data_global #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Dr. Jagadese J. Vittal Department of Chemistry National University of Singapore 3 Science Drive 3 SINGAPORE 117543 ; _publ_contact_author_phone '(65) 6874 2677' _publ_contact_author_fax '(65) 6779 1691' _publ_contact_author_email chmjjv@nus.edu.sg _publ_requested_journal 'Crystal Growth & Design' _publ_requested_coeditor_name ' ' _publ_contact_letter ; '' ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _iucr_compatibility_tag ACTA95 _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year 2000 _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; A Metal Coordination Polymer with the Hexagonal Diamondoid (or Lonsdaleite) Network Topology ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Jagadese J. Vittal ; Department of Chemistry National University of Singapore SINGAPORE 117543 ; 'Bellam Sreenivasulu' ; Department of Chemistry National University of Singapore SINGAPORE 117543 ; #============================================================================== _data_compound 2 #data_bs6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H32 Cu2 N2 O7' _chemical_formula_weight 611.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Ia-3d loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'y+3/4, x+1/4, -z+1/4' '-y+3/4, -x+3/4, -z+3/4' 'y+1/4, -x+1/4, z+3/4' '-y+1/4, x+3/4, z+1/4' 'x+3/4, z+1/4, -y+1/4' '-x+1/4, z+3/4, y+1/4' '-x+3/4, -z+3/4, -y+3/4' 'x+1/4, -z+1/4, y+3/4' 'z+3/4, y+1/4, -x+1/4' 'z+1/4, -y+1/4, x+3/4' '-z+1/4, y+3/4, x+1/4' '-z+3/4, -y+3/4, -x+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1, -x+1, -y+1/2' '-z+1, -x+1/2, y+1' '-z+1/2, x+1, -y+1' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1, -x+1' 'y+1, -z+1, -x+1/2' '-y+1, -z+1/2, x+1' 'y+5/4, x+3/4, -z+3/4' '-y+5/4, -x+5/4, -z+5/4' 'y+3/4, -x+3/4, z+5/4' '-y+3/4, x+5/4, z+3/4' 'x+5/4, z+3/4, -y+3/4' '-x+3/4, z+5/4, y+3/4' '-x+5/4, -z+5/4, -y+5/4' 'x+3/4, -z+3/4, y+5/4' 'z+5/4, y+3/4, -x+3/4' 'z+3/4, -y+3/4, x+5/4' '-z+3/4, y+5/4, x+3/4' '-z+5/4, -y+5/4, -x+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' '-y-3/4, -x-1/4, z-1/4' 'y-3/4, x-3/4, z-3/4' '-y-1/4, x-1/4, -z-3/4' 'y-1/4, -x-3/4, -z-1/4' '-x-3/4, -z-1/4, y-1/4' 'x-1/4, -z-3/4, -y-1/4' 'x-3/4, z-3/4, y-3/4' '-x-1/4, z-1/4, -y-3/4' '-z-3/4, -y-1/4, x-1/4' '-z-1/4, y-1/4, -x-3/4' 'z-1/4, -y-3/4, -x-1/4' 'z-3/4, y-3/4, x-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'x+1/2, -y, z' '-x, y, z+1/2' '-z+1/2, -x+1/2, -y+1/2' '-z, x, y+1/2' 'z, x+1/2, -y' 'z+1/2, -x, y' '-y+1/2, -z+1/2, -x+1/2' 'y+1/2, -z, x' '-y, z, x+1/2' 'y, z+1/2, -x' '-y-1/4, -x+1/4, z+1/4' 