C32 . H321 . 119.5 no C28 . C33 . C32 . 118.8(4) yes C28 . C33 . N8 . 114.1(3) yes C32 . C33 . N8 . 127.1(3) yes N8 . C34 . C35 . 123.8(4) yes N8 . C34 . H341 . 117.6 no C35 . C34 . H341 . 118.6 no C34 . C35 . C36 . 125.5(4) yes C34 . C35 . H351 . 116.1 no C36 . C35 . H351 . 118.3 no C35 . C36 . N5 . 123.7(4) yes C35 . C36 . H361 . 118.5 no N5 . C36 . H361 . 117.8 no C40 2_665 C37 . C41 . 63.6(4) yes C40 2_665 C37 . H371 . 46.2 no C41 . C37 . H371 . 109.6 no C40 2_665 C37 . H372 . 120.9 no C41 . C37 . H372 . 109.9 no H371 . C37 . H372 . 109.5 no C40 2_665 C37 . H373 . 128.7 no C41 . C37 . H373 . 109.0 no H371 . C37 . H373 . 109.5 no H372 . C37 . H373 . 109.5 no C37 . C38 . C39 . 124.9(6) yes C37 . C38 . H381 . 117.7 no C39 . C38 . H381 . 117.4 no C41 2_665 C39 . C40 . 63.6(4) yes C41 2_665 C39 . C41 . 60.02(5) yes C40 . C39 . C41 . 123.4(4) yes C41 2_665 C39 . H391 . 122.0 no C40 . C39 . H391 . 58.4 no C41 . C39 . H391 . 175.0 no C41 2_665 C39 . H392 . 174.9 no C40 . C39 . H392 . 118.0 no C41 . C39 . H392 . 118.5 no H391 . C39 . H392 . 59.9 no C41 2_665 C40 . C37 2_665 58.2(2) yes C41 2_665 C40 . C39 . 58.2(2) yes C37 2_665 C40 . C39 . 116.4(4) yes C41 2_665 C40 . H401 . 179.7 no C37 2_665 C40 . H401 . 121.8 no C39 . C40 . H401 . 121.8 no C40 2_665 C41 . C37 . 58.2(2) yes C40 2_665 C41 . C41 2_665 118.0(2) yes C37 . C41 . C41 2_665 174.0(10) yes C40 2_665 C41 . C39 2_665 58.2(2) yes C37 . C41 . C39 2_665 116.4(4) yes C41 2_665 C41 . C39 2_665 59.98(6) yes C40 2_665 C41 . C39 . 175.3(8) yes C37 . C41 . C39 . 123.4(4) yes C41 2_665 C41 . C39 . 60.00(5) yes C39 2_665 C41 . C39 . 119.98(5) yes C43 . C42 . H424 . 122.6 no C42 . C43 . C44 . 121.7(4) yes C42 . C43 . H431 . 119.3 no C44 . C43 . H431 . 119.0 no C43 . C44 . H441 . 61.7 no C43 . C44 . H442 . 118.6 no H441 . C44 . H442 . 56.9 no C42 2_756 C45 . C44 . 124.1(7) yes C42 2_756 C45 . C46 2_756 60.3(5) yes C44 . C45 . C46 2_756 63.9(4) yes C42 2_756 C45 . H451 . 118.1 no C44 . C45 . H451 . 117.8 no C46 2_756 C45 . H451 . 177.7 no C46 2_756 C46 . C44 2_756 56.1(4) yes C46 2_756 C46 . C44 . 59.5(3) yes C44 2_756 C46 . C44 . 115.6(4) yes C46 2_756 C46 . C42 . 177.0(10) yes C44 2_756 C46 . C42 . 122.7(4) yes C44 . C46 . C42 . 121.6(4) yes C46 2_756 C46 . C45 2_756 115.9(6) yes C44 2_756 C46 . C45 2_756 59.8(3) yes C44 . C46 . C45 2_756 175.2(6) yes C42 . C46 . C45 2_756 62.9(4) yes _iucr_refine_instruction_details_constraints ; # # Punched on 27/04/11 at 18:00:14 # #LIST 12 BLOCK SCALE X'S, U'S SUMFIX ELEMENT SCALES RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 27,X'S) H ( 271,X'S) RIDE C ( 29,X'S) H ( 291,X'S) RIDE C ( 30,X'S) H ( 301,X'S) RIDE C ( 31,X'S) H ( 311,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 36,X'S) H ( 361,X'S) RIDE C ( 37,X'S) H ( 371,X'S) H ( 372,X'S) H ( 373,X'S) RIDE C ( 38,X'S) H ( 381,X'S) RIDE C ( 39,X'S) H ( 391,X'S) H ( 392,X'S) RIDE C ( 40,X'S) H ( 401,X'S) RIDE C ( 42,X'S) H ( 424,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) H ( 442,X'S) RIDE C ( 45,X'S) H ( 451,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 27/04/11 at 18:00:14 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) DIST 1.35 , 0.001 = C(37) TO C(40,-1,1,1,1) DIST 1.35 , 0.001 = C(41) TO C(39,-1,1,1,1) DIST 1.35 , 0.001 = C(41) TO C(41,-1,1,1,1) DIST 1.35 , 0.001 = C(37) TO C(41) DIST 1.35 , 0.001 = C(39) TO C(41) DIST 1.35 , 0.001 = C(37) TO C(38) DIST 1.35 , 0.001 = C(39) TO C(40) ANGLE 120.000000 , 1.0000 = C(39) TO C(41) TO C(37) ANGLE 120.000000 , 1.0000 = C(41) TO C(39) TO C(40) ANGLE 120.000000 , 1.0000 = C(37) TO C(38) TO C(39) ANGLE 120.000000 , 1.0000 = C(38) TO C(39) TO C(41,-1,1,1,1) ANGLE 120.000000 , 1.0000 = C(39) TO C(41) TO C(39,-1,1,1,1) ANGLE 180.000000 , 1.0000 = C(38) TO C(39) TO C(40) U(IJ)'S 0.0, 0.01000 = C(38) TO C(40) U(IJ)'S 0.0, 0.01000 = C(38) TO C(41) U(IJ)'S 0.0, 0.010000 = C(39) TO C(37) DIST 1.35 , 0.001 = C(37) TO C(40,-1,1,1,1) DIST 1.35 , 0.001 = C(41) TO C(39,-1,1,1,1) DIST 1.35 , 0.001 = C(41) TO C(41,-1,1,1,1) DIST 1.35 , 0.001 = C(42) TO C(43) DIST 1.35 , 0.001 = C(42) TO C(46) DIST 1.35 , 0.001 = C(43) TO C(44) DIST 1.35 , 0.001 = C(44) TO C(45) DIST 1.35 , 0.001 = C(44) TO C(46) ANGLE 120.000000 , 1.0000 = C(42) TO C(43) TO C(44) ANGLE 120.000000 , 1.0000 = C(42) TO C(46) TO C(44) ANGLE 120.000000 , 1.0000 = C(45) TO C(44) TO C(46) ANGLE 120.000000 , 1.0000 = C(43) TO C(44) TO C(46,-1,1,2,0,1) ANGLE 120.000000 , 1.0000 = C(44) TO C(46) TO C(44,-1,1,2,0,1) ANGLE 180.000000 , 1.0000 = C(43) TO C(44) TO C(45) U(IJ)'S 0.0, 0.010000 = C(46) TO C(45) U(IJ)'S 0.0, 0.010000 = C(44) TO C(43) U(IJ)'S 0.0, 0.010000 = C(42) TO C(45) U(IJ)'S 0.0, 0.010000 = C(44) TO C(39) U(IJ)'S 0.0, 0.010000 = C(46) TO C(41) END ; #============================================================================== data___Cu_dbtaa-3 _database_code_depnum_ccdc_archive 'CCDC 882249' #TrackingRef '- Cu_dbtaa.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C18 H14 Cu N4 ' _chemical_formula_moiety 'C18 H14 Cu N4 ' _chemical_formula_weight 349.88 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 19.416(5) _cell_length_b 5.1511(12) _cell_length_c 14.878(4) _cell_angle_alpha 90.0000 _cell_angle_beta 112.394(3) _cell_angle_gamma 90.0000 _cell_volume 1375.8(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3454 _cell_measurement_theta_min 4.