Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_B108704E _database_code_CSD 164885 _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Can-Zhong Lu' ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; 'Chuan-De Wu' ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; 'Shao-Fang Lu' ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; 'Jia-Cheng Liu' ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; 'Qiang-Jin Wu' ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; 'Hong-Hui Zhuang' ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; 'Jin-Shun Huang' ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; _publ_contact_author_name 'Dr Can-Zhong Lu' _publ_contact_author_address ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; _publ_contact_author_email 'czlu@ms.fjirsm.ac.cn' _publ_contact_author_phone '86-591-3792865' _publ_contact_author_fax '86-591-3714946' _publ_requested_journal 'Chemical Communications' _publ_contact_letter ; Please consider this CIF submission for publication in Chemical Communications ; _publ_section_title ; A Three-dimensional Zeolite-like Organic-inorganic Hybrid Material Constructed From {CuMo~2~O~8~N}n Double Helical Chains Linked via [Cu(4,4กฏ-bpy)]~n~ Fragments ; _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Sheldrick G.M.(1997), The SHELX-97 Manual ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H14 Cu2 Mo2 N2 O11' _chemical_formula_weight 657.19 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' 'Mo' 'Mo' -1.6832 0.6857 '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 7.4488(2) _cell_length_b 9.2576(1) _cell_length_c 13.9332(4) _cell_angle_alpha 71.992(2) _cell_angle_beta 89.745(2) _cell_angle_gamma 73.640(2) _cell_volume 873.14(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2182 _cell_measurement_theta_min 1.54 _cell_measurement_theta_max 25.04 _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Green' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 _exptl_absorpt_coefficient_mu 3.867 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.5340 _exptl_absorpt_correction_T_max 0.8913 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 4567 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0988 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.04 _reflns_number_total 3052 _reflns_number_gt 2137 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0004(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3052 _refine_ls_number_parameters 266 _refine_ls_number_restraints 9 _refine_ls_R_factor_ref 0.0922 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1328 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.997 _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 Mo1 Mo 0.19658(12) 0.68816(10) 0.50206(6) 0.0172(3) Uani 1 1 d . . . Mo2 Mo -0.62994(12) 1.00472(10) 0.60852(6) 0.0176(3) Uani 1 1 d . . . Cu1 Cu -0.10258(17) 0.93012(13) 0.60092(9) 0.0178(3) Uani 1 1 d . . . Cu2 Cu -0.30357(17) 0.66426(13) 0.57469(9) 0.0192(3) Uani 1 1 d . . . O1 O -0.6547(10) 0.9462(8) 0.7350(5) 0.0312(18) Uani 1 1 d . . . OW1 O 0.4579(18) 0.3310(13) 0.7235(8) 0.079(4) Uani 1 1 d D . . HW1 H 0.4349 0.3583 0.7801 0.119 Uiso 1 1 d GD . . HW2 H 0.3446 0.3366 0.6967 0.119 Uiso 1 1 d GD . . O2 O 0.1835(10) 0.8529(7) 