# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 1145/156 data_1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C H Mo0.50 N0.50 O1.50' _chemical_formula_weight 91.99 _chemical_melting_point ? _chemical_compound_source ? 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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' _cell_length_a 5.2702(15) _cell_length_b 5.2674(7) _cell_length_c 14.2310(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 395.06(13) _cell_formula_units_Z 8 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used 18 _cell_measurement_theta_min 5.47 _cell_measurement_theta_max 12.67 _exptl_crystal_description PLATE _exptl_crystal_colour LIGHT-COLOURED _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.093 _exptl_crystal_density_method ? _exptl_crystal_F_000 348 _exptl_absorpt_coefficient_mu 3.181 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.8009 _exptl_absorpt_correction_T_max 0.9911 _exptl_special_details ; ? ; _diffrn_ambient_temperature 297(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 4.36 _diffrn_reflns_number 438 _diffrn_reflns_av_R_equivalents 0.0159 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 27.50 _reflns_number_total 375 _reflns_number_observed 361 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0154P)^2^+0.2956P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0301(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(16) _refine_ls_number_reflns 374 _refine_ls_number_parameters 35 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0179 _refine_ls_R_factor_obs 0.0169 _refine_ls_wR_factor_all 0.0433 _refine_ls_wR_factor_obs 0.0414 _refine_ls_goodness_of_fit_all 1.194 _refine_ls_goodness_of_fit_obs 1.201 _refine_ls_restrained_S_all 1.230 _refine_ls_restrained_S_obs 1.201 _refine_ls_shift/esd_max 0.157 _refine_ls_shift/esd_mean 0.025 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.5000 0.5000 0.72713(2) 0.0139(2) Uani 1 d S . O1 O 0.5000 0.5000 0.6090(2) 0.0193(7) Uani 1 d S . O2 O 0.7009(5) 0.7987(5) 0.7495(3) 0.0162(5) Uani 1 d . . N1 N 0.5000 0.5000 0.9016(2) 0.0157(8) Uani 1 d S . C1A C 0.4975(37) 0.2824(11) 0.9514(4) 0.0162(11) Uiso 0.50 d P . H1A H 0.4963(37) 0.1034(11) 0.9105(4) 0.019 Uiso 0.50 d PR . C1B C 0.7169(11) 0.5047(38) 0.9506(4) 0.0158(11) Uiso 0.50 d P . H1B H 0.8554(11) 0.5022(38) 0.9207(4) 0.019 Uiso 0.50 d PR . 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 0.0156(3) 0.0162(3) 0.0100(2) 0.000 0.000 -0.0005(4) O1 0.023(2) 0.021(2) 0.0137(14) 0.000 0.000 -0.005(16) O2 0.0130(11) 0.0138(11) 0.0220(11) 0.003(2) -0.002(2) -0.0028(13) N1 0.020(2) 0.015(2) 0.012(2) 0.000 0.000 0.007(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 Mo1 O1 1.681(3) . ? Mo1 O2 1.923(3) . ? Mo1 O2 1.923(3) 2_665 ? Mo1 O2 1.929(3) 7_646 ? Mo1 O2 1.929(3) 8_466 ? Mo1 N1 2.483(3) . ? O2 Mo1 1.929(3) 7_656 ? N1 C1B 1.339(6) . ? N1 C1B 1.339(6) 2_665 ? N1 C1A 1.347(6) 2_665 ? N1 C1A 1.347(6) . ? C1A C1A 1.385(11) 3_657 ? C1A C1B 1.59(2) 2_665 ? C1A C1B 1.65(2) . ? C1B C1B 1.407(11) 4_567 ? C1B C1A 1.59(2) 2_665 ? 