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 150.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716.00 _exptl_absorpt_coefficient_mu 1.592 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.866 _exptl_absorpt_correction_T_max 0.938 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 10218 _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_ambient_temperature 150.1 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3140 _reflns_number_gt 2679 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.1050 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 3140 _refine_ls_number_parameters 212 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0550P)^2^+0.9865P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.72 _refine_diff_density_min -0.77 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Cu(1) Cu 0.5000 0.5000 0.5000 0.01251(12) Uani 1.00 2 d S . . Cu(2) Cu 0.0000 0.5000 0.5000 0.01152(12) Uani 1.00 2 d S . . N(1) N 0.40471(9) 0.4078(3) 0.50279(12) 0.0154(3) Uani 1.00 1 d . . . N(2) N 0.49925(9) 0.2369(3) 0.40756(11) 0.0153(3) Uani 1.00 1 d . . . N(3) N -0.00267(9) 0.7662(3) 0.58966(11) 0.0139(3) Uani 1.00 1 d . . . N(4) N -0.09487(9) 0.5880(3) 0.40032(11) 0.0141(3) Uani 1.00 1 d . . . C(1) C 0.38355(11) 0.5674(3) 0.56519(13) 0.0150(3) Uani 1.00 1 d . . . C(2) C 0.31718(12) 0.5492(4) 0.58116(15) 0.0185(4) Uani 1.00 1 d . . . C(3) C 0.30242(11) 0.7240(4) 0.64259(14) 0.0198(4) Uani 1.00 1 d . . . C(4) C 0.35330(12) 0.9178(4) 0.68895(15) 0.0205(4) Uani 1.00 1 d . . . C(5) C 0.41960(12) 0.9378(4) 0.67432(15) 0.0189(4) Uani 1.00 1 d . . . C(6) C 0.43573(10) 0.7639(3) 0.61319(13) 0.0149(3) Uani 1.00 1 d . . . C(7) C 0.44496(11) 0.0665(4) 0.36922(14) 0.0175(3) Uani 1.00 1 d . . . C(8) C 0.38019(11) 0.0559(4) 0.38860(15) 0.0188(4) Uani 1.00 1 d . . . C(9) C 0.36225(10) 0.2162(4) 0.45155(14) 0.0176(3) Uani 1.00 1 d . . . C(10) C 0.06159(10) 0.7699(3) 0.67561(13) 0.0142(3) Uani 1.00 1 d . . . C(11) C 0.07689(12) 0.9480(4) 0.75145(15) 0.0171(3) Uani 1.00 1 d . . . C(12) C 0.14243(12) 0.9303(4) 0.83329(15) 0.0187(4) Uani 1.00 1 d . . . C(13) C 0.19346(11) 0.7350(4) 0.84013(14) 0.0179(3) Uani 1.00 1 d . . . C(14) C 0.17928(11) 0.5558(4) 0.76559(15) 0.0170(3) Uani 1.00 1 d . . . C(15) C 0.11422(11) 0.5730(3) 0.68195(13) 0.0138(3) Uani 1.00 1 d . . . C(16) C -0.13911(10) 0.7758(3) 0.40822(14) 0.0161(3) Uani 1.00 1 d . . . C(17) C -0.12296(11) 0.9364(4) 0.48869(15) 0.0175(3) Uani 1.00 1 d . . . C(18) C -0.05833(11) 0.9303(4) 0.57328(14) 0.0159(3) Uani 1.00 1 d . . . H(1) H 0.2821 0.4169 0.5499 0.022 Uiso 1.00 1 c R . . H(2) H 0.2572 0.7109 0.6530 0.024 Uiso 1.00 1 c R . . H(3) H 0.3427 1.0369 0.7307 0.025 Uiso 1.00 1 c R . . H(4) H 0.4542 1.0709 0.7062 0.023 Uiso 1.00 1 c R . . H(5) H 0.4505 -0.0578 0.3253 0.021 Uiso 1.00 1 c R . . H(6) H 0.3448 -0.0738 0.3555 0.023 Uiso 1.00 1 c R . . H(7) H 0.3162 0.1864 0.4584 0.021 Uiso 1.00 1 c R . . H(8) H 0.0422 1.0823 0.7471 0.020 Uiso 1.00 1 c R . . H(9) H 0.1523 1.0521 0.8847 0.022 Uiso 1.00 1 c R . . H(10) H 0.2383 0.7239 0.8961 0.021 Uiso 1.00 1 c R . . H(11) H 0.2140 0.4206 0.7714 0.020 Uiso 1.00 1 c R . . H(12) H -0.1851 0.8022 0.3550 0.019 Uiso 1.00 1 c R . . H(13) H -0.1594 1.0626 0.4860 0.021 Uiso 1.00 1 c R . . H(14) H -0.0542 1.0534 0.6226 0.019 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0124(2) 0.0132(2) 0.0125(2) -0.00255(11) 0.00539(15) -0.00141(11) Cu(2) 0.0119(2) 0.0115(2) 0.01094(19) 0.00229(10) 0.00405(15) 0.00021(10) N(1) 0.0144(7) 0.0164(8) 0.0151(7) -0.0021(6) 0.0053(6) -0.0003(6) N(2) 0.0149(7) 0.0166(7) 0.0146(7) -0.0010(6) 0.0059(6) 0.0003(6) N(3) 0.0141(7) 0.0146(7) 0.0135(7) 0.0009(6) 0.0058(6) 0.0007(6) N(4) 0.0141(7) 0.0149(7) 0.0130(7) 0.0016(6) 0.0049(6) 0.0003(6) C(1) 0.0166(9) 0.0155(8) 0.0128(8) 0.0023(7) 0.0056(7) 0.0030(7) C(2) 0.0161(9) 0.0218(9) 0.0179(9) 0.0001(7) 0.0069(8) 0.0037(8) C(3) 0.0180(9) 0.0241(10) 0.0194(9) 0.0053(8) 0.0098(7) 0.0070(8) C(4) 0.0241(10) 0.0216(10) 0.0172(9) 0.0066(8) 0.0095(8) 0.0030(8) C(5) 0.0215(10) 0.0186(8) 0.0154(9) 0.0008(8) 0.0058(8) 0.0003(8) C(6) 0.0168(8) 0.0158(8) 0.0122(8) 0.0004(7) 0.0057(6) 0.0037(7) C(7) 0.0205(10) 0.0172(8) 0.0138(8) -0.0028(8) 0.0056(7) -0.0014(7) C(8) 0.0174(10) 0.0198(9) 0.0166(9) -0.0054(8) 0.0035(7) -0.0022(8) C(9) 0.0146(8) 0.0193(9) 0.0178(9) -0.0032(7) 0.0050(7) -0.0001(7) C(10) 0.0148(8) 0.0148(8) 0.0140(8) -0.0009(7) 0.0068(7) 0.0024(7) C(11) 0.0198(10) 0.0164(8) 0.0167(9) 0.0014(7) 0.0090(8) 0.0003(7) C(12) 0.0210(10) 0.0187(9) 0.0179(9) -0.0024(8) 0.0090(8) -0.0023(8) C(13) 0.0145(8) 0.0215(9) 0.0156(8) -0.0010(7) 0.0035(7) 0.0015(7) C(14) 0.0153(9) 0.0190(8) 0.0168(9) 0.0028(7) 0.0062(7) 0.0006(7) C(15) 0.0179(9) 0.0129(8) 0.0129(8) -0.0014(7) 0.0083(7) 0.0008(7) C(16) 0.0143(8) 0.0183(9) 0.0160(8) 0.0035(7) 0.0060(7) 0.0038(7) C(17) 0.0164(9) 0.0172(8) 0.0193(9) 0.0059(7) 0.0073(7) 0.0006(8) C(18) 0.0196(9) 0.0142(8) 0.0159(9) 0.0020(7) 0.0091(7) 0.0001(7) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cu(1) N(1) 1.9258(18) yes . . Cu(1) N(1) 1.9258(18) yes . 3_666 Cu(1) N(2) 1.9268(16) yes . . Cu(1) N(2) 1.9268(16) yes . 3_666 Cu(2) N(3) 1.9276(16) yes . . Cu(2) N(3) 1.9276(16) yes . 3_566 Cu(2) N(4) 1.9278(13) yes . . Cu(2) N(4) 1.9278(13) yes . 3_566 N(1) C(1) 1.413(2) yes . . N(1) C(9) 1.325(2) yes . . N(2) C(6) 1.409(2) yes . 