Hybrid compounds assembled from copper-triazole complex and polyoxometalate acid as advanced catalysts for olefins oxidation with oxygen
Jia, Mingjun; Song, Xiaojing; Yan, Yan; Wang, Yanning; Hu, Dianwen; Xiao, Lina; Yu, Jie-hui; Zhang, Wenxiang; Dalton Transactions  (2017) –; doi:10.1039/C7DT03198J

data_7044700
_publ_section_title
;
 Hybrid compounds assembled from copper-triazole complex and
 polyoxometalate acid as advanced catalysts for olefins oxidation with
 oxygen
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT03198J
_journal_year                    2017
_chemical_formula_sum            'C12 H24 Cu6 Mo24 N24 O80 P2'
_chemical_formula_weight         4530.30
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-11-05 deposited with the CCDC.
2017-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   17.6135(3)
_cell_length_b                   17.6135(3)
_cell_length_c                   23.0663(7)
_cell_measurement_reflns_used    8969
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.2864
_cell_measurement_theta_min      2.2138
_cell_volume                     6197.3(2)
_computing_cell_refinement       'Bruker SMAR'
_computing_data_collection       'Bruker SMAR'
_computing_data_reduction        'Bruker SMAR'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            15253
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.286
_diffrn_reflns_theta_min         1.600
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.186
_exptl_absorpt_correction_T_max  0.595
_exptl_absorpt_correction_T_min  0.515
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6348
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.629
_refine_diff_density_min         -2.315
_refine_diff_density_rms         0.259
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         3410
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+30.9039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0714
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3193
_reflns_number_total             3410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03198j2.cif
_cod_data_source_block           2-1
_cod_depositor_comments
;

2018-06-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C6 H12 Cu3 Mo12 N12 O40 P'
_cod_original_formula_weight         2265.15
_cod_original_formula_units_Z            6
_cod_original_cell_volume        6197.3(3)
_cod_database_code               7044700
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              51969