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 Mo1 O2 99.52(14) . . ? O1 Mo1 O2 99.52(14) . 2_665 ? O2 Mo1 O2 161.0(3) . 2_665 ? O1 Mo1 O2 99.95(14) . 7_646 ? O2 Mo1 O2 88.35(3) . 7_646 ? O2 Mo1 O2 88.38(3) 2_665 7_646 ? O1 Mo1 O2 99.95(14) . 8_466 ? O2 Mo1 O2 88.38(3) . 8_466 ? O2 Mo1 O2 88.35(3) 2_665 8_466 ? O2 Mo1 O2 160.1(3) 7_646 8_466 ? O1 Mo1 N1 180.0 . . ? O2 Mo1 N1 80.48(14) . . ? O2 Mo1 N1 80.48(14) 2_665 . ? O2 Mo1 N1 80.05(14) 7_646 . ? O2 Mo1 N1 80.05(14) 8_466 . ? Mo1 O2 Mo1 158.19(14) . 7_656 ? C1B N1 C1B 117.3(5) . 2_665 ? C1B N1 C1A 72.7(11) . 2_665 ? C1B N1 C1A 75.6(11) 2_665 2_665 ? C1B N1 C1A 75.6(11) . . ? C1B N1 C1A 72.7(11) 2_665 . ? C1A N1 C1A 116.6(5) 2_665 . ? C1B N1 Mo1 121.4(3) . . ? C1B N1 Mo1 121.4(3) 2_665 . ? C1A N1 Mo1 121.7(3) 2_665 . ? C1A N1 Mo1 121.7(3) . . ? N1 C1A C1A 121.7(3) . 3_657 ? N1 C1A C1B 53.4(5) . 2_665 ? C1A C1A C1B 91.2(12) 3_657 2_665 ? N1 C1A C1B 52.0(6) . . ? C1A C1A C1B 89.6(12) 3_657 . ? C1B C1A C1B 89.9(4) 2_665 . ? N1 C1B C1B 121.3(3) . 4_567 ? N1 C1B C1A 53.9(6) . 2_665 ? C1B C1B C1A 91.0(11) 4_567 2_665 ? N1 C1B C1A 52.4(5) . . ? C1B C1B C1A 88.2(12) 4_567 . ? C1A C1B C1A 90.1(4) 2_665 . ? _refine_diff_density_max 0.406 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.100 #===END data_2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C2 H5 Cu Mo N O4' _chemical_formula_weight 266.55 _chemical_melting_point ? _chemical_compound_source ? 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.568(2) _cell_length_b 6.829(2) _cell_length_c 9.2460(12) _cell_angle_alpha 100.716(12) _cell_angle_beta 101.521(15) _cell_angle_gamma 112.50(3) _cell_volume 304.56(13) _cell_formula_units_Z 2 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used 16 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 9.96 _exptl_crystal_description PRISM _exptl_crystal_colour BLUE _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.907 _exptl_crystal_density_method ? _exptl_crystal_F_000 254 _exptl_absorpt_coefficient_mu 5.487 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.7592 _exptl_absorpt_correction_T_max 0.9923 _exptl_special_details ; ? ; _diffrn_ambient_temperature 297(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 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.54 _diffrn_reflns_number 1804 _diffrn_reflns_av_R_equivalents 0.0158 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1379 _reflns_number_observed 