3_666 N(2) C(7) 1.323(2) yes . . N(3) C(10) 1.406(2) yes . . N(3) C(18) 1.319(2) yes . . N(4) C(15) 1.406(2) yes . 3_566 N(4) C(16) 1.328(2) yes . . C(1) C(2) 1.400(3) yes . . C(1) C(6) 1.418(2) yes . . C(2) C(3) 1.388(3) yes . . C(3) C(4) 1.389(2) yes . . C(4) C(5) 1.389(3) yes . . C(5) C(6) 1.395(3) yes . . C(7) C(8) 1.394(3) yes . . C(8) C(9) 1.389(3) yes . . C(10) C(11) 1.396(2) yes . . C(10) C(15) 1.417(2) yes . . C(11) C(12) 1.389(2) yes . . C(12) C(13) 1.388(3) yes . . C(13) C(14) 1.387(2) yes . . C(14) C(15) 1.398(2) yes . . C(16) C(17) 1.389(2) yes . . C(17) C(18) 1.399(2) yes . . C(2) H(1) 0.950 no . . C(3) H(2) 0.950 no . . C(4) H(3) 0.950 no . . C(5) H(4) 0.950 no . . C(7) H(5) 0.950 no . . C(8) H(6) 0.950 no . . C(9) H(7) 0.950 no . . C(11) H(8) 0.950 no . . C(12) H(9) 0.950 no . . C(13) H(10) 0.950 no . . C(14) H(11) 0.950 no . . C(16) H(12) 0.950 no . . C(17) H(13) 0.950 no . . C(18) H(14) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 N(1) Cu(1) N(1) 180.00(9) yes . . 3_666 N(1) Cu(1) N(2) 95.50(7) yes . . . N(1) Cu(1) N(2) 84.50(7) yes . . 3_666 N(1) Cu(1) N(2) 84.50(7) yes 3_666 . . N(1) Cu(1) N(2) 95.50(7) yes 3_666 . 3_666 N(2) Cu(1) N(2) 180.00(9) yes . . 3_666 N(3) Cu(2) N(3) 180.00(9) yes . . 3_566 N(3) Cu(2) N(4) 95.47(6) yes . . . N(3) Cu(2) N(4) 84.53(6) yes . . 3_566 N(3) Cu(2) N(4) 84.53(6) yes 3_566 . . N(3) Cu(2) N(4) 95.47(6) yes 3_566 . 3_566 N(4) Cu(2) N(4) 180.00(10) yes . . 3_566 Cu(1) N(1) C(1) 113.14(12) yes . . . Cu(1) N(1) C(9) 124.30(16) yes . . . C(1) N(1) C(9) 122.57(19) yes . . . Cu(1) N(2) C(6) 113.25(11) yes . . 3_666 Cu(1) N(2) C(7) 124.25(16) yes . . . C(6) N(2) C(7) 122.46(18) yes 3_666 . . Cu(2) N(3) C(10) 112.98(13) yes . . . Cu(2) N(3) C(18) 124.33(11) yes . . . C(10) N(3) C(18) 122.69(16) yes . . . Cu(2) N(4) C(15) 113.02(12) yes . . 3_566 Cu(2) N(4) C(16) 124.32(12) yes . . . C(15) N(4) C(16) 122.64(14) yes 3_566 . . N(1) C(1) C(2) 126.13(17) yes . . . N(1) C(1) C(6) 114.55(19) yes . . . C(2) C(1) C(6) 119.32(19) yes . . . C(1) C(2) C(3) 120.18(18) yes . . . C(2) C(3) C(4) 120.5(2) yes . . . C(3) C(4) C(5) 120.1(2) yes . . . C(4) C(5) C(6) 120.42(18) yes . . . N(2) C(6) C(1) 114.54(18) yes 3_666 . . N(2) C(6) C(5) 125.97(17) yes 3_666 . . C(1) C(6) C(5) 119.5(2) yes . . . N(2) C(7) C(8) 124.8(2) yes . . . C(7) C(8) C(9) 126.43(18) yes . . . N(1) C(9) C(8) 124.7(2) yes . . . N(3) C(10) C(11) 125.87(17) yes . . . N(3) C(10) C(15) 114.74(16) yes . . . C(11) C(10) C(15) 119.38(15) yes . . . C(10) C(11) C(12) 120.5(2) yes . . . C(11) C(12) C(13) 120.11(19) yes . . . C(12) C(13) C(14) 120.32(16) yes . . . C(13) C(14) C(15) 120.41(19) yes . . . N(4) C(15) C(10) 114.67(14) yes 3_566 . . N(4) C(15) C(14) 126.07(19) yes 3_566 . . C(10) C(15) C(14) 119.25(17) yes . . . N(4) C(16) C(17) 124.65(15) yes . . . C(16) C(17) C(18) 126.35(19) yes . . . N(3) C(18) C(17) 124.86(19) yes . . . C(1) C(2) H(1) 119.9 no . . . C(3) C(2) H(1) 119.9 no . . . C(2) C(3) H(2) 119.8 no . . . C(4) C(3) H(2) 119.8 no . . . C(3) C(4) H(3) 119.9 no . . . C(5) C(4) H(3) 119.9 no . . . C(4) C(5) H(4) 119.8 no . . . C(6) C(5) H(4) 119.8 no . . . N(2) C(7) H(5) 117.6 no . . . C(8) C(7) H(5) 117.6 no . . . C(7) C(8) H(6) 116.8 no . . . C(9) C(8) H(6) 116.8 no . . . N(1) C(9) H(7) 117.6 no . . . C(8) C(9) H(7) 117.6 no . . . C(10) C(11) H(8) 119.8 no . . . C(12) C(11) H(8) 119.8 no . . . C(11) C(12) H(9) 119.9 no . . . C(13) C(12) H(9) 119.9 no . . . C(12) C(13) H(10) 119.8 no . . . C(14) C(13) H(10) 119.8 no . . . C(13) C(14) H(11) 119.8 no . . . C(15) C(14) H(11) 119.8 no . . . N(4) C(16) H(12) 117.7 no . . . C(17) C(16) H(12) 117.7 no . . . C(16) C(17) H(13) 116.8 no . . . C(18) C(17) H(13) 116.8 no . . . N(3) C(18) H(14) 117.6 no . . . C(17) C(18) H(14) 117.6 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 N(1) Cu(1) N(2) C(7) -0.80(15) ? . . . . N(1) Cu(1) N(2) C(6) -178.51(12) ? . . . 3_666 N(2) Cu(1) N(1) C(1) -179.31(12) ? . . . . N(2) Cu(1) N(1) C(9) 0.28(16) ? . . . . N(1) Cu(1) N(2) C(7) -179.20(15) ? . . 3_666 3_666 N(1) Cu(1) N(2) C(6) -1.49(12) ? . . 3_666 . N(2) Cu(1) N(1) C(1) 0.69(12) ? 3_666 . . . N(2) Cu(1) N(1) C(9) -179.72(16) ? 3_666 . . . N(1) Cu(1) N(2) C(7) 179.20(15) ? 3_666 . . . N(1) Cu(1) N(2) C(6) 1.49(12) ? 3_666 . . 3_666 N(2) Cu(1) N(1) C(1) -0.69(12) ? . . 3_666 3_666 N(2) Cu(1) N(1) C(9) 179.72(16) ? . . 3_666 3_666 N(1) Cu(1) N(2) C(7) 0.80(15) ? 3_666 . 3_666 3_666 N(1) Cu(1) N(2) C(6) 178.51(12) ? 3_666 . 3_666 . N(2) Cu(1) N(1) C(1) 179.31(12) ? 3_666 . 3_666 3_666 N(2) Cu(1) N(1) C(9) -0.28(16) ? 3_666 . 3_666 3_666 N(3) Cu(2) N(4) C(16) -1.43(18) ? . . . . N(3) Cu(2) N(4) C(15) -179.67(15) ? . . . 3_566 N(4) Cu(2) N(3) C(10) -178.46(14) ? . . . . N(4) Cu(2) N(3) C(18) 1.32(19) ? . . . . N(3) Cu(2) N(4) C(16) -178.57(18) ? . . 3_566 3_566 N(3) Cu(2) N(4) C(15) -0.33(15) ? . . 3_566 . N(4) Cu(2) N(3) C(10) 1.54(14) ? 3_566 . . . N(4) Cu(2) N(3) C(18) -178.68(19) ? 3_566 . . . N(3) Cu(2) N(4) C(16) 178.57(18) ? 3_566 . . . N(3) Cu(2) N(4) C(15) 0.33(15) ? 3_566 . . 3_566 N(4) Cu(2) N(3) C(10) -1.54(14) ? . . 3_566 3_566 N(4) Cu(2) N(3) C(18) 178.68(19) ? . . 3_566 3_566 N(3) Cu(2) N(4) C(16) 1.43(18) ? 3_566 . 3_566 3_566 N(3) Cu(2) N(4) C(15) 179.67(15) ? 3_566 . 3_566 . N(4) Cu(2) N(3) C(10) 178.46(14) ? 3_566 . 3_566 3_566 N(4) Cu(2) N(3) C(18) -1.32(19) ? 