'y-1/4, x-1/4, z-1/4' '-y+1/4, x+1/4, -z-1/4' 'y+1/4, -x-1/4, -z+1/4' '-x-1/4, -z+1/4, y+1/4' 'x+1/4, -z-1/4, -y+1/4' 'x-1/4, z-1/4, y-1/4' '-x+1/4, z+1/4, -y-1/4' '-z-1/4, -y+1/4, x+1/4' '-z+1/4, y+1/4, -x-1/4' 'z+1/4, -y-1/4, -x+1/4' 'z-1/4, y-1/4, x-1/4' _cell_length_a 33.5375(3) _cell_length_b 33.5375(3) _cell_length_c 33.5375(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 37721.8(6) _cell_formula_units_Z 48 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8972 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 24.3 _exptl_crystal_description blocks _exptl_crystal_colour green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 15168 _exptl_absorpt_coefficient_mu 1.393 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7400 _exptl_absorpt_correction_T_max 0.8397 _exptl_absorpt_process_details 'SADABS (Sheldrick 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS APEX CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66509 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2781 _reflns_number_gt 2364 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS, SMART' _computing_cell_refinement 'Bruker AXS, SAINT' _computing_data_reduction 'Bruker AXS, SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS, SHELXTL' _computing_publication_material 'Bruker AXS, SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1105P)^2^+62.8848P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2781 _refine_ls_number_parameters 177 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1519 _refine_ls_wR_factor_gt 0.1427 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.063699(12) 0.158521(11) 0.856841(12) 0.0264(2) Uani 1 1 d . A . O1 O 0.06434(7) 0.10049(7) 0.85236(7) 0.0315(6) Uani 1 1 d . . . C1 C 0.02989(10) 0.08232(10) 0.86182(11) 0.0305(7) Uani 1 1 d . . . C2 C 0.01104(11) 0.05689(11) 0.83514(13) 0.0410(9) Uani 1 1 d . . . H2 H 0.0225 0.0519 0.8101 0.049 Uiso 1 1 calc R . . C3 C -0.02435(13) 0.03911(14) 0.84547(17) 0.0609(13) Uani 1 1 d . . . H3 H -0.0371 0.0219 0.8274 0.073 Uiso 1 1 calc R . . C4 C -0.04134(15) 0.04638(15) 0.88236(19) 0.0758(18) Uani 1 1 d . . . H4 H -0.0656 0.0341 0.8894 0.091 Uiso 1 1 calc R . . C5 C -0.02249(14) 0.07180(13) 0.90892(16) 0.0565(13) Uani 1 1 d . . . H5 H -0.0341 0.0767 0.9339 0.068 Uiso 1 1 calc R . . C6 C 0.01300(11) 0.09001(10) 0.89926(11) 0.0333(8) Uani 1 1 d . . . C7 C 0.03471(11) 0.11660(10) 0.92819(10) 0.0330(8) Uani 1 1 d . A . H7A H 0.0194 0.1185 0.9530 0.040 Uiso 1 1 calc R . . H7B H 0.0607 0.1048 0.9346 0.040 Uiso 1 1 calc R . . N1 N 0.04076(8) 0.15728(8) 0.91146(8) 0.0246(6) Uani 1 1 d . . . H1 H 0.0191(11) 0.1675(11) 0.9086(10) 