1218 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 12 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+0.3431P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1367 _refine_ls_number_parameters 82 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_obs 0.0254 _refine_ls_wR_factor_all 0.0606 _refine_ls_wR_factor_obs 0.0532 _refine_ls_goodness_of_fit_all 1.067 _refine_ls_goodness_of_fit_obs 1.089 _refine_ls_restrained_S_all 1.170 _refine_ls_restrained_S_obs 1.089 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.69786(7) 0.66168(5) 0.38921(4) 0.01174(9) Uani 1 d . . Cu1 Cu 0.44127(9) 0.88429(7) 0.61938(5) 0.01106(11) Uani 1 d . . O1 O 0.7812(7) 0.6991(5) 0.2242(4) 0.0263(7) Uani 1 d . . O2 O 0.9979(6) 0.7583(5) 0.5351(4) 0.0255(7) Uani 1 d . . O3 O 0.4974(6) 0.3703(5) 0.3542(3) 0.0181(6) Uani 1 d . . O4 O 0.5052(6) 0.8255(4) 0.4174(3) 0.0129(5) Uani 1 d . . N1 N 0.4481(7) 0.9882(5) 0.8369(3) 0.0148(6) Uani 1 d . . H1N H 0.4012(7) 1.1026(5) 0.8427(3) 0.018 Uiso 1 calc R . C1 C 0.7265(9) 1.0792(8) 0.9427(4) 0.0240(9) Uani 1 d . . H1A H 0.8489(9) 1.1931(8) 0.9085(4) 0.029 Uiso 1 calc R . H1B H 0.7856(9) 0.9623(8) 0.9382(4) 0.029 Uiso 1 calc R . C2 C 0.2541(9) 0.8233(7) 0.8925(4) 0.0234(9) Uani 1 d . . H2A H 0.2933(9) 0.6957(7) 0.8854(4) 0.028 Uiso 1 calc R . H2B H 0.0700(9) 0.7735(7) 0.8271(4) 0.028 Uiso 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 Mo1 0.0141(2) 0.0113(2) 0.0133(2) 0.00488(11) 0.00595(12) 0.00754(12) Cu1 0.0169(3) 0.0128(2) 0.0082(2) 0.0047(2) 0.0064(2) 0.0092(2) O1 0.042(2) 0.028(2) 0.027(2) 0.0150(13) 0.0223(15) 0.024(2) O2 0.0134(15) 0.029(2) 0.030(2) 0.0080(13) 0.0021(12) 0.0074(13) O3 0.022(2) 0.0151(13) 0.0200(13) 0.0054(10) 0.0055(12) 0.0115(12) O4 0.0192(14) 0.0117(12) 0.0122(12) 0.0058(9) 0.0088(11) 0.0083(11) N1 0.024(2) 0.017(2) 0.0089(13) 0.0059(11) 0.0085(13) 0.0124(14) C1 0.017(2) 0.037(2) 0.010(2) 0.003(2) 0.006(2) 0.005(2) C2 0.022(2) 0.026(2) 0.011(2) 0.0018(15) 0.007(2) 0.000(2) _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 O1 1.717(3) . ? Mo1 O2 1.724(3) . ? Mo1 O3 1.796(3) . ? Mo1 O4 1.842(3) . ? Cu1 O3 1.944(3) 2_666 ? Cu1 O4 1.967(2) . ? Cu1 N1 1.992(3) . ? Cu1 O4 1.993(3) 2_676 ? Cu1 O2 2.190(3) 1_455 ? Cu1 Cu1 2.9801(9) 2_676 ? O2 Cu1 2.190(3) 1_655 ? O3 Cu1 1.944(3) 2_666 ? O4 Cu1 1.993(3) 2_676 ? N1 C1 1.475(5) . ? N1 C2 1.485(5) . ? C1 C2 1.510(5) 2_677 ? C2 C1 1.510(5) 2_677 ? 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 Mo1 O2 107.5(2) . . ? O1 Mo1 O3 107.54(14) . . ? O2 Mo1 O3 111.06(14) . . ? O1 Mo1 O4 103.71(13) . . ? O2 Mo1 O4 113.33(14) . . ? O3 Mo1 O4 113.14(13) . . ? O3 Cu1 O4 87.36(11) 2_666 . ? O3 Cu1 N1 94.69(12) 2_666 . ? O4 Cu1 N1 169.22(13) . . ? O3 Cu1 O4 161.78(12) 2_666 2_676 ? O4 Cu1 O4 82.38(11) . 