3_566 . 3_566 3_566 Cu(1) N(1) C(1) C(2) 179.15(15) ? . . . . Cu(1) N(1) C(1) C(6) 0.25(19) ? . . . . Cu(1) N(1) C(9) C(8) -0.2(2) ? . . . . C(1) N(1) C(9) C(8) 179.34(18) ? . . . . C(9) N(1) C(1) C(2) -0.4(2) ? . . . . C(9) N(1) C(1) C(6) -179.35(16) ? . . . . Cu(1) N(2) C(6) C(1) -2.02(19) ? . . 3_666 3_666 Cu(1) N(2) C(6) C(5) 177.50(15) ? . . 3_666 3_666 Cu(1) N(2) C(7) C(8) 1.3(2) ? . . . . C(6) N(2) C(7) C(8) 178.82(17) ? 3_666 . . . C(7) N(2) C(6) C(1) -179.78(16) ? . . 3_666 3_666 C(7) N(2) C(6) C(5) -0.3(2) ? . . 3_666 3_666 Cu(2) N(3) C(10) C(11) 176.81(18) ? . . . . Cu(2) N(3) C(10) C(15) -2.5(2) ? . . . . Cu(2) N(3) C(18) C(17) -0.5(3) ? . . . . C(10) N(3) C(18) C(17) 179.3(2) ? . . . . C(18) N(3) C(10) C(11) -3.0(3) ? . . . . C(18) N(3) C(10) C(15) 177.7(2) ? . . . . Cu(2) N(4) C(15) C(10) 1.0(2) ? . . 3_566 3_566 Cu(2) N(4) C(15) C(14) -179.84(18) ? . . 3_566 3_566 Cu(2) N(4) C(16) C(17) 0.7(3) ? . . . . C(15) N(4) C(16) C(17) 178.8(2) ? 3_566 . . . C(16) N(4) C(15) C(10) -177.3(2) ? . . 3_566 3_566 C(16) N(4) C(15) C(14) 1.9(3) ? . . 3_566 3_566 N(1) C(1) C(2) C(3) -178.16(17) ? . . . . N(1) C(1) C(6) N(2) -1.5(2) ? . . . 3_666 N(1) C(1) C(6) C(5) 178.07(16) ? . . . . C(2) C(1) C(6) N(2) 179.53(16) ? . . . 3_666 C(2) C(1) C(6) C(5) -0.9(2) ? . . . . C(6) C(1) C(2) C(3) 0.7(2) ? . . . . C(1) C(2) C(3) C(4) -0.2(2) ? . . . . C(2) C(3) C(4) C(5) -0.2(2) ? . . . . C(3) C(4) C(5) C(6) -0.1(2) ? . . . . C(4) C(5) C(6) N(2) -179.90(17) ? . . . 3_666 C(4) C(5) C(6) C(1) 0.6(2) ? . . . . N(2) C(7) C(8) C(9) -1.2(3) ? . . . . C(7) C(8) C(9) N(1) 0.6(3) ? . . . . N(3) C(10) C(11) C(12) 179.6(2) ? . . . . N(3) C(10) C(15) N(4) 2.3(2) ? . . . 3_566 N(3) C(10) C(15) C(14) -178.5(2) ? . . . . C(11) C(10) C(15) N(4) -177.1(2) ? . . . 3_566 C(11) C(10) C(15) C(14) 2.2(3) ? . . . . C(15) C(10) C(11) C(12) -1.1(3) ? . . . . C(10) C(11) C(12) C(13) 0.2(3) ? . . . . C(11) C(12) C(13) C(14) -0.2(3) ? . . . . C(12) C(13) C(14) C(15) 1.3(3) ? . . . . C(13) C(14) C(15) N(4) 176.9(2) ? . . . 3_566 C(13) C(14) C(15) C(10) -2.3(3) ? . . . . N(4) C(16) C(17) C(18) 0.7(3) ? . . . . C(16) C(17) C(18) N(3) -0.8(3) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cu(1) C(7) 3.444(2) ? . 1_565 Cu(1) C(7) 3.444(2) ? . 3_656 Cu(2) C(18) 3.468(2) ? . 1_545 Cu(2) C(18) 3.468(2) ? . 3_576 N(1) C(5) 3.449(2) ? . 1_545 N(2) C(7) 3.450(2) ? . 3_656 N(2) C(8) 3.397(2) ? . 3_656 N(2) C(9) 3.575(2) ? . 3_656 N(3) C(11) 3.598(3) ? . 2_546 N(3) C(17) 3.438(3) ? . 3_576 N(3) C(18) 3.451(3) ? . 3_576 N(4) C(11) 3.396(2) ? . 3_576 C(1) C(5) 3.574(2) ? . 1_545 C(2) C(4) 3.576(3) ? . 1_545 C(4) C(2) 3.576(3) ? . 1_565 C(4) C(7) 3.598(2) ? . 4_555 C(5) N(1) 3.449(2) ? . 1_565 C(5) C(1) 3.574(2) ? . 1_565 C(5) C(9) 3.387(2) ? . 1_565 C(6) C(8) 3.442(2) ? . 1_565 C(6) C(9) 3.261(2) ? . 1_565 C(7) Cu(1) 3.444(2) ? . 1_545 C(7) N(2) 3.450(2) ? . 3_656 C(7) C(4) 3.598(2) ? . 4_554 C(8) N(2) 3.397(2) ? . 3_656 C(8) C(6) 3.442(2) ? . 1_545 C(9) N(2) 3.575(2) ? . 3_656 C(9) C(5) 3.387(2) ? . 1_545 C(9) C(6) 3.261(2) ? . 1_545 C(10) C(16) 3.275(2) ? . 3_576 C(10) C(17) 3.450(3) ? . 3_576 C(11) N(3) 3.598(3) ? . 2_556 C(11) N(4) 3.396(2) ? . 3_576 C(11) C(15) 3.540(3) ? . 1_565 C(11) C(16) 3.364(3) ? . 3_576 C(12) C(14) 3.529(3) ? . 1_565 C(14) C(12) 3.529(3) ? . 1_545 C(15) C(11) 3.540(3) ? . 1_545 C(16) C(10) 3.275(2) ? . 3_576 C(16) C(11) 3.364(3) ? . 3_576 C(17) N(3) 3.438(3) ? . 3_576 C(17) C(10) 3.450(3) ? . 3_576 C(18) Cu(2) 3.468(2) ? . 1_565 C(18) N(3) 3.451(3) ? . 3_576 Cu(1) H(5) 3.311 ? . 1_565 Cu(1) H(5) 3.311 ? . 3_656 Cu(2) H(14) 3.345 ? . 1_545 Cu(2) H(14) 3.345 ? . 3_576 N(1) H(4) 3.298 ? . 1_545 N(1) H(5) 3.495 ? . 3_656 N(1) H(6) 3.368 ? . 1_565 N(1) H(10) 3.557 ? . 4_564 N(2) H(3) 3.380 ? . 4_564 N(2) H(4) 2.954 ? . 4_564 N(3) H(8) 2.968 ? . 2_546 N(3) H(9) 3.264 ? . 2_546 N(4) H(2) 3.321 ? . 3_566 N(4) H(8) 3.232 ? . 3_576 N(4) H(13) 3.425 ? . 1_545 N(4) H(14) 3.558 ? . 3_576 C(1) H(4) 3.260 ? . 1_545 C(1) H(5) 3.582 ? . 4_555 C(1) H(6) 3.454 ? . 1_565 C(1) H(7) 3.580 ? . 1_565 C(1) H(10) 3.167 ? . 4_564 C(2) H(3) 3.365 ? . 1_545 C(2) H(4) 3.583 ? . 1_545 C(2) H(5) 3.568 ? . 4_555 C(2) H(9) 3.454 ? . 4_564 C(2) H(10) 2.842 ? . 4_564 C(2) H(12) 3.551 ? . 3_566 C(2) H(13) 3.472 ? . 3_576 C(3) H(5) 3.230 ? . 4_555 C(3) H(6) 3.053 ? . 4_555 C(3) H(10) 3.404 ? . 4_564 C(3) H(11) 3.401 ? . . C(3) H(12) 3.550 ? . 3_566 C(3) H(12) 3.348 ? . 3_576 C(3) H(13) 2.921 ? . 3_576 C(4) H(1) 3.259 ? . 1_565 C(4) H(5) 2.863 ? . 4_555 C(4) H(6) 3.101 ? . 4_555 C(4) H(7) 3.510 ? . 1_565 C(4) H(12) 3.399 ? . 3_576 C(5) H(1) 3.588 ? . 1_565 C(5) H(4) 3.069 ? . 2_646 C(5) H(5) 2.865 ? . 4_555 C(5) H(7) 3.328 ? . 1_565 C(6) H(4) 2.899 ? . 2_646 C(6) H(5) 3.237 ? . 4_555 C(6) H(7) 3.370 ? . 1_565 C(7) H(3) 3.040 ? . 4_564 C(7) H(4) 3.121 ? . 4_564 C(8) H(3) 3.024 ? . 4_564 C(8) H(10) 3.149 ? . 4_554 C(8) H(11) 3.030 ? . 4_554 C(9) H(3) 3.407 ? . 4_564 C(9) H(4) 3.598 ? . 1_545 C(9) H(10) 3.178 ? . 4_554 C(9) H(11) 3.176 ? . 4_554 C(10) H(8) 2.843 ? . 2_546 C(10) H(12) 3.413 ? . 3_576 C(10) H(14) 3.256 ? . 2_546 C(11) H(8) 2.989 ? . 2_546 C(11) H(11) 3.535 ? . 1_565 C(11) H(12) 3.334 ? . 3_576 C(11) H(14) 2.910 ? . 2_546 C(12) H(1) 3.421 ? . 4_565 C(12) H(11) 3.183 ? . 1_565 C(12) H(12) 3.493 ? . 3_576 C(12) H(13) 3.202 ? . 2_546 C(12) H(14) 2.827 ? . 