0.021(9) Uiso 1 1 d . . . C8 C 0.06506(10) 0.18610(10) 0.93495(10) 0.0308(8) Uani 1 1 d D A 1 C9 C 0.04628(14) 0.19768(13) 0.97508(11) 0.0481(10) Uani 1 1 d D A 1 H9A H 0.0328 0.2235 0.9730 0.058 Uiso 1 1 calc R A 1 H9B H 0.0267 0.1776 0.9834 0.058 Uiso 1 1 calc R A 1 C10 C 0.0798(3) 0.1999(3) 1.00460(19) 0.110(3) Uani 1 1 d D A 1 H10A H 0.0703 0.1960 1.0320 0.132 Uiso 1 1 calc R A 1 H10B H 0.0940 0.2254 1.0028 0.132 Uiso 1 1 calc R A 1 C11 C 0.1066(3) 0.1646(3) 0.9906(2) 0.097(3) Uani 0.75 1 d P A 1 H11A H 0.1335 0.1668 1.0017 0.116 Uiso 1 1 calc R A 1 H11B H 0.0951 0.1390 0.9986 0.116 Uiso 1 1 calc R A 1 C12 C 0.10703(12) 0.16893(14) 0.94571(16) 0.0546(12) Uani 1 1 d D A 1 H12A H 0.1112 0.1430 0.9328 0.066 Uiso 1 1 calc R A 1 H12B H 0.1282 0.1872 0.9373 0.066 Uiso 1 1 calc R A 1 C13 C 0.07233(10) 0.22193(10) 0.90760(10) 0.0288(7) Uani 1 1 d . . . O2 O 0.07344(8) 0.21442(7) 0.87002(7) 0.0327(6) Uani 1 1 d . A . O3 O 0.07794(8) 0.25497(7) 0.92260(7) 0.0369(6) Uani 1 1 d . A . O1S O -0.1250 0.0000 0.7500 0.165(8) Uiso 0.50 4 d SP . . O2S O -0.1250 -0.0300(19) 0.7800(19) 0.165(8) Uiso 0.13 2 d SP . . O3S O -0.1250 0.0238(19) 0.7738(19) 0.165(8) Uiso 0.13 2 d SP . . O4S O 0.1025(10) 0.1025(10) 1.1025(10) 0.165(8) Uiso 0.25 3 d SP . . O5S O 0.0699(10) 0.0699(10) 1.0699(10) 0.165(8) Uiso 0.25 3 d SP . . O6S O 0.0446(10) 0.0446(10) 1.0446(10) 0.165(8) Uiso 0.25 3 d SP . . C11A C 0.1197(9) 0.1939(9) 0.9822(6) 0.100(9) Uiso 0.25 1 d PD B 2 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 Cu1 0.0305(3) 0.0214(3) 0.0274(3) -0.00024(15) 0.00752(16) 0.00015(15) O1 0.0331(13) 0.0223(12) 0.0391(14) -0.0024(10) 0.0142(10) -0.0030(9) C1 0.0280(17) 0.0220(16) 0.042(2) 0.0021(14) 0.0066(14) 0.0018(13) C2 0.037(2) 0.0336(19) 0.052(2) -0.0097(17) 0.0047(17) 0.0019(16) C3 0.041(2) 0.049(3) 0.093(4) -0.034(3) 0.010(2) -0.009(2) C4 0.047(3) 0.055(3) 0.125(5) -0.041(3) 0.043(3) -0.025(2) C5 0.048(2) 0.043(2) 0.078(3) -0.018(2) 0.037(2) -0.011(2) C6 0.0329(19) 0.0227(16) 0.044(2) -0.0006(14) 0.0100(15) 0.0013(14) C7 0.041(2) 0.0285(18) 0.0295(18) 0.0059(14) 0.0096(15) -0.0019(15) N1 0.0212(14) 0.0245(14) 0.0281(14) 0.0012(11) 0.0029(11) 0.0021(11) C8 0.0315(18) 0.0322(18) 0.0288(18) 0.0011(14) -0.0003(14) -0.0013(14) C9 0.064(3) 0.050(2) 0.030(2) -0.0060(17) 0.0082(19) -0.021(2) C10 0.139(7) 0.139(6) 0.051(4) -0.011(4) -0.035(4) -0.016(6) C11 0.141(8) 0.075(5) 0.076(5) 0.010(4) -0.082(6) 0.006(5) C12 0.033(2) 0.047(2) 0.084(3) 0.015(2) -0.018(2) -0.0036(18) C13 0.0256(16) 0.0277(18) 0.0331(18) -0.0027(14) 0.0020(14) -0.0009(13) O2 0.0450(14) 0.0229(12) 0.0302(13) -0.0007(9) 0.0060(11) -0.0032(10) O3 0.0488(15) 