0.3924(5) 0.0237(16) Uani 1 1 d . . . OW2 O -0.6957(16) 0.9841(14) 0.9297(8) 0.068(3) Uani 1 1 d D . . HW3 H -0.6111 1.0349 0.9008 0.101 Uiso 1 1 d GD . . HW4 H -0.7112 0.9282 0.8887 0.101 Uiso 1 1 d GD . . O3 O -0.6491(9) 1.2090(7) 0.5710(5) 0.0224(16) Uani 1 1 d . . . OW3 O 0.4338(19) 0.2407(12) 0.9298(8) 0.077(3) Uani 1 1 d D . . HW5 H 0.4206 0.3265 0.8744 0.116 Uiso 1 1 d GD . . HW6 H 0.4259 0.1612 0.9067 0.116 Uiso 1 1 d GD . . O4 O -0.8167(9) 0.9673(7) 0.5484(5) 0.0187(15) Uani 1 1 d . . . O5 O 0.1948(9) 0.5298(7) 0.4598(5) 0.0224(16) Uani 1 1 d . . . O6 O 0.4040(9) 0.6332(8) 0.5796(5) 0.0253(17) Uani 1 1 d . . . O7 O -0.0025(9) 0.7244(7) 0.5742(5) 0.0211(16) Uani 1 1 d . . . O8 O -0.4023(9) 0.8806(7) 0.5950(5) 0.0191(15) Uani 1 1 d . . . N1 N -0.0265(12) 0.8348(9) 0.7486(6) 0.021(2) Uani 1 1 d . . . N2 N -0.2426(11) 0.5430(9) 0.7236(6) 0.022(2) Uani 1 1 d . . . C1 C -0.1436(14) 0.3835(11) 0.9330(7) 0.022(2) Uani 1 1 d . . . C2 C -0.0613(18) 0.3217(14) 0.8596(8) 0.039(3) Uani 1 1 d . . . H2A H 0.0284 0.2225 0.8793 0.047 Uiso 1 1 calc R . . C3 C -0.1089(17) 0.4033(13) 0.7586(8) 0.037(3) Uani 1 1 d . . . H3A H -0.0453 0.3594 0.7119 0.045 Uiso 1 1 calc R . . C4 C -0.3330(16) 0.6014(12) 0.7943(8) 0.033(3) Uani 1 1 d . . . H4A H -0.4308 0.6957 0.7728 0.040 Uiso 1 1 calc R . . C5 C -0.2860(15) 0.5271(13) 0.8961(8) 0.033(3) Uani 1 1 d . . . H5A H -0.3504 0.5733 0.9417 0.039 Uiso 1 1 calc R . . C6 C -0.1010(15) 0.9069(12) 0.8158(8) 0.029(3) Uani 1 1 d . . . H6A H -0.1912 1.0056 0.7920 0.035 Uiso 1 1 calc R . . C7 C 0.1034(15) 0.6956(13) 0.7844(8) 0.032(3) Uani 1 1 d . . . H7A H 0.1562 0.6436 0.7390 0.038 Uiso 1 1 calc R . . C8 C 0.1646(17) 0.6233(13) 0.8868(8) 0.036(3) Uani 1 1 d . . . H8A H 0.2581 0.5263 0.9080 0.044 Uiso 1 1 calc R . . C9 C -0.0492(17) 0.8404(12) 0.9190(8) 0.034(3) Uani 1 1 d . . . H9A H -0.1063 0.8935 0.9630 0.041 Uiso 1 1 calc R . . C10 C 0.0880(14) 0.6943(11) 0.9570(7) 0.023(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0196(5) 0.0158(5) 0.0139(5) -0.0046(4) 0.0008(4) -0.0019(4) Mo2 0.0183(5) 0.0174(5) 0.0156(5) -0.0060(4) 0.0004(4) -0.0022(4) Cu1 0.0211(7) 0.0169(6) 0.0147(7) -0.0058(5) 0.0016(5) -0.0034(5) Cu2 0.0238(7) 0.0166(6) 0.0154(7) -0.0059(5) -0.0003(5) -0.0025(5) O1 0.042(5) 0.031(4) 0.021(4) -0.009(3) 0.003(3) -0.011(4) OW1 0.154(11) 0.060(7) 0.039(6) -0.015(5) -0.005(7) -0.055(8) O2 0.034(4) 0.022(4) 0.018(4) -0.009(3) 0.005(3) -0.010(3) OW2 0.074(8) 0.085(8) 0.052(7) -0.042(6) 0.010(5) -0.014(6) O3 0.023(4) 0.026(4) 0.018(4) -0.010(3) 0.001(3) -0.003(3) OW3 0.100(9) 0.054(7) 0.064(7) -0.008(5) 0.007(7) -0.014(7) O4 0.024(4) 0.015(3) 0.014(4) -0.003(3) -0.004(3) -0.003(3) O5 0.025(4) 0.018(4) 0.021(4) -0.007(3) -0.002(3) 0.000(3) O6 0.020(4) 0.026(4) 0.028(4) -0.008(3) -0.006(3) -0.004(3) O7 0.022(4) 0.023(4) 0.015(4) -0.007(3) 0.000(3) 0.001(3) O8 0.021(4) 0.015(3) 0.018(4) -0.006(3) 0.001(3) -0.001(3) N1 0.030(5) 0.010(4) 0.019(5) 0.000(4) -0.005(4) -0.004(4) N2 0.016(5) 0.021(5) 0.026(5) -0.007(4) 0.001(4) -0.002(4) C1 0.024(6) 0.023(6) 0.015(6) 0.000(4) 0.001(4) -0.008(5) C2 0.053(8) 0.031(6) 0.020(6) -0.006(5) -0.004(6) 0.006(6) C3 0.053(8) 0.029(6) 0.017(6) -0.011(5) -0.007(5) 0.012(6) C4 0.035(7) 0.021(6) 0.028(7) 0.002(5) -0.010(5) 0.005(5) C5 