2_676 ? N1 Cu1 O4 92.75(12) . 2_676 ? O3 Cu1 O2 105.05(13) 2_666 1_455 ? O4 Cu1 O2 97.51(12) . 1_455 ? N1 Cu1 O2 92.19(14) . 1_455 ? O4 Cu1 O2 91.24(12) 2_676 1_455 ? O3 Cu1 Cu1 127.20(9) 2_666 2_676 ? O4 Cu1 Cu1 41.51(7) . 2_676 ? N1 Cu1 Cu1 132.90(10) . 2_676 ? O4 Cu1 Cu1 40.87(7) 2_676 2_676 ? O2 Cu1 Cu1 95.78(9) 1_455 2_676 ? Mo1 O2 Cu1 152.0(2) . 1_655 ? Mo1 O3 Cu1 137.6(2) . 2_666 ? Mo1 O4 Cu1 117.01(13) . . ? Mo1 O4 Cu1 130.45(14) . 2_676 ? Cu1 O4 Cu1 97.62(11) . 2_676 ? C1 N1 C2 110.0(3) . . ? C1 N1 Cu1 110.8(2) . . ? C2 N1 Cu1 115.8(2) . . ? N1 C1 C2 112.7(4) . 2_677 ? N1 C2 C1 111.2(3) . 2_677 ? _refine_diff_density_max 0.570 _refine_diff_density_min -0.907 _refine_diff_density_rms 0.133 #===END data_3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'H Cu1.50 Mo O5' _chemical_formula_weight 272.26 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 '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' '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.358(6) _cell_length_b 5.574(15) _cell_length_c 7.632(6) _cell_angle_alpha 103.74(15) _cell_angle_beta 106.25(9) _cell_angle_gamma 97.37(23) _cell_volume 207.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used 17 _cell_measurement_theta_min 4.97 _cell_measurement_theta_max 10.87 _exptl_crystal_description ? _exptl_crystal_colour 'greenish blue' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.351 _exptl_crystal_density_method ? _exptl_crystal_F_000 253 _exptl_absorpt_coefficient_mu 10.521 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.7616 _exptl_absorpt_correction_T_max 0.9218 _exptl_special_details ; ? ; _diffrn_ambient_temperature 297(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 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.80 _diffrn_reflns_number 988 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 733 _reflns_number_observed 670 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+0.7961P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0264(24) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 729 _refine_ls_number_parameters 71 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_obs 0.0250 _refine_ls_wR_factor_all 0.0721 _refine_ls_wR_factor_obs 0.0645 _refine_ls_goodness_of_fit_all 1.067 _refine_ls_goodness_of_fit_obs 1.080 _refine_ls_restrained_S_all 1.152 _refine_ls_restrained_S_obs 1.080 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.31735(9) 0.28079(8) 0.68873(6) 0.0077(2) Uani 1 d . . Cu1 Cu 0.78647(13) 0.91750(12) 0.80611(9) 0.0092(2) Uani 1 d . . Cu2 Cu 1.0000 0.5000 1.0000 0.0091(3) Uani 1 d S . O1 O 0.2159(9) 0.2674(8) 0.4475(6) 0.0174(9) Uani 1 d . . H1 H 0.1184(9) 0.2657(8) 0.3413(6) 0.026 Uiso 1 d R . O2 O 0.0358(8) 0.2855(7) 