0.0288(13) 0.0331(13) -0.0044(10) 0.0033(11) -0.0038(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.950(2) 22_455 ? Cu1 O1 1.952(2) . ? Cu1 O2 1.954(2) . ? Cu1 N1 1.987(3) . ? Cu1 O3 2.249(2) 64_567 ? Cu1 Cu1 3.0401(8) 22_455 ? O1 C1 1.344(4) . ? O1 Cu1 1.950(2) 22_455 ? C1 C2 1.388(5) . ? C1 C6 1.401(5) . ? C2 C3 1.372(6) . ? C3 C4 1.384(7) . ? C4 C5 1.386(7) . ? C5 C6 1.377(5) . ? C6 C7 1.506(5) . ? C7 N1 1.489(4) . ? N1 C8 1.489(4) . ? C8 C13 1.531(5) . ? C8 C9 1.536(5) . ? C8 C12 1.563(5) . ? C9 C10 1.501(8) . ? C10 C11 1.558(12) . ? C11 C12 1.514(9) . ? C13 O3 1.231(4) . ? C13 O2 1.286(4) . ? O3 Cu1 2.249(2) 87_557 ? O1S O3S 1.13(9) . ? O1S O3S 1.13(9) 28_446 ? O1S O2S 1.42(9) . ? O1S O2S 1.42(9) 28_446 ? O2S O3S 1.81(8) 28_446 ? O2S O3S 1.81(8) . ? O3S O2S 1.81(8) 28_446 ? O5S O6S 1.47(7) . ? 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 O1 Cu1 O1 77.40(10) 22_455 . ? O1 Cu1 O2 101.70(10) 22_455 . ? O1 Cu1 O2 166.47(11) . . ? O1 Cu1 N1 158.08(11) 22_455 . ? O1 Cu1 N1 93.12(11) . . ? O2 Cu1 N1 82.89(10) . . ? O1 Cu1 O3 107.01(10) 22_455 64_567 ? O1 Cu1 O3 100.21(10) . 64_567 ? O2 Cu1 O3 92.99(10) . 64_567 ? N1 Cu1 O3 94.02(10) . 64_567 ? O1 Cu1 Cu1 38.85(7) 22_455 22_455 ? O1 Cu1 Cu1 38.81(7) . 22_455 ? O2 Cu1 Cu1 137.54(7) . 22_455 ? N1 Cu1 Cu1 127.41(8) . 22_455 ? O3 Cu1 Cu1 110.92(7) 64_567 22_455 ? C1 O1 Cu1 135.6(2) . 22_455 ? C1 O1 Cu1 115.1(2) . . ? Cu1 O1 Cu1 102.34(10) 22_455 . ? O1 C1 C2 121.2(3) . . ? O1 C1 C6 118.4(3) . . ? C2 C1 C6 120.4(3) . . ? C3 C2 C1 119.9(4) . . ? C2 C3 C4 120.3(4) . . ? C3 C4 C5 119.7(4) . . ? C6 C5 C4 121.1(4) . . ? C5 C6 C1 118.6(4) . . ? C5 C6 C7 122.0(4) . . ? C1 C6 C7 119.4(3) . . ? N1 C7 C6 111.5(3) . . ? C7 N1 C8 118.0(3) . . ? C7 N1 Cu1 114.8(2) . . ? C8 N1 Cu1 105.2(2) . . ? N1 C8 C13 106.2(3) . . ? N1 C8 C9 113.8(3) . . ? C13 C8 C9 113.1(3) . . ? N1 C8 C12 112.1(3) . . ? C13 C8 C12 106.5(3) . . ? C9 C8 C12 105.1(3) . . ? C10 C9 C8 106.5(4) . . ? C9 C10 C11 101.2(5) . . ? C12 C11 C10 103.5(5) . . ? C11 C12 C8 104.8(5) . . ? O3 C13 O2 124.9(3) . . ? O3 C13 C8 119.1(3) . . ? O2 C13 C8 116.0(3) . . ? C13 O2 Cu1 113.9(2) . . ? C13 O3 Cu1 129.7(2) . 87_557 ? O3S O1S O3S 180(9) . 28_446 ? O3S O1S O2S 90.001(12) . . ? O3S O1S O2S 89.999(16) 28_446 . ? O3S O1S O2S 89.999(17) . 28_446 ? O3S O1S O2S 90.001(11) 28_446 28_446 ? O2S O1S O2S 180(4) . 28_446 ? O1S O2S O3S 38(3) . 28_446 ? O1S O2S O3S 38(3) . . ? O3S O2S O3S 77(6) 28_446 . ? O1S O3S O2S 52(3) . . ? O1S O3S O2S 52(3) . 28_446 ? O2S O3S O2S 103(6) . 28_446 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.590 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.113 #=====#END _data_compound 3 #data_bs9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H46 Cu2 N2 O10' _chemical_formula_weight 745.