0.027(6) 0.036(7) 0.024(6) -0.013(5) 0.004(5) 0.011(5) C6 0.033(7) 0.023(6) 0.018(6) -0.001(5) 0.000(5) 0.005(5) C7 0.032(7) 0.036(7) 0.022(6) -0.011(5) 0.003(5) 0.000(5) C8 0.040(7) 0.023(6) 0.029(7) 0.000(5) -0.015(6) 0.009(5) C9 0.052(8) 0.026(6) 0.014(6) -0.009(5) -0.001(5) 0.009(6) C10 0.029(6) 0.018(5) 0.019(6) -0.006(4) -0.002(5) -0.004(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 Mo1 O5 1.744(6) . ? Mo1 O6 1.745(6) . ? Mo1 O2 1.774(6) . ? Mo1 O7 1.799(7) . ? Mo2 O1 1.702(7) . ? Mo2 O3 1.763(6) . ? Mo2 O4 1.794(6) . ? Mo2 O8 1.807(6) . ? Cu1 O2 1.960(6) 2_576 ? Cu1 N1 1.984(8) . ? Cu1 O7 1.989(6) . ? Cu1 O4 2.015(6) 2_476 ? Cu1 O4 2.330(7) 1_655 ? Cu1 O8 2.409(7) . ? Cu2 O5 1.956(6) 2_566 ? Cu2 O3 1.980(6) 2_476 ? Cu2 N2 2.014(8) . ? Cu2 O8 2.038(6) . ? Cu2 O6 2.274(7) 1_455 ? O2 Cu1 1.960(6) 2_576 ? O3 Cu2 1.980(6) 2_476 ? O4 Cu1 2.015(6) 2_476 ? O4 Cu1 2.330(7) 1_455 ? O5 Cu2 1.956(6) 2_566 ? O6 Cu2 2.274(7) 1_655 ? N1 C7 1.323(12) . ? N1 C6 1.343(12) . ? N2 C3 1.338(12) . ? N2 C4 1.354(14) . ? C1 C2 1.381(14) . ? C1 C5 1.394(13) . ? C1 C10 1.481(13) 2_567 ? C2 C3 1.370(14) . ? C4 C5 1.369(14) . ? C6 C9 1.386(13) . ? C7 C8 1.391(14) . ? C8 C10 1.377(14) . ? C9 C10 1.392(13) . ? C10 C1 1.481(13) 2_567 ? 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 O5 Mo1 O6 108.2(3) . . ? O5 Mo1 O2 106.6(3) . . ? O6 Mo1 O2 112.0(3) . . ? O5 Mo1 O7 107.9(3) . . ? O6 Mo1 O7 109.8(3) . . ? O2 Mo1 O7 112.1(3) . . ? O1 Mo2 O3 107.0(3) . . ? O1 Mo2 O4 106.4(3) . . ? O3 Mo2 O4 111.8(3) . . ? O1 Mo2 O8 105.1(3) . . ? O3 Mo2 O8 114.0(3) . . ? O4 Mo2 O8 111.9(3) . . ? O2 Cu1 N1 93.0(3) 2_576 . ? O2 Cu1 O7 170.9(3) 2_576 . ? N1 Cu1 O7 93.7(3) . . ? O2 Cu1 O4 85.4(3) 2_576 2_476 ? N1 Cu1 O4 178.4(3) . 2_476 ? O7 Cu1 O4 87.8(2) . 2_476 ? O2 Cu1 O4 89.4(3) 2_576 1_655 ? N1 Cu1 O4 97.9(3) . 1_655 ? O7 Cu1 O4 83.6(2) . 1_655 ? O4 Cu1 O4 82.3(2) 2_476 1_655 ? O2 Cu1 O8 100.2(3) 2_576 . ? N1 Cu1 O8 100.1(3) . . ? O7 Cu1 O8 84.7(2) . . ? O4 Cu1 O8 79.9(2) 2_476 . ? O4 Cu1 O8 159.0(2) 1_655 . ? O5 Cu2 O3 90.4(3) 2_566 2_476 ? O5 Cu2 N2 91.1(3) 2_566 . ? O3 Cu2 N2 176.1(3) 2_476 . ? O5 Cu2 O8 172.8(3) 2_566 . ? O3 Cu2 O8 83.7(3) 2_476 . ? N2 Cu2 O8 94.6(3) . . ? O5 Cu2 O6 93.0(3) 2_566 1_455 ? O3 Cu2 O6 92.2(3) 2_476 1_455 ? N2 Cu2 O6 91.2(3) . 1_455 ? O8 Cu2 O6 91.4(3) . 1_455 ? Mo1 O2 Cu1 120.5(4) . 2_576 ? Mo2 O3 Cu2 119.5(3) . 2_476 ? Mo2 O4 Cu1 122.2(3) . 2_476 ? Mo2 O4 Cu1 132.5(3) . 1_455 ? Cu1 O4 Cu1 97.7(2) 2_476 1_455 ? Mo1 O5 Cu2 156.2(4) . 2_566 ? Mo1 O6 Cu2 140.8(4) . 1_655 ? Mo1 O7 Cu1 121.6(4) . . ? Mo2 O8 Cu2 135.4(4) . . ? Mo2 O8 Cu1 128.1(3) . . ? Cu2 O8 Cu1 96.5(2) . . ? C7 N1 C6 117.2(9) . . ? C7 N1 Cu1 120.2(7) . . ? C6 N1 Cu1 122.6(6) . . ? C3 N2 C4 116.3(9) . . ? C3 N2 Cu2 122.4(7) . . ? C4 N2 Cu2 121.2(7) . . ? C2 C1 C5 114.9(9) . . ? C2 C1 C10 123.6(9) . 2_567 ? C5 C1 C10 121.5(9) . 2_567 ? C3 C2 C1 121.4(10) . . ? N2 C3 C2 123.2(10) . . ? N2 C4 C5 122.6(10) . . ? C4 C5 C1 121.3(10) . . ? N1 C6 C9 122.8(9) . . ? N1 C7 C8 123.0(10) . . ? C10 C8 C7 120.6(10) . . ? C6 C9 C10 120.2(10) . . ? C8 C10 C9 116.2(9) . . ? C8 C10 C1 121.8(9) . 2_567 ? C9 C10 C1 122.0(9) . 2_567 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.081 _refine_diff_density_min -1.321 _refine_diff_density_rms 0.239