Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Shuxia Liu' _publ_contact_author_address ; Key Laboratory of Polyoxometalates Science of Ministry of Education, Northeast Normal Universit College of Chemistry Changchun City JiLin 130024 CHINA ; _publ_contact_author_email LIUSX@NENU.EDU.CN _publ_section_title ; Design and construction of a microporous metal-organic framework based on the pillared-layer motif ; loop_ _publ_author_name 'Shuxia Liu' 'Jianfang Cao' 'Chaoying Gao' 'Yuan-Hang Ren' ; Chunyan Sun ; 'Linhua Xie' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 636900' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H99 N15 Ni3 O27' _chemical_formula_weight 1232.70 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' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P-62m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+y, -x, -z' '-y, x-y, z' 'x, y, -z' '-x+y, -x, z' '-y, x-y, -z' 'y, x, z' 'x-y, -y, -z' '-x, -x+y, z' 'y, x, -z' 'x-y, -y, z' '-x, -x+y, -z' _cell_length_a 16.634(2) _cell_length_b 16.634(2) _cell_length_c 11.234(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2691.9(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.760 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 0.560 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21183 _diffrn_reflns_av_R_equivalents 0.0959 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1774 _reflns_number_gt 1678 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0778P)^2^+0.3251P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(3) _refine_ls_number_reflns 1774 _refine_ls_number_parameters 114 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1206 _refine_ls_wR_factor_gt 0.1188 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1742(4) 0.1742(4) 0.0000 0.0287(16) Uani 1 4 d S A . C2 C 0.0838(4) 0.0838(4) 0.0000 0.0254(15) Uani 1 4 d S . . C3 C 0.0000 0.0830(4) 0.0000 0.0308(16) Uani 1 4 d S . . H3 H 0.0000 0.1389 0.0000 0.037 Uiso 1 4 calc SR . . C4 C 0.5306(3) 0.3923(3) 0.0000 0.0419(14) Uani 1 2 d S A . C5 C 0.6013(3) 0.3626(4) 0.0000 0.0406(14) Uani 1 2 d S . . C6 C 0.5724(3) 0.2684(3) 0.0000 0.0423(15) Uani 1 2 d S . . H6 H 0.5093 0.2249 0.0000 0.051 Uiso 1 2 calc SR . . C7 C 0.3210(3) 0.3210(3) 0.4342(5) 0.0539(12) Uani 1 2 d SD . . C8 C 0.2853(10) 0.3625(10) 0.3684(7) 0.115(6) Uani 0.774(12) 1 d PD A 1 H8 H 0.2555 0.3900 0.4066 0.138 Uiso 0.774(12) 1 calc PR A 1 C9 C 0.2910(10) 0.3660(10) 0.2462(7) 0.101(5) Uani 0.774(12) 1 d P A 1 H9 H 0.2716 0.4021 0.2055 0.122 Uiso 