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5399(6) _cell_length_b 10.3300(8) _cell_length_c 11.3540(9) _cell_angle_alpha 81.523(2) _cell_angle_beta 73.016(2) _cell_angle_gamma 78.365(2) _cell_volume 824.68(11) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2805 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 29.12 _exptl_crystal_description rod _exptl_crystal_colour greenish _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 390 _exptl_absorpt_coefficient_mu 1.349 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5151 _exptl_absorpt_correction_T_max 0.8622 _exptl_absorpt_process_details 'Sadabs (Sheldrick 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6784 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 30.02 _reflns_number_total 4514 _reflns_number_gt 3613 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS, SMART' _computing_cell_refinement 'Bruker AXS, SAINT' _computing_data_reduction 'Bruker AXS, SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS, SHELXTL' _computing_publication_material 'Bruker AXS, SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+0.5524P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4514 _refine_ls_number_parameters 222 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.0909 _refine_ls_wR_factor_gt 0.0886 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.64017(4) 0.54292(3) 0.55055(3) 0.02438(9) Uani 1 1 d . . . O1 O 0.4774(2) 0.61131(16) 0.43967(15) 0.0253(4) Uani 1 1 d . . . C1 C 0.5098(3) 0.7112(2) 0.3498(2) 0.0258(5) Uani 1 1 d . . . C2 C 0.4753(4) 0.7094(3) 0.2364(2) 0.0354(6) Uani 1 1 d . . . H2 H 0.4302 0.6366 0.2215 0.042 Uiso 1 1 calc R . . C3 C 0.5065(4) 0.8135(3) 0.1452(3) 0.0410(7) Uani 1 1 d . . . H3 H 0.4824 0.8105 0.0690 0.049 Uiso 1 1 calc R . . C4 C 0.5723(4) 0.9214(3) 0.1645(3) 0.0386(6) Uani 1 1 d . . . H4 H 0.5913 0.9928 0.1031 0.046 Uiso 1 1 calc R . . C5 C 0.6096(4) 0.9222(3) 0.2762(2) 0.0322(6) Uani 1 1 d . . . H5 H 0.6558 0.9952 0.2897 0.039 Uiso 1 1 calc R . . C6 C 0.5816(3) 0.8198(2) 0.3689(2) 0.0267(5) Uani 1 1 d . . . C7 C 0.6258(4) 0.8231(2) 0.4890(2) 0.0295(5) Uani 1 1 d . . . H7A H 0.6811 0.9022 0.4854 0.035 Uiso 1 1 calc R . . H7B H 0.5097 0.8280 0.5567 0.035 Uiso 1 1 calc R . . N1 N 0.7596(3) 0.7020(2) 0.51278(19) 0.0240(4) Uani 1 1 d . . . H1 H 0.845(4) 0.690(2) 0.440(2) 0.022(6) Uiso 1 1 d . . . C8 C 0.8609(3) 0.7026(2) 0.6077(2) 0.0248(5) Uani 1 1 d . . . C9 C 1.0117(4) 0.7938(3) 0.5662(3) 0.0349(6) Uani 1 1 d . . . H9A H 1.1383 0.7409 0.5507 0.042 