Heteroanionic Materials Based on Copper Clusters, Bisphosphonates, and Polyoxometalates: Magnetic Properties and Comparative Electrocatalytic NO(x) Reduction Studies.
Oms, Olivier; Yang, Shu; Salomon, William; Marrot, Jérôme; Dolbecq, Anne; Rivière, Eric; Bonnefont, Antoine; Ruhlmann, Laurent; Mialane, Pierre; Inorganic chemistry 55 (2016) 1551–1561; doi:10.1021/acs.inorgchem.5b02456

data_4346962
_publ_section_title
;
 Heteroanionic Materials Based on Copper Clusters, Bisphosphonates, and
 Polyoxometalates: Magnetic Properties and Comparative Electrocatalytic
 NO(x) Reduction Studies.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1551
_journal_page_last               1561
_journal_paper_doi               10.1021/acs.inorgchem.5b02456
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C20 H210 Cu9 N5 Na12 O116.5 P10 Si W9'
_chemical_formula_weight         5226.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 99.6330(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.3560(8)
_cell_length_b                   22.4995(8)
_cell_length_c                   28.2725(9)
_cell_measurement_reflns_used    9053
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.45
_cell_measurement_theta_min      2.28
_cell_volume                     14647.7(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0984
_diffrn_reflns_av_unetI/netI     0.1051
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            235727
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.109
_diffrn_reflns_theta_min         0.884
_exptl_absorpt_coefficient_mu    8.577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, V2.10)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.370
_exptl_crystal_description       needle
_exptl_crystal_F_000             10080
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_exptl_transmission_factor_max   0.7460
_exptl_transmission_factor_min   0.4266
_refine_diff_density_max         6.586
_refine_diff_density_min         -3.196
_refine_diff_density_rms         0.526
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1636
_refine_ls_number_reflns         42833
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1398
_refine_ls_R_factor_gt           0.0827
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0811P)^2^+650.8566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1890
_refine_ls_wR_factor_ref         0.2191
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27519
_reflns_number_total             42833
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02456_si_002.cif
_cod_data_source_block           siw9cuale_
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C20 H210 Cu9 N5 Na12 O116.50 P10 Si W9'
_cod_database_code               4346962
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.153
_shelx_estimated_absorpt_t_max   0.847
_exptl_absorpt_special_details   'Blessing, Acta Cryst. (1995) A51, 33-38'