0.774(12) 1 calc PR A 1 C10 C 0.3923(15) 0.3923(15) 0.374(3) 0.063(17) Uani 0.151(8) 2 d SPD A 2 H10 H 0.4410 0.4410 0.4145 0.075 Uiso 0.151(8) 2 calc SPR A 2 C11 C 0.3905(14) 0.3905(14) 0.255(3) 0.12(3) Uani 0.151(8) 2 d SPD A 2 H11 H 0.4395 0.4395 0.2154 0.146 Uiso 0.151(8) 2 calc SPR A 2 C12 C 0.2438(14) 0.2709(15) 0.371(2) 0.10(3) Uani 0.151(8) 1 d PD A 2 H12 H 0.1879 0.2344 0.4106 0.116 Uiso 0.151(8) 1 calc PR A 2 C13 C 0.2456(13) 0.2724(14) 0.2505(18) 0.06(2) Uani 0.151(8) 1 d PD A 2 H13 H 0.1899 0.2365 0.2103 0.075 Uiso 0.151(8) 1 calc PR A 2 N1 N 0.3217(2) 0.3217(2) 0.1861(3) 0.0412(8) Uani 1 2 d SD . . Ni1 Ni 0.31981(4) 0.31981(4) 0.0000 0.0232(2) Uani 1 4 d S . . O1 O 0.2498(2) 0.17319(19) 0.0000 0.0333(8) Uani 1 2 d S . . O2 O 0.4492(2) 0.3340(2) 0.0000 0.0415(11) Uani 1 2 d S . . O3 O 0.5615(3) 0.4786(3) 0.0000 0.104(2) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.022(2) 0.022(2) 0.034(4) 0.000 0.000 0.005(3) C2 0.020(2) 0.020(2) 0.035(4) 0.000 0.000 0.009(3) C3 0.030(4) 0.024(3) 0.041(5) 0.000 0.000 0.0148(18) C4 0.023(3) 0.022(3) 0.080(4) 0.000 0.000 0.011(2) C5 0.023(2) 0.020(2) 0.080(4) 0.000 0.000 0.012(2) C6 0.017(2) 0.015(2) 0.092(5) 0.000 0.000 0.006(2) C7 0.062(3) 0.062(3) 0.043(3) -0.003(2) -0.003(2) 0.035(3) C8 0.221(16) 0.176(14) 0.046(4) -0.013(8) -0.004(8) 0.173(14) C9 0.192(13) 0.148(11) 0.048(4) 0.015(7) 0.014(8) 0.147(11) C10 0.046(16) 0.046(16) 0.000(14) -0.002(9) -0.002(9) -0.050(17) C11 0.05(2) 0.05(2) 0.11(5) 0.018(15) 0.018(15) -0.09(3) C12 0.037(16) 0.08(4) 0.08(2) 0.02(2) 0.018(14) -0.04(2) C13 0.018(10) 0.08(3) 0.019(11) 0.006(15) 0.003(8) -0.031(19) N1 0.0452(16) 0.0452(16) 0.039(2) 0.0004(14) 0.0004(14) 0.027(2) Ni1 0.0151(3) 0.0151(3) 0.0380(4) 0.000 0.000 0.0065(3) O1 0.0161(18) 0.0252(15) 0.058(2) 0.000 0.000 0.0098(15) O2 0.0189(17) 0.029(2) 0.079(3) 0.000 0.000 0.0139(16) O3 0.024(2) 0.021(2) 0.271(7) 0.000 0.000 0.0152(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.267(5) . ? C1 O1 1.267(5) 7 ? C1 C2 1.505(8) . ? C2 C3 1.387(4) 2 ? C2 C3 1.387(4) . ? C3 C2 1.387(4) 3 ? C3 H3 0.9300 . ? C4 O2 1.209(6) . ? C4 O3 1.260(6) . ? C4 C5 1.486(7) . ? C5 C6 1.390(7) . ? C5 C6 1.396(6) 2_665 ? C6 C5 1.396(6) 3_655 ? C6 H6 0.9300 . ? C7 C12 1.33(2) 7 ? C7 C12 1.33(2) . ? C7 C8 1.337(8) 7 ? C7 C8 1.337(8) . ? C7 C10 1.37(3) . ? C7 C7 1.478(10) 4_556 ? C8 C9 1.375(11) . ? C8 H8 0.9300 . ? C9 N1 1.280(7) . ? C9 H9 0.9300 . ? C10 C11 1.33(4) . ? C10 H10 0.9300 . ? C11 N1 1.38(3) . ? C11 H11 0.9300 . ? C12 C13 1.36(3) . ? C12 H12 0.9300 . ? C13 N1 1.33(2) . ? C13 H13 0.9300 . ? N1 C9 1.280(7) 7 ? N1 C13 1.33(2) 7 ? N1 Ni1 2.090(4) . ? Ni1 O2 2.045(3) . ? Ni1 O2 2.045(3) 7 ? Ni1 N1 2.090(4) 4 ? Ni1 O1 2.113(3) . ? Ni1 O1 2.113(3) 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 C1 O1 121.3(6) . 