Uiso 1 1 calc R . . H9B H 1.0001 0.8498 0.4904 0.042 Uiso 1 1 calc R . . C10 C 0.9752(5) 0.8789(3) 0.6726(3) 0.0586(9) Uani 1 1 d . . . H10A H 1.0940 0.8888 0.6863 0.070 Uiso 1 1 calc R . . H10B H 0.9063 0.9673 0.6546 0.070 Uiso 1 1 calc R . . C11 C 0.8587(4) 0.8059(3) 0.7850(3) 0.0462(8) Uani 1 1 d . . . H11A H 0.9382 0.7343 0.8222 0.055 Uiso 1 1 calc R . . H11B H 0.7863 0.8665 0.8475 0.055 Uiso 1 1 calc R . . C12 C 0.7308(4) 0.7513(3) 0.7310(2) 0.0322(6) Uani 1 1 d . . . H12A H 0.6274 0.8206 0.7168 0.039 Uiso 1 1 calc R . . H12B H 0.6782 0.6779 0.7861 0.039 Uiso 1 1 calc R . . C13 C 0.9412(3) 0.5560(2) 0.6356(2) 0.0246(5) Uani 1 1 d . . . O2 O 0.8451(2) 0.47001(16) 0.62646(15) 0.0260(4) Uani 1 1 d . . . O3 O 1.0872(2) 0.52448(17) 0.66942(17) 0.0311(4) Uani 1 1 d . . . O4 O 0.3851(3) 0.6206(3) 0.7121(2) 0.0454(6) Uani 1 1 d D . . H4A H 0.363(5) 0.653(4) 0.766(3) 0.057(12) Uiso 1 1 d D . . H4B H 0.308(4) 0.599(3) 0.706(3) 0.048(11) Uiso 1 1 d D . . O5 O 0.2549(4) 0.7675(3) 0.9193(3) 0.0796(8) Uani 1 1 d . . . C14 C 0.1716(6) 0.7131(5) 1.0192(4) 0.0732(12) Uani 1 1 d . . . C15 C 0.2000(11) 0.5683(7) 1.0340(5) 0.161(3) Uani 1 1 d . . . H15A H 0.3048 0.5338 0.9673 0.242 Uiso 1 1 calc R . . H15B H 0.0871 0.5385 1.0318 0.242 Uiso 1 1 calc R . . H15C H 0.2272 0.5364 1.1126 0.242 Uiso 1 1 calc R . . C16 C 0.0529(6) 0.7789(7) 1.1226(5) 0.138(3) Uani 1 1 d . . . H16A H 0.0441 0.8742 1.1026 0.207 Uiso 1 1 calc R . . H16B H 0.1049 0.7522 1.1929 0.207 Uiso 1 1 calc R . . H16C H -0.0715 0.7554 1.1430 0.207 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 Cu1 0.02153(15) 0.02576(16) 0.03093(17) -0.00017(11) -0.01390(12) -0.00728(11) O1 0.0227(8) 0.0283(9) 0.0302(9) 0.0033(7) -0.0148(7) -0.0094(7) C1 0.0201(11) 0.0285(13) 0.0297(13) 0.0010(10) -0.0094(10) -0.0049(9) C2 0.0384(15) 0.0385(15) 0.0376(15) 0.0022(12) -0.0202(12) -0.0150(12) C3 0.0477(17) 0.0483(18) 0.0341(15) 0.0087(12) -0.0231(13) -0.0155(14) C4 0.0422(16) 0.0351(15) 0.0406(16) 0.0118(12) -0.0188(13) -0.0111(12) C5 0.0303(13) 0.0255(13) 0.0431(16) 0.0005(11) -0.0156(12) -0.0046(10) C6 0.0228(11) 0.0246(12) 0.0346(14) -0.0019(10) -0.0127(10) -0.0015(9) C7 0.0292(13) 0.0247(13) 0.0385(14) -0.0039(10) -0.0160(11) -0.0027(10) N1 0.0208(10) 0.0259(11) 0.0283(11) -0.0030(8) -0.0109(8) -0.0043(8) C8 0.0210(11) 0.0268(12) 0.0315(13) -0.0035(10) -0.0117(10) -0.0081(9) C9 0.0314(13) 0.0327(14) 0.0467(16) 0.0044(12) -0.0172(12) -0.0153(11) C10 0.073(2) 0.048(2) 0.070(2) -0.0100(17) -0.024(2) -0.0338(18) C11 0.0472(17) 0.0517(19) 0.0499(19) -0.0218(15) -0.0212(15) -0.0072(14) C12 0.0296(13) 0.0352(14) 0.0354(14) -0.0110(11) -0.0126(11) -0.0026(11) C13 