2_546 C(13) H(1) 3.439 ? . 4_565 C(13) H(2) 3.453 ? . . C(13) H(6) 2.978 ? . 4_555 C(13) H(7) 3.208 ? . 4_555 C(13) H(13) 3.037 ? . 2_546 C(13) H(14) 3.104 ? . 2_546 C(14) H(2) 2.769 ? . . C(14) H(6) 2.976 ? . 4_555 C(14) H(7) 3.323 ? . 4_555 C(14) H(8) 3.542 ? . 1_545 C(14) H(9) 3.294 ? . 1_545 C(14) H(14) 3.427 ? . 2_546 C(15) H(2) 3.051 ? . . C(15) H(8) 3.212 ? . 1_545 C(15) H(8) 3.576 ? . 2_546 C(15) H(13) 3.493 ? . 3_576 C(15) H(14) 3.522 ? . 2_546 C(16) H(1) 3.226 ? . 3_566 C(16) H(2) 3.284 ? . 3_566 C(16) H(2) 3.389 ? . 3_576 C(16) H(8) 3.567 ? . 3_576 C(16) H(9) 3.390 ? . 2_546 C(17) H(1) 3.441 ? . 3_566 C(17) H(2) 3.218 ? . 3_576 C(17) H(9) 2.935 ? . 2_546 C(18) H(8) 3.133 ? . 2_546 C(18) H(9) 2.896 ? . 2_546 H(1) C(4) 3.259 ? . 1_545 H(1) C(5) 3.588 ? . 1_545 H(1) C(12) 3.421 ? . 4_564 H(1) C(13) 3.439 ? . 4_564 H(1) C(16) 3.226 ? . 3_566 H(1) C(17) 3.441 ? . 3_566 H(1) H(3) 3.169 ? . 1_545 H(1) H(9) 2.775 ? . 4_564 H(1) H(10) 2.810 ? . 4_564 H(1) H(12) 2.976 ? . 3_566 H(1) H(13) 3.332 ? . 3_566 H(1) H(13) 3.491 ? . 3_576 H(2) N(4) 3.321 ? . 3_566 H(2) C(13) 3.453 ? . . H(2) C(14) 2.769 ? . . H(2) C(15) 3.051 ? . . H(2) C(16) 3.284 ? . 3_566 H(2) C(16) 3.389 ? . 3_576 H(2) C(17) 3.218 ? . 3_576 H(2) H(6) 2.927 ? . 4_555 H(2) H(11) 2.678 ? . . H(2) H(12) 2.972 ? . 3_566 H(2) H(12) 2.853 ? . 3_576 H(2) H(13) 2.501 ? . 3_576 H(3) N(2) 3.380 ? . 4_565 H(3) C(2) 3.365 ? . 1_565 H(3) C(7) 3.040 ? . 4_565 H(3) C(8) 3.024 ? . 4_565 H(3) C(9) 3.407 ? . 4_565 H(3) H(1) 3.169 ? . 1_565 H(3) H(5) 3.194 ? . 4_555 H(3) H(5) 3.364 ? . 4_565 H(3) H(6) 3.013 ? . 4_555 H(3) H(6) 3.322 ? . 4_565 H(3) H(11) 3.416 ? . 1_565 H(3) H(12) 2.951 ? . 3_576 H(4) N(1) 3.298 ? . 1_565 H(4) N(2) 2.954 ? . 4_565 H(4) C(1) 3.260 ? . 1_565 H(4) C(2) 3.583 ? . 1_565 H(4) C(5) 3.069 ? . 2_656 H(4) C(6) 2.899 ? . 2_656 H(4) C(7) 3.121 ? . 4_565 H(4) C(9) 3.598 ? . 1_565 H(4) H(4) 3.120 ? . 2_646 H(4) H(4) 3.120 ? . 2_656 H(4) H(5) 3.198 ? . 4_555 H(4) H(5) 3.088 ? . 4_565 H(5) Cu(1) 3.311 ? . 1_545 H(5) N(1) 3.495 ? . 3_656 H(5) C(1) 3.582 ? . 4_554 H(5) C(2) 3.568 ? . 4_554 H(5) C(3) 3.230 ? . 4_554 H(5) C(4) 2.863 ? . 4_554 H(5) C(5) 2.865 ? . 4_554 H(5) C(6) 3.237 ? . 4_554 H(5) H(3) 3.194 ? . 4_554 H(5) H(3) 3.364 ? . 4_564 H(5) H(4) 3.198 ? . 4_554 H(5) H(4) 3.088 ? . 4_564 H(6) N(1) 3.368 ? . 1_545 H(6) C(1) 3.454 ? . 1_545 H(6) C(3) 3.053 ? . 4_554 H(6) C(4) 3.101 ? . 4_554 H(6) C(13) 2.978 ? . 4_554 H(6) C(14) 2.976 ? . 4_554 H(6) H(2) 2.927 ? . 4_554 H(6) H(3) 3.013 ? . 4_554 H(6) H(3) 3.322 ? . 4_564 H(6) H(10) 2.489 ? . 4_554 H(6) H(11) 2.494 ? . 4_554 H(7) C(1) 3.580 ? . 1_545 H(7) C(4) 3.510 ? . 1_545 H(7) C(5) 3.328 ? . 1_545 H(7) C(6) 3.370 ? . 1_545 H(7) C(13) 3.208 ? . 4_554 H(7) C(14) 3.323 ? . 4_554 H(7) H(9) 3.237 ? . 4_564 H(7) H(10) 2.558 ? . 4_554 H(7) H(10) 3.362 ? . 4_564 H(7) H(11) 2.788 ? . 4_554 H(8) N(3) 2.968 ? . 2_556 H(8) N(4) 3.232 ? . 3_576 H(8) C(10) 2.843 ? . 2_556 H(8) C(11) 2.989 ? . 2_556 H(8) C(14) 3.542 ? . 1_565 H(8) C(15) 3.212 ? . 1_565 H(8) C(15) 3.576 ? . 2_556 H(8) C(16) 3.567 ? . 3_576 H(8) C(18) 3.133 ? . 2_556 H(8) H(8) 3.072 ? . 2_546 H(8) H(8) 3.072 ? . 2_556 H(8) H(14) 3.300 ? . 2_546 H(8) H(14) 3.059 ? . 2_556 H(9) N(3) 3.264 ? . 2_556 H(9) C(2) 3.454 ? . 4_565 H(9) C(14) 3.294 ? . 1_565 H(9) C(16) 3.390 ? . 2_556 H(9) C(17) 2.935 ? . 2_556 H(9) C(18) 2.896 ? . 2_556 H(9) H(1) 2.775 ? . 4_565 H(9) H(7) 3.237 ? . 4_565 H(9) H(11) 3.068 ? . 1_565 H(9) H(13) 3.143 ? . 2_546 H(9) H(13) 3.231 ? . 2_556 H(9) H(14) 3.176 ? . 2_546 H(9) H(14) 3.186 ? . 2_556 H(10) N(1) 3.557 ? . 4_565 H(10) C(1) 3.167 ? . 4_565 H(10) C(2) 2.842 ? . 4_565 H(10) C(3) 3.404 ? . 4_565 H(10) C(8) 3.149 ? . 4_555 H(10) C(9) 3.178 ? . 4_555 H(10) H(1) 2.810 ? . 4_565 H(10) H(6) 2.489 ? . 4_555 H(10) H(7) 2.558 ? . 4_555 H(10) H(7) 3.362 ? . 4_565 H(10) H(13) 2.857 ? . 2_546 H(10) H(14) 3.587 ? . 2_546 H(11) C(3) 3.401 ? . . H(11) C(8) 3.030 ? . 4_555 H(11) C(9) 3.176 ? . 4_555 H(11) C(11) 3.535 ? . 1_545 H(11) C(12) 3.183 ? . 1_545 H(11) H(2) 2.678 ? . . H(11) H(3) 3.416 ? . 1_545 H(11) H(6) 2.494 ? . 4_555 H(11) H(7) 2.788 ? . 4_555 H(11) H(9) 3.068 ? . 1_545 H(12) C(2) 3.551 ? . 3_566 H(12) C(3) 3.550 ? . 3_566 H(12) C(3) 3.348 ? . 3_576 H(12) C(4) 3.399 ? . 3_576 H(12) C(10) 3.413 ? . 3_576 H(12) C(11) 3.334 ? . 3_576 H(12) C(12) 3.493 ? . 3_576 H(12) H(1) 2.976 ? . 3_566 H(12) H(2) 2.972 ? . 3_566 H(12) H(2) 2.853 ? . 3_576 H(12) H(3) 2.951 ? . 3_576 H(13) N(4) 3.425 ? . 1_565 H(13) C(2) 3.472 ? . 3_576 H(13) C(3) 2.921 ? . 3_576 H(13) C(12) 3.202 ? . 2_556 H(13) C(13) 3.037 ? . 2_556 H(13) C(15) 3.493 ? . 3_576 H(13) H(1) 3.332 ? . 3_566 H(13) H(1) 3.491 ? . 3_576 H(13) H(2) 2.501 ? . 3_576 H(13) H(9) 3.231 ? . 2_546 H(13) H(9) 3.143 ? . 2_556 H(13) H(10) 2.857 ? . 2_556 H(14) Cu(2) 3.345 ? . 1_565 H(14) N(4) 3.558 ? . 3_576 H(14) C(10) 3.256 ? . 2_556 H(14) C(11) 2.910 ? . 2_556 H(14) C(12) 2.827 ? . 2_556 H(14) C(13) 3.104 ? . 2_556 H(14) C(14) 3.427 ? . 2_556 H(14) C(15) 3.522 ? . 2_556 H(14) H(8) 3.059 ? . 2_546 H(14) H(8) 3.300 ? . 2_556 H(14) H(9) 3.186 ? . 2_546 H(14) H(9) 3.176 ? . 2_556 H(14) H(10) 3.587 ? . 2_556 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment '- Ni_dntaa.cif' data___Ni_dntaa _database_code_depnum_ccdc_archive 'CCDC 882250' #TrackingRef '- Ni_dntaa.