0.7713(6) 0.0118(8) Uani 1 d . . O3 O 0.4465(8) 0.0126(8) 0.7214(6) 0.0162(9) Uani 1 d . . O4 O 0.5587(8) 0.5529(7) 0.8243(5) 0.0149(9) Uani 1 d . . O5 O 1.1138(8) 0.8187(7) 0.9434(5) 0.0108(8) Uani 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 0.0095(3) 0.0073(3) 0.0072(3) 0.0022(2) 0.0041(2) 0.0015(2) Cu1 0.0110(4) 0.0091(4) 0.0078(4) 0.0022(3) 0.0030(3) 0.0035(3) Cu2 0.0133(5) 0.0064(5) 0.0096(5) 0.0026(4) 0.0062(4) 0.0022(4) O1 0.026(2) 0.019(2) 0.009(2) 0.003(2) 0.006(2) 0.009(2) O2 0.012(2) 0.011(2) 0.014(2) 0.003(2) 0.008(2) 0.003(2) O3 0.015(2) 0.014(2) 0.020(2) 0.005(2) 0.005(2) 0.003(2) O4 0.018(2) 0.015(2) 0.010(2) 0.003(2) 0.006(2) -0.002(2) O5 0.016(2) 0.009(2) 0.010(2) 0.0033(15) 0.007(2) 0.004(2) _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 O4 1.745(7) . ? Mo1 O1 1.748(4) . ? Mo1 O3 1.767(6) . ? Mo1 O2 1.791(4) . ? Cu1 O3 1.941(5) 1_565 ? Cu1 O1 1.960(5) 2_666 ? Cu1 O5 1.992(5) . ? Cu1 O5 1.998(6) 2_777 ? Cu1 O4 2.287(7) . ? Cu1 O2 2.412(8) 1_665 ? Cu1 Cu1 3.036(6) 2_777 ? Cu2 O2 1.941(5) 2_667 ? Cu2 O2 1.941(5) 1_655 ? Cu2 O5 1.987(6) . ? Cu2 O5 1.987(6) 2_767 ? Cu2 O4 2.463(7) . ? Cu2 O4 2.463(7) 2_767 ? O1 Cu1 1.960(5) 2_666 ? O2 Cu2 1.941(5) 1_455 ? O2 Cu1 2.412(7) 1_445 ? O3 Cu1 1.941(5) 1_545 ? O5 Cu1 1.998(6) 2_777 ? 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 Mo1 O1 111.1(2) . . ? O4 Mo1 O3 109.2(3) . . ? O1 Mo1 O3 110.4(2) . . ? O4 Mo1 O2 108.6(2) . . ? O1 Mo1 O2 108.9(2) . . ? O3 Mo1 O2 108.7(2) . . ? O3 Cu1 O1 96.3(2) 1_565 2_666 ? O3 Cu1 O5 167.5(2) 1_565 . ? O1 Cu1 O5 94.3(2) 2_666 . ? O3 Cu1 O5 91.0(3) 1_565 2_777 ? O1 Cu1 O5 161.2(2) 2_666 2_777 ? O5 Cu1 O5 80.9(2) . 2_777 ? O3 Cu1 O4 87.6(3) 1_565 . ? O1 Cu1 O4 88.5(2) 2_666 . ? O5 Cu1 O4 86.1(3) . . ? O5 Cu1 O4 109.1(2) 2_777 . ? O3 Cu1 O2 94.1(2) 1_565 1_665 ? O1 Cu1 O2 88.0(2) 2_666 1_665 ? O5 Cu1 O2 92.8(2) . 1_665 ? O5 Cu1 O2 74.2(2) 2_777 1_665 ? O4 Cu1 O2 176.29(14) . 1_665 ? O3 Cu1 Cu1 130.7(2) 1_565 2_777 ? O1 Cu1 Cu1 132.3(2) 2_666 2_777 ? O5 Cu1 Cu1 40.54(14) . 2_777 ? O5 Cu1 Cu1 40.4(2) 2_777 2_777 ? O4 Cu1 Cu1 99.9(2) . 2_777 ? O2 Cu1 Cu1 81.5(2) 1_665 2_777 ? O2 Cu2 O2 180.000(1) 2_667 1_655 ? O2 Cu2 O5 86.0(2) 2_667 . ? O2 Cu2 O5 94.0(2) 1_655 . ? O2 Cu2 O5 94.0(2) 2_667 2_767 ? O2 Cu2 O5 86.0(2) 1_655 2_767 ? O5 Cu2 O5 180.0 . 2_767 ? O4 Cu2 O5 81.6(2) . . ? O4 Cu2 O2 92.1(2) . 2_667 ? O4 Cu2 O2 93.3(2) . 1_655 ? Mo1 O1 Cu1 144.5(3) . 2_666 ? Mo1 O2 Cu2 130.0(3) . 1_455 ? Mo1 O2 Cu1 123.6(2) . 1_445 ? Cu2 O2 Cu1 91.7(2) 1_455 1_445 ? Mo1 O3 Cu1 139.8(3) . 1_545 ? Mo1 O4 Cu1 143.1(2) . . ? Cu2 O5 Cu1 107.4(3) . . ? Cu2 O5 Cu1 104.0(2) . 2_777 ? Cu1 O5 Cu1 99.1(2) . 2_777 ? _refine_diff_density_max 0.802 _refine_diff_density_min -0.856 _refine_diff_density_rms 0.187 #===END