7 ? O1 C1 C2 119.3(3) . . ? O1 C1 C2 119.3(3) 7 . ? C3 C2 C3 119.0(6) 2 . ? C3 C2 C1 120.5(3) 2 . ? C3 C2 C1 120.5(3) . . ? C2 C3 C2 121.0(6) 3 . ? C2 C3 H3 119.5 3 . ? C2 C3 H3 119.5 . . ? O2 C4 O3 124.8(5) . . ? O2 C4 C5 119.2(4) . . ? O3 C4 C5 116.1(4) . . ? C6 C5 C6 119.5(5) . 2_665 ? C6 C5 C4 119.4(4) . . ? C6 C5 C4 121.1(4) 2_665 . ? C5 C6 C5 120.5(5) . 3_655 ? C5 C6 H6 119.8 . . ? C5 C6 H6 119.8 3_655 . ? C12 C7 C12 34.1(14) 7 . ? C12 C7 C8 59.4(10) 7 7 ? C12 C7 C8 88.8(10) . 7 ? C12 C7 C8 88.8(10) 7 . ? C12 C7 C8 59.4(10) . . ? C8 C7 C8 112.7(7) 7 . ? C12 C7 C10 115.2(15) 7 . ? C12 C7 C10 115.2(15) . . ? C8 C7 C10 72.2(9) 7 . ? C8 C7 C10 72.2(9) . . ? C12 C7 C7 122.1(10) 7 4_556 ? C12 C7 C7 122.1(10) . 4_556 ? C8 C7 C7 123.6(4) 7 4_556 ? C8 C7 C7 123.6(4) . 4_556 ? C10 C7 C7 119.8(13) . 4_556 ? C7 C8 C9 122.4(6) . . ? C7 C8 H8 118.8 . . ? C9 C8 H8 118.8 . . ? N1 C9 C8 122.8(6) . . ? N1 C9 H9 118.6 . . ? C8 C9 H9 118.6 . . ? C11 C10 C7 118(2) . . ? C11 C10 H10 120.8 . . ? C7 C10 H10 120.8 . . ? C10 C11 N1 125(2) . . ? C10 C11 H11 117.3 . . ? N1 C11 H11 117.3 . . ? C7 C12 C13 121.0(17) . . ? C7 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? N1 C13 C12 124.1(16) . . ? N1 C13 H13 117.9 . . ? C12 C13 H13 117.9 . . ? C9 N1 C9 115.3(7) 7 . ? C9 N1 C13 62.3(10) 7 7 ? C9 N1 C13 91.6(9) . 7 ? C9 N1 C13 91.6(9) 7 . ? C9 N1 C13 62.3(10) . . ? C13 N1 C13 33.8(14) 7 . ? C9 N1 C11 68.4(9) 7 . ? C9 N1 C11 68.4(9) . . ? C13 N1 C11 110.2(15) 7 . ? C13 N1 C11 110.2(15) . . ? C9 N1 Ni1 121.9(3) 7 . ? C9 N1 Ni1 121.9(3) . . ? C13 N1 Ni1 122.2(9) 7 . ? C13 N1 Ni1 122.2(9) . . ? C11 N1 Ni1 125.0(13) . . ? O2 Ni1 O2 108.57(19) . 7 ? O2 Ni1 N1 89.49(6) . . ? O2 Ni1 N1 89.49(6) 7 . ? O2 Ni1 N1 89.49(6) . 4 ? O2 Ni1 N1 89.49(6) 7 4 ? N1 Ni1 N1 178.3(2) . 4 ? O2 Ni1 O1 94.21(14) . . ? O2 Ni1 O1 157.22(13) 7 . ? N1 Ni1 O1 90.75(8) . . ? N1 Ni1 O1 90.75(8) 4 . ? O2 Ni1 O1 157.22(13) . 7 ? O2 Ni1 O1 94.21(14) 7 7 ? N1 Ni1 O1 90.75(8) . 7 ? N1 Ni1 O1 90.75(8) 4 7 ? O1 Ni1 O1 63.0(2) . 