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C26 H18 N4 Ni ' _chemical_formula_moiety 'C26 H18 N4 Ni ' _chemical_formula_weight 445.15 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m c 21' _symmetry_space_group_name_Hall 'C 2c -2' _symmetry_Int_Tables_number 36 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,+Z 3 +X,-Y,1/2+Z 4 -X,-Y,1/2+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,+Z 7 1/2+X,1/2-Y,1/2+Z 8 1/2-X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 20.428(4) _cell_length_b 12.905(2) _cell_length_c 6.9730(12) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 1838.3(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2876 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 150.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920.00 _exptl_absorpt_coefficient_mu 1.079 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.892 _exptl_absorpt_correction_T_max 0.958 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 7216 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_ambient_temperature 150.1 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). When refinement was complete a residual peak approximately 2.63 e.A-3 high was observed,approximately 2.78 A from the closest C atom. The position of the peak was such that we felt it belonged to the Ni centre of a second, overlapping orientation of the complex. A disorder model was thus created. However, other residual peaks did not clearly indicate, for example, the naphthalene ring which had to be constrained to ideal geometry during refinement to stop the model from blowing apart. Constrained or unconstrained, the occupancy of the minor component never rose above 2%. We feel that, even if there truly is a minor second orientation in the crystal, the number of constraints and restraints which would be needed to keep the complex geometry within chemically sensible limits far exceeds the usefulness to the overall structure, and needlessly complicates the refinement. Given that the ordered model refines well, we have retained it, but note the residual peak and our attempts to model that peak. ; _reflns_number_total 2063 _reflns_number_gt 1953 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0962 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2063 _refine_ls_number_parameters 146 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0663P)^2^+0.9136P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 2.63 _refine_diff_density_min -0.36 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 897 Friedel Pairs' _refine_ls_abs_structure_Flack 0.05(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Ni(1) Ni 1.0000 0.62695(3) 0.33203(12) 0.01100(14) Uani 1.00 2 d S . . N(1) N 0.93270(10) 0.53134(15) 0.3694(3) 0.0134(5) Uani 1.00 1 d . . . N(2) N 0.93265(10) 0.72172(16) 0.2890(3) 0.0122(5) Uani 1.00 1 d . . . C(1) C 0.86885(12) 0.57345(19) 0.3581(5) 0.0117(6) Uani 1.00 1 d . . . C(2) C 0.81073(12) 0.5240(2) 0.3971(4) 0.0144(5) Uani 1.00 1 d . . . C(3) C 0.75044(11) 0.57460(18) 0.3628(5) 0.0113(5) Uani 1.00 1 d . . . C(4) C 0.68952(13) 0.5257(2) 0.3987(4) 0.0167(6) Uani 1.00 1 d . . . C(5) C 0.63182(12) 0.5742(2) 0.3547(6) 0.0158(6) Uani 1.00 1 d . . . C(6) C 0.63212(14) 0.6740(2) 0.2681(4) 0.0174(6) Uani 1.00 1 d . . . C(7) C 0.68977(12) 0.7238(2) 0.2353(4) 0.0139(5) Uani 1.00 1 d . . . C(8) C 0.75056(12) 0.6764(2) 0.2816(5) 0.0133(6) Uani 1.00 1 d . . . C(9) C 0.81122(12) 0.7275(2) 0.2506(4) 0.0127(5) Uani 1.00 1 d . . . C(10) C 0.86881(13) 0.6791(2) 0.2966(4) 0.0142(7) Uani 1.00 1 d . . . C(11) C 0.94020(12) 0.42942(19) 0.3835(3) 0.0143(6) Uani 1.00 1 d . . . C(12) C 1.0000 0.3789(3) 0.3891(6) 0.0154(8) Uani 1.00 2 d S . . C(13) C 0.94000(13) 0.8225(2) 0.2526(4) 0.0161(5) Uani 1.00 1 d . . . C(14) C 1.0000 0.8717(3) 0.2351(7) 0.0202(8) Uani 1.00 2 d S . . H(1) H 0.8111 0.4556 0.4472 0.017 Uiso 1.00 1 c R . . H(2) H 0.6887 0.4584 0.4541 0.020 Uiso 1.00 1 c R . . H(3) H 0.5914 0.5410 0.3821 0.019 Uiso 1.00 1 c R . . H(4) H 0.5920 0.7059 0.2331 0.021 Uiso 1.00 1 c R . . H(5) H 0.6894 0.7912 0.1807 0.017 Uiso 1.00 1 c R . . H(6) H 0.8119 0.7953 0.1978 0.015 Uiso 1.00 1 c R . . H(7) H 0.9018 0.3882 0.3903 0.017 Uiso 1.00 1 c R . . H(8) H 1.0000 0.3054 0.3972 0.019 Uiso 1.00 2 c R . . H(9) H 0.9016 0.8632 0.2375 0.019 Uiso 1.00 1 c R . . H(10) H 1.0000 0.9440 0.2096 0.024 Uiso 1.00 2 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(1) 0.00930(19) 0.0089(2) 0.0148(2) 0.0000 0.0000 0.0008(2) N(1) 0.0119(8) 0.0113(9) 0.0170(15) -0.0004(7) 0.0002(8) 0.0003(9) N(2) 0.0115(9) 0.0124(10) 0.0127(13) 0.0003(7) 0.0009(7) 0.0009(7) C(1) 0.0123(10) 0.0134(11) 0.0094(16) 0.0014(7) 0.0010(11) -0.0019(10) C(2) 0.0179(13) 0.0125(13) 0.0130(12) -0.0011(9) -0.0001(9) -0.0011(10) C(3) 0.0114(12) 0.0144(12) 0.0080(15) -0.0013(7) -0.0003(8) 0.0004(11) C(4) 0.0203(13) 0.0149(13) 0.0148(13) -0.0013(9) 0.0034(10) -0.0031(10) C(5) 0.0109(10) 0.0189(12) 0.0176(18) -0.0031(8) 0.0000(13) -0.0055(13) C(6) 0.0127(12) 0.0195(14) 0.0201(13) 0.0025(9) -0.0016(11) -0.0058(10) C(7) 0.0103(11) 0.0159(14) 0.0156(13) 0.0020(8) -0.0003(9) -0.0009(10) C(8) 0.0114(14) 0.0146(13) 0.0141(15) 0.0004(8) 0.0011(7) -0.0032(10) C(9) 0.0105(11) 0.0138(13) 0.0138(12) -0.0003(8) -0.0000(10) 0.0014(10) C(10) 0.0128(12) 0.0118(11) 0.0179(19) -0.0008(8) 0.0040(10) -0.0008(9) C(11) 0.0146(11) 0.0118(12) 0.0163(16) -0.0025(8) 0.0009(8) 0.0002(9) C(12) 0.0169(16) 0.0101(17) 0.019(2) 0.0000 0.0000 0.0019(14) C(13) 0.0156(12) 0.0108(12) 0.0218(14) 0.0007(9) -0.0014(10) 0.0023(10) C(14) 0.0184(19) 0.013(2) 0.029(2) 0.0000 0.0000 0.0020(16) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ni(1) N(1) 1.866(2) yes . . Ni(1) N(1) 1.866(2) yes . 