0.0192(11) 0.0325(13) 0.0241(12) -0.0040(9) -0.0067(9) -0.0064(9) O2 0.0237(8) 0.0250(9) 0.0340(9) -0.0001(7) -0.0146(7) -0.0066(7) O3 0.0226(8) 0.0332(10) 0.0436(11) -0.0046(8) -0.0177(8) -0.0048(7) O4 0.0278(11) 0.0710(17) 0.0458(14) -0.0244(12) -0.0074(10) -0.0174(11) O5 0.083(2) 0.100(2) 0.0681(19) -0.0281(16) -0.0119(16) -0.0419(18) C14 0.053(2) 0.131(4) 0.048(2) -0.007(2) -0.0239(19) -0.029(2) C15 0.272(10) 0.140(6) 0.073(4) 0.022(4) -0.041(5) -0.070(6) C16 0.057(3) 0.253(8) 0.088(4) -0.049(4) -0.024(3) 0.041(4) _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 Cu1 O1 1.9483(16) 2_666 ? Cu1 O2 1.9531(15) . ? Cu1 N1 1.965(2) . ? Cu1 O1 1.9701(15) . ? Cu1 O4 2.336(2) . ? Cu1 Cu1 3.0076(6) 2_666 ? O1 C1 1.346(3) . ? O1 Cu1 1.9483(16) 2_666 ? C1 C2 1.389(3) . ? C1 C6 1.408(3) . ? C2 C3 1.385(4) . ? C3 C4 1.377(4) . ? C4 C5 1.378(4) . ? C5 C6 1.380(3) . ? C6 C7 1.502(3) . ? C7 N1 1.485(3) . ? N1 C8 1.493(3) . ? C8 C13 1.536(3) . ? C8 C12 1.544(3) . ? C8 C9 1.547(3) . ? C9 C10 1.525(4) . ? C10 C11 1.516(5) . ? C11 C12 1.514(4) . ? C13 O3 1.238(3) . ? C13 O2 1.287(3) . ? O5 C14 1.239(5) . ? C14 C16 1.420(6) . ? C14 C15 1.459(7) . ? 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 O1 Cu1 O2 102.50(7) 2_666 . ? O1 Cu1 N1 170.90(8) 2_666 . ? O2 Cu1 N1 83.29(7) . . ? O1 Cu1 O1 79.73(7) 2_666 . ? O2 Cu1 O1 167.37(7) . . ? N1 Cu1 O1 93.11(7) . . ? O1 Cu1 O4 88.11(8) 2_666 . ? O2 Cu1 O4 105.38(8) . . ? N1 Cu1 O4 97.19(9) . . ? O1 Cu1 O4 87.05(8) . . ? O1 Cu1 Cu1 40.13(4) 2_666 2_666 ? O2 Cu1 Cu1 141.20(5) . 2_666 ? N1 Cu1 Cu1 132.47(6) . 2_666 ? O1 Cu1 Cu1 39.60(5) . 2_666 ? O4 Cu1 Cu1 86.84(6) . 2_666 ? C1 O1 Cu1 130.65(14) . 2_666 ? C1 O1 Cu1 123.69(14) . . ? Cu1 O1 Cu1 100.27(7) 2_666 . ? O1 C1 C2 121.2(2) . . ? O1 C1 C6 120.2(2) . . ? C2 C1 C6 118.5(2) . . ? C3 C2 C1 120.8(3) . . ? C4 C3 C2 120.8(2) . . ? C3 C4 C5 118.4(2) . . ? C4 C5 C6 122.3(2) . . ? C5 C6 C1 119.0(2) . . ? C5 C6 C7 121.0(2) . . ? C1 C6 C7 120.0(2) . . ? N1 C7 C6 109.97(19) . . ? C7 N1 C8 118.04(19) . . ? C7 N1 Cu1 111.45(15) . . ? C8 N1 Cu1 108.65(15) . . ? N1 C8 C13 104.74(18) . . ? N1 C8 C12 113.63(19) . . ? C13 C8 C12 106.8(2) . . ? N1 C8 C9 113.4(2) . . ? C13 C8 C9 113.54(19) . . ? C12 C8 C9 104.8(2) . . ? C10 C9 C8 105.8(2) . . ? C11 C10 C9 105.7(2) . . ? C12 C11 C10 102.4(2) . . ? C11 C12 C8 104.0(2) . . ? O3 C13 O2 122.6(2) . . ? O3 C13 C8 120.8(2) . . ? O2 C13 C8 116.53(19) . . ? C13 O2 Cu1 114.37(14) . . ? O5 C14 C16 125.9(6) . . ? O5 C14 C15 117.6(4) . . ? C16 C14 C15 116.5(5) . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 0.643 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.081 #=====#END