7 ? C1 O1 Ni1 87.8(3) . . ? C4 O2 Ni1 141.6(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.376 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.079 data_compound1 _database_code_depnum_ccdc_archive 'CCDC 636901' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H17 N2 Ni O8' _chemical_formula_weight 412.02 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3)/mcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-y, -x, -z' '-x+y, y, -z' 'x, x-y, -z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' 'y, x, z' 'x-y, -y, z' '-x, -x+y, z' _cell_length_a 16.609(2) _cell_length_b 16.609(2) _cell_length_c 14.325(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3422.2(10) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description hexagon _exptl_crystal_colour yellow-green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1278 _exptl_absorpt_coefficient_mu 0.886 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25128 _diffrn_reflns_av_R_equivalents 0.0765 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1115 _reflns_number_gt 992 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0726P)^2^+3.5333P] 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 1115 _refine_ls_number_parameters 84 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1469 _refine_ls_wR_factor_gt 0.1416 _refine_ls_goodness_of_fit_ref 1.193 _refine_ls_restrained_S_all 1.193 _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 Ni1 Ni 0.67976(4) 0.0000 0.2500 0.0383(4) Uani 1 4 d S . . C1 C 0.8257(4) 0.0000 0.2500 0.0324(14) Uani 1 4 d S . . C2 C 0.9166(3) 0.0000 0.2500 0.0261(12) Uani 1 4 d S . . C3 C 1.0000 0.0836(3) 0.2500 0.0291(13) Uani 1 4 d S . . H3 H 1.0000 0.1396 0.2500 0.035 Uiso 1 4 calc SR . . C4 C 0.6091(3) 0.1377(3) 0.2500 0.0413(12) Uani 1 2 d S . . C5 C 0.6389(3) 0.2398(3) 0.2500 0.0342(11) Uani 1 2 d S . . C6 C 0.7319(3) 0.3056(3) 0.2500 0.0384(11) Uani 1 2 d S . . H6 H 0.7762 0.2869 0.2500 0.046 Uiso 1 2 calc SR . . C7 C 0.6728(7) -0.0298(7) 0.0593(11) 0.078(3) Uani 0.50 1 d P . . H7 H 0.6532 -0.0851 0.0270 0.093 Uiso 0.50 1 calc PR . . C8 C 0.7439(13) 0.0835(12) -0.1089(11) 0.288(9) Uani 1 1 d . . . H8A H 0.7315 0.0631 -0.1727 0.431 Uiso 1 1 calc R . . H8B H 0.8090 0.1093 -0.0961 0.431 Uiso 1 1 calc R . . H8C H 0.7266 0.1300 -0.0985 0.431 Uiso 1 1 calc R . . N1 N 0.6869(6) 0.0000 -0.0436(7) 0.153(5) Uani 1 2 d S . . O1 O 0.8259(2) 0.0752(2) 0.2500 0.0509(10) Uani 1 2 d S . . O2 O 0.6676(2) 0.1148(2) 0.2500 0.0873(19) Uani 1 2 d S . . O3 O 0.5236(2) 0.0829(2) 0.2500 0.0866(19) Uani 1 2 d S . . O4 O 0.6741(6) 0.0000 0.1144(6) 0.141(4) Uani 1 2 d S . . 