2_755 Ni(1) N(2) 1.865(2) yes . . Ni(1) N(2) 1.865(2) yes . 2_755 N(1) C(1) 1.415(3) yes . . N(1) C(11) 1.328(3) yes . . N(2) C(10) 1.416(3) yes . . N(2) C(13) 1.334(3) yes . . C(1) C(2) 1.375(3) yes . . C(1) C(10) 1.429(3) yes . . C(2) C(3) 1.414(3) yes . . C(3) C(4) 1.418(3) yes . . C(3) C(8) 1.430(3) yes . . C(4) C(5) 1.370(3) yes . . C(5) C(6) 1.422(4) yes . . C(6) C(7) 1.361(3) yes . . C(7) C(8) 1.421(3) yes . . C(8) C(9) 1.420(3) yes . . C(9) C(10) 1.370(3) yes . . C(11) C(12) 1.385(3) yes . . C(13) C(14) 1.386(3) yes . . C(2) H(1) 0.950 no . . C(4) H(2) 0.950 no . . C(5) H(3) 0.950 no . . C(6) H(4) 0.950 no . . C(7) H(5) 0.950 no . . C(9) H(6) 0.950 no . . C(11) H(7) 0.950 no . . C(12) H(8) 0.950 no . . C(13) H(9) 0.950 no . . C(14) H(10) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 N(1) Ni(1) N(1) 94.94(8) yes . . 2_755 N(1) Ni(1) N(2) 84.98(8) yes . . . N(1) Ni(1) N(2) 178.73(10) yes . . 2_755 N(1) Ni(1) N(2) 178.73(10) yes 2_755 . . N(1) Ni(1) N(2) 84.98(8) yes 2_755 . 2_755 N(2) Ni(1) N(2) 95.06(9) yes . . 2_755 Ni(1) N(1) C(1) 114.68(15) yes . . . Ni(1) N(1) C(11) 125.48(17) yes . . . C(1) N(1) C(11) 119.4(2) yes . . . Ni(1) N(2) C(10) 114.75(16) yes . . . Ni(1) N(2) C(13) 125.95(17) yes . . . C(10) N(2) C(13) 119.3(2) yes . . . N(1) C(1) C(2) 127.4(2) yes . . . N(1) C(1) C(10) 112.5(2) yes . . . C(2) C(1) C(10) 120.1(2) yes . . . C(1) C(2) C(3) 120.3(2) yes . . . C(2) C(3) C(4) 121.9(2) yes . . . C(2) C(3) C(8) 119.3(2) yes . . . C(4) C(3) C(8) 118.7(2) yes . . . C(3) C(4) C(5) 120.8(2) yes . . . C(4) C(5) C(6) 120.4(2) yes . . . C(5) C(6) C(7) 120.2(2) yes . . . C(6) C(7) C(8) 121.0(2) yes . . . C(3) C(8) C(7) 118.9(2) yes . . . C(3) C(8) C(9) 119.2(2) yes . . . C(7) C(8) C(9) 121.9(2) yes . . . C(8) C(9) C(10) 120.1(2) yes . . . N(2) C(10) C(1) 112.4(2) yes . . . N(2) C(10) C(9) 127.2(2) yes . . . C(1) C(10) C(9) 120.4(2) yes . . . N(1) C(11) C(12) 124.8(2) yes . . . C(11) C(12) C(11) 123.7(3) yes . . 2_755 N(2) C(13) C(14) 124.3(2) yes . . . C(13) C(14) C(13) 124.4(3) yes . . 2_755 C(1) C(2) H(1) 119.8 no . . . C(3) C(2) H(1) 119.8 no . . . C(3) C(4) H(2) 119.6 no . . . C(5) C(4) H(2) 119.6 no . . . C(4) C(5) H(3) 119.8 no . . . C(6) C(5) H(3) 119.8 no . . . C(5) C(6) H(4) 119.9 no . . . C(7) C(6) H(4) 119.9 no . . . C(6) C(7) H(5) 119.5 no . . . C(8) C(7) H(5) 119.5 no . . . C(8) C(9) H(6) 119.9 no . . . C(10) C(9) H(6) 119.9 no . . . N(1) C(11) H(7) 117.6 no . . . C(12) C(11) H(7) 117.6 no . . . C(11) C(12) H(8) 118.1 no . . . C(11) C(12) H(8) 118.1 no 2_755 . . N(2) C(13) H(9) 117.9 no . . . C(14) C(13) H(9) 117.9 no . . . C(13) C(14) H(10) 117.8 no . . . C(13) C(14) H(10) 117.8 no 2_755 . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 N(1) Ni(1) N(1) C(1) -178.4(2) ? . . 2_755 2_755 N(1) Ni(1) N(1) C(11) 9.3(2) ? . . 2_755 2_755 N(1) Ni(1) N(1) C(1) 178.4(2) ? 2_755 . . . N(1) Ni(1) N(1) C(11) -9.3(2) ? 2_755 . . . N(1) Ni(1) N(2) C(10) -2.27(18) ? . . . . N(1) Ni(1) N(2) C(13) 177.9(2) ? . . . . N(2) Ni(1) N(1) C(1) -2.9(2) ? . . . . N(2) Ni(1) N(1) C(11) 169.4(2) ? . . . . N(1) Ni(1) N(2) C(10) -84(4) ? . . 2_755 2_755 N(1) Ni(1) N(2) C(13) 95(4) ? . . 2_755 2_755 N(2) Ni(1) N(1) C(1) -95(4) ? 2_755 . . . N(2) Ni(1) N(1) C(11) 77(4) ? 2_755 . . . N(1) Ni(1) N(2) C(10) 84(4) ? 2_755 . . . N(1) Ni(1) N(2) C(13) -95(4) ? 2_755 . . . N(2) Ni(1) N(1) C(1) 95(4) ? . . 2_755 2_755 N(2) Ni(1) N(1) C(11) -77(4) ? . . 2_755 2_755 N(1) Ni(1) N(2) C(10) 2.27(18) ? 2_755 . 2_755 2_755 N(1) Ni(1) N(2) C(13) -177.9(2) ? 2_755 . 2_755 2_755 N(2) Ni(1) N(1) C(1) 2.9(2) ? 2_755 . 2_755 2_755 N(2) Ni(1) N(1) C(11) -169.4(2) ? 2_755 . 2_755 2_755 N(2) Ni(1) N(2) C(10) -176.46(18) ? . . 2_755 2_755 N(2) Ni(1) N(2) C(13) 3.4(2) ? . . 2_755 2_755 N(2) Ni(1) N(2) C(10) 176.46(18) ? 2_755 . . . N(2) Ni(1) N(2) C(13) -3.4(2) ? 2_755 . . . Ni(1) N(1) C(1) C(2) -173.4(2) ? . . . . Ni(1) N(1) C(1) C(10) 7.3(3) ? . . . . Ni(1) N(1) C(11) C(12) 5.8(4) ? . . . . C(1) N(1) C(11) C(12) 177.8(3) ? . . . . C(11) N(1) C(1) C(2) 13.8(5) ? . . . . C(11) N(1) C(1) C(10) -165.5(2) ? . . . . Ni(1) N(2) C(10) C(1) 6.8(3) ? . . . . Ni(1) N(2) C(10) C(9) -172.4(2) ? . . . . Ni(1) N(2) C(13) C(14) 2.2(4) ? . . . . C(10) N(2) C(13) C(14) -177.6(3) ? . . . . C(13) N(2) C(10) C(1) -173.4(2) ? . . . . C(13) N(2) C(10) C(9) 7.5(4) ? . . . . N(1) C(1) C(2) C(3) -174.5(3) ? . . . . N(1) C(1) C(10) N(2) -8.9(3) ? . . . . N(1) C(1) C(10) C(9) 170.4(2) ? . . . . C(2) C(1) C(10) N(2) 171.7(2) ? . . . . C(2) C(1) C(10) C(9) -9.0(4) ? . . . . C(10) C(1) C(2) C(3) 4.8(5) ? . . . . C(1) C(2) C(3) C(4) 179.1(3) ? . . . . C(1) C(2) C(3) C(8) 2.0(5) ? . . . . C(2) C(3) C(4) C(5) -176.5(3) ? . . . . C(2) C(3) C(8) C(7) 175.7(3) ? . . . . C(2) C(3) C(8) C(9) -4.7(5) ? . . . . C(4) C(3) C(8) C(7) -1.6(5) ? . . . . C(4) C(3) C(8) C(9) 178.0(3) ? . . . . C(8) C(3) C(4) C(5) 0.7(5) ? . . . . C(3) C(4) C(5) C(6) 1.3(5) ? . . . . C(4) C(5) C(6) C(7) -2.6(5) ? . . . . C(5) C(6) C(7) C(8) 1.8(4) ? . . . . C(6) C(7) C(8) C(3) 0.3(4) ? . . . . C(6) C(7) C(8) C(9) -179.3(3) ? . . . . C(3) C(8) C(9) C(10) 0.6(4) ? . . . . C(7) C(8) C(9) C(10) -179.9(2) ? . . . . C(8) C(9) C(10) N(2) -174.7(2) ? . . . . C(8) C(9) C(10) C(1) 6.2(4) ? . . . . N(1) C(11) C(12) C(11) 1.0(5) ? . . . 