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_4346963
_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
'C48 H443 Cl Cu24 Li32 N12 Na5 O323.5 P24 Sb4 W36'
_chemical_formula_weight         16113.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                75.951(4)
_cell_angle_beta                 78.016(5)
_cell_angle_gamma                78.695(5)
_cell_formula_units_Z            2
_cell_length_a                   22.384(3)
_cell_length_b                   32.340(4)
_cell_length_c                   34.221(4)
_cell_measurement_reflns_used    9772
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      2.50
_cell_volume                     23229(5)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0954
_diffrn_reflns_av_unetI/netI     0.0997
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            333971
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.226
_diffrn_reflns_theta_max         25.226
_diffrn_reflns_theta_min         0.941
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    10.359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, V2.10)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.304
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             14990
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.040
_exptl_transmission_factor_max   0.7452
_exptl_transmission_factor_min   0.3801
_refine_diff_density_max         4.297
_refine_diff_density_min         -6.700
_refine_diff_density_rms         0.528
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     4165
_refine_ls_number_reflns         82318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.0918
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1234P)^2^+1657.1104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2469
_refine_ls_wR_factor_ref         0.2679
_reflns_Friedel_coverage         0.000
_reflns_number_gt                57466
_reflns_number_total             82318
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02456_si_002.cif
_cod_data_source_block           SbW9Cuale_
_cod_original_formula_sum
'C48 H443 Cl Cu24 Li32 N12 Na5 O323.50 P24 Sb4 W36'
_cod_database_code               4346963
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.160
_shelx_estimated_absorpt_t_max   0.682
_exptl_absorpt_special_details   'Blessing, Acta Cryst. (1995) A51, 33-38'