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 Ni1 0.0173(4) 0.0187(4) 0.0792(7) 0.000 0.000 0.0094(2) C1 0.026(2) 0.024(3) 0.047(4) 0.000 0.000 0.0118(15) C2 0.019(2) 0.018(3) 0.041(3) 0.000 0.000 0.0092(13) C3 0.031(3) 0.023(2) 0.036(3) 0.000 0.000 0.0154(16) C4 0.024(2) 0.022(2) 0.077(3) 0.000 0.000 0.0109(19) C5 0.021(2) 0.019(2) 0.064(3) 0.000 0.000 0.0103(16) C6 0.022(2) 0.024(2) 0.073(3) 0.000 0.000 0.0139(18) C7 0.048(5) 0.053(6) 0.131(11) -0.007(6) -0.010(7) 0.024(4) C8 0.33(2) 0.35(2) 0.153(14) 0.040(11) 0.051(12) 0.139(18) N1 0.143(6) 0.268(15) 0.089(6) 0.000 -0.019(4) 0.134(8) O1 0.0217(16) 0.0249(16) 0.110(3) 0.000 0.000 0.0146(13) O2 0.0269(19) 0.0194(17) 0.220(6) 0.000 0.000 0.0146(15) O3 0.026(2) 0.0177(17) 0.215(6) 0.000 0.000 0.0098(15) O4 0.156(7) 0.200(11) 0.081(5) 0.000 -0.037(4) 0.100(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 Ni1 O4 1.945(8) . ? Ni1 O4 1.945(8) 16_556 ? Ni1 O2 2.015(3) 8 ? Ni1 O2 2.015(3) . ? Ni1 O1 2.102(3) . ? Ni1 O1 2.102(3) 8 ? C1 O1 1.248(4) 8 ? C1 O1 1.248(4) . ? C1 C2 1.509(8) . ? C2 C3 1.387(4) . ? C2 C3 1.387(4) 2_645 ? C3 C2 1.387(4) 3_765 ? C4 O2 1.207(5) . ? C4 O3 1.246(6) . ? C4 C5 1.510(5) . ? C5 C6 1.376(6) . ? C5 C6 1.379(6) 3_665 ? C6 C5 1.379(6) 2_655 ? C7 C7 0.86(2) 23 ? C7 O4 0.926(14) . ? C7 N1 1.535(16) . ? C8 N1 1.543(15) . ? N1 C7 1.535(16) 23 ? N1 C8 1.543(15) 23 ? O4 C7 0.926(14) 23 ? 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 O4 Ni1 O4 174.5(6) . 16_556 ? O4 Ni1 O2 88.42(17) . 8 ? O4 Ni1 O2 88.42(17) 16_556 8 ? O4 Ni1 O2 88.42(17) . . ? O4 Ni1 O2 88.42(17) 16_556 . ? O2 Ni1 O2 110.03(19) 8 . ? O4 Ni1 O1 92.4(3) . . ? O4 Ni1 O1 92.4(3) 16_556 . ? O2 Ni1 O1 155.97(12) 8 . ? O2 Ni1 O1 94.00(13) . . ? O4 Ni1 O1 92.4(3) . 8 ? O4 Ni1 O1 92.4(3) 16_556 8 ? O2 Ni1 O1 94.00(13) 8 8 ? O2 Ni1 O1 155.97(12) . 8 ? O1 Ni1 O1 61.97(16) . 8 ? O1 C1 O1 120.2(5) 8 . ? O1 C1 C2 119.9(3) 8 . ? O1 C1 C2 119.9(3) . . ? C3 C2 C3 120.2(6) . 2_645 ? C3 C2 C1 119.9(3) . . ? C3 C2 C1 119.9(3) 2_645 . ? C2 C3 C2 119.8(6) . 3_765 ? O2 C4 O3 125.0(4) . . ? O2 C4 C5 119.3(4) . . ? O3 C4 C5 115.7(4) . . ? C6 C5 C6 119.4(4) . 3_665 ? C6 C5 C4 119.9(3) . . ? C6 C5 C4 120.7(4) 3_665 . ? C5 C6 C5 120.6(4) . 2_655 ? C7 C7 O4 62.4(7) 23 . ? C7 C7 N1 73.8(4) 23 . ? O4 C7 N1 133.3(10) . . ? C7 N1 C7 32.4(8) . 23 ? C7 N1 C8 111.3(8) . 23 ? C7 N1 C8 142.9(9) 23 23 ? C7 N1 C8 142.9(9) . . ? C7 N1 C8 111.3(8) 23 . ? C8 N1 C8 102.2(14) 23 . ? C1 O1 Ni1 88.9(3) . . ? C4 O2 Ni1 140.8(3) . . ? C7 O4 C7 55.2(14) 23 . ? C7 O4 Ni1 147.1(9) 23 . ? C7 O4 Ni1 147.1(9) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.278 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.084