2_755 N(2) C(13) C(14) C(13) 0.2(5) ? . . . 2_755 loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Ni(1) C(11) 3.436(2) ? . 3_564 Ni(1) C(11) 3.436(2) ? . 4_764 Ni(1) C(12) 3.089(4) ? . 3_564 N(1) N(1) 3.579(3) ? . 3_564 N(1) N(1) 3.579(3) ? . 3_565 N(1) C(11) 3.429(3) ? . 3_564 N(2) C(11) 3.438(3) ? . 3_564 N(2) C(12) 3.370(4) ? . 3_564 C(2) C(2) 3.541(4) ? . 3_564 C(2) C(2) 3.541(4) ? . 3_565 C(4) C(4) 3.549(4) ? . 3_564 C(4) C(4) 3.549(4) ? . 3_565 C(5) C(13) 3.410(5) ? . 8_665 C(7) C(9) 3.438(4) ? . 8_664 C(7) C(10) 3.516(4) ? . 8_664 C(9) C(7) 3.438(4) ? . 8_665 C(10) C(7) 3.516(4) ? . 8_665 C(10) C(11) 3.519(3) ? . 3_564 C(11) Ni(1) 3.436(2) ? . 3_565 C(11) N(1) 3.429(3) ? . 3_565 C(11) N(2) 3.438(3) ? . 3_565 C(11) C(10) 3.519(3) ? . 3_565 C(12) Ni(1) 3.089(4) ? . 3_565 C(12) N(2) 3.370(4) ? . 3_565 C(12) N(2) 3.370(4) ? . 4_765 C(13) C(5) 3.410(5) ? . 8_664 Ni(1) H(8) 3.155 ? . 3_564 N(1) H(7) 3.555 ? . 3_564 N(2) H(4) 3.273 ? . 8_665 N(2) H(7) 3.184 ? . 3_564 N(2) H(8) 3.078 ? . 3_564 C(1) H(1) 3.121 ? . 3_564 C(1) H(5) 3.086 ? . 8_665 C(1) H(7) 3.368 ? . 3_564 C(2) H(1) 3.148 ? . 3_564 C(2) H(5) 3.362 ? . 6_645 C(2) H(5) 3.098 ? . 8_665 C(3) H(1) 3.175 ? . 3_564 C(3) H(2) 3.146 ? . 3_564 C(3) H(5) 3.070 ? . 8_665 C(3) H(6) 3.146 ? . 8_665 C(4) H(2) 3.108 ? . 3_564 C(4) H(6) 3.286 ? . 6_645 C(4) H(6) 3.112 ? . 8_665 C(4) H(9) 3.021 ? . 6_645 C(4) H(9) 3.332 ? . 8_665 C(5) H(2) 3.055 ? . 3_564 C(5) H(6) 3.144 ? . 8_665 C(5) H(9) 2.924 ? . 6_645 C(5) H(9) 2.872 ? . 8_665 C(5) H(10) 3.332 ? . 5_445 C(6) H(2) 3.009 ? . 3_564 C(6) H(6) 3.232 ? . 8_665 C(6) H(7) 2.974 ? . 6_655 C(6) H(8) 3.312 ? . 5_455 C(6) H(9) 3.379 ? . 8_665 C(7) H(1) 3.336 ? . 6_655 C(7) H(2) 3.062 ? . 3_564 C(7) H(6) 3.235 ? . 8_665 C(7) H(7) 3.027 ? . 6_655 C(8) H(1) 3.141 ? . 3_564 C(8) H(2) 3.136 ? . 3_564 C(8) H(5) 3.070 ? . 8_665 C(8) H(6) 3.191 ? . 8_665 C(9) H(1) 3.171 ? . 3_564 C(9) H(2) 3.301 ? . 6_655 C(9) H(5) 3.009 ? . 8_665 C(9) H(7) 3.458 ? . 3_564 C(10) H(1) 3.217 ? . 3_564 C(10) H(4) 3.479 ? . 8_665 C(10) H(5) 2.955 ? . 8_665 C(10) H(7) 3.039 ? . 3_564 C(11) H(4) 3.138 ? . 6_645 C(11) H(5) 3.491 ? . 6_645 C(12) H(4) 3.114 ? . 5_545 C(12) H(4) 3.114 ? . 6_645 C(13) H(2) 3.459 ? . 6_655 C(13) H(3) 3.030 ? . 6_655 C(13) H(3) 3.192 ? . 8_664 C(13) H(4) 3.433 ? . 8_665 C(13) H(8) 3.219 ? . 3_564 C(14) H(3) 3.051 ? . 5_555 C(14) H(3) 3.051 ? . 6_655 C(14) H(3) 3.288 ? . 7_564 C(14) H(3) 3.288 ? . 8_664 C(14) H(8) 3.282 ? . 3_564 H(1) C(1) 3.121 ? . 3_565 H(1) C(2) 3.148 ? . 3_565 H(1) C(3) 3.175 ? . 3_565 H(1) C(7) 3.336 ? . 6_645 H(1) C(8) 3.141 ? . 3_565 H(1) C(9) 3.171 ? . 3_565 H(1) C(10) 3.217 ? . 3_565 H(1) H(5) 2.820 ? . 6_645 H(2) C(3) 3.146 ? . 3_565 H(2) C(4) 3.108 ? . 3_565 H(2) C(5) 3.055 ? . 3_565 H(2) C(6) 3.009 ? . 3_565 H(2) C(7) 3.062 ? . 3_565 H(2) C(8) 3.136 ? . 3_565 H(2) C(9) 3.301 ? . 6_645 H(2) C(13) 3.459 ? . 6_645 H(2) H(3) 3.587 ? . 3_565 H(2) H(4) 3.491 ? . 3_565 H(2) H(5) 3.589 ? . 3_565 H(2) H(6) 2.761 ? . 6_645 H(2) H(9) 2.682 ? . 6_645 H(2) H(9) 3.551 ? . 8_665 H(3) C(13) 3.030 ? . 6_645 H(3) C(13) 3.192 ? . 8_665 H(3) C(14) 3.051 ? . 5_445 H(3) C(14) 3.288 ? . 7_465 H(3) H(2) 3.587 ? . 3_564 H(3) H(9) 2.510 ? . 6_645 H(3) H(9) 2.773 ? . 8_665 H(3) H(10) 2.549 ? . 5_445 H(3) H(10) 2.956 ? . 7_465 H(4) N(2) 3.273 ? . 8_664 H(4) C(10) 3.479 ? . 8_664 H(4) C(11) 3.138 ? . 6_655 H(4) C(12) 3.114 ? . 5_455 H(4) C(13) 3.433 ? . 8_664 H(4) H(2) 3.491 ? . 3_564 H(4) H(7) 2.597 ? . 6_655 H(4) H(8) 2.547 ? . 5_455 H(4) H(9) 3.571 ? . 8_664 H(5) C(1) 3.086 ? . 8_664 H(5) C(2) 3.362 ? . 6_655 H(5) C(2) 3.098 ? . 8_664 H(5) C(3) 3.070 ? . 8_664 H(5) C(8) 3.070 ? . 8_664 H(5) C(9) 3.009 ? . 8_664 H(5) C(10) 2.955 ? . 8_664 H(5) C(11) 3.491 ? . 6_655 H(5) H(1) 2.820 ? . 6_655 H(5) H(2) 3.589 ? . 3_564 H(5) H(6) 3.548 ? . 8_664 H(5) H(7) 2.677 ? . 6_655 H(6) C(3) 3.146 ? . 8_664 H(6) C(4) 3.286 ? . 6_655 H(6) C(4) 3.112 ? . 8_664 H(6) C(5) 3.144 ? . 8_664 H(6) C(6) 3.232 ? . 8_664 H(6) C(7) 3.235 ? . 8_664 H(6) C(8) 3.191 ? . 8_664 H(6) H(2) 2.761 ? . 6_655 H(6) H(5) 3.548 ? . 8_665 H(7) N(1) 3.555 ? . 3_565 H(7) N(2) 3.184 ? . 3_565 H(7) C(1) 3.368 ? . 3_565 H(7) C(6) 2.974 ? . 6_645 H(7) C(7) 3.027 ? . 6_645 H(7) C(9) 3.458 ? . 3_565 H(7) C(10) 3.039 ? . 3_565 H(7) H(4) 2.597 ? . 6_645 H(7) H(5) 2.677 ? . 6_645 H(8) Ni(1) 3.155 ? . 3_565 H(8) N(2) 3.078 ? . 3_565 H(8) N(2) 3.078 ? . 4_765 H(8) C(6) 3.312 ? . 5_545 H(8) C(6) 3.312 ? . 6_645 H(8) C(13) 3.219 ? . 3_565 H(8) C(13) 3.219 ? . 4_765 H(8) C(14) 3.282 ? . 3_565 H(8) H(4) 2.547 ? . 5_545 H(8) H(4) 2.547 ? . 6_645 H(9) C(4) 3.021 ? . 6_655 H(9) C(4) 3.332 ? . 8_664 H(9) C(5) 2.924 ? . 6_655 H(9) C(5) 2.872 ? . 8_664 H(9) C(6) 3.379 ? . 8_664 H(9) H(2) 2.682 ? . 6_655 H(9) H(2) 3.551 ? . 8_664 H(9) H(3) 2.510 ? . 6_655 H(9) H(3) 2.773 ? . 8_664 H(9) H(4) 3.571 ? . 8_665 H(10) C(5) 3.332 ? . 5_555 H(10) C(5) 3.332 ? . 6_655 H(10) H(3) 2.549 ? . 5_555 H(10) H(3) 2.549 ? . 6_655 H(10) H(3) 2.956 ? . 7_564 H(10) H(3) 2.956 ? . 8_664 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================