Two mixed-addenda Nb/W polyoxometalates-based hybrid compounds containing multicopper units: synthesis, structures, electrochemical and magnetic properties
Weng, Zhewei; Ren, Yuanhang; Gu, Min; Yue, Bin; He, Heyong; Dalton Transactions  (2017) –; doi:10.1039/C7DT03968A

data_7044860
_publ_section_title
;
 Two mixed-addenda Nb/W polyoxometalates-based hybrid compounds containing
 multicopper units: synthesis, structures, electrochemical and magnetic
 properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT03968A
_journal_year                    2017
_chemical_formula_sum            'C12 H12 Cu8 N18 Nb3 O56.5 P W9'
_chemical_formula_weight         3785.07
_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_Hall           '-I 4bd 2c'
_space_group_name_H-M_alt        'I 41/a c d'
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2017-11-20 deposited with the CCDC.
2017-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.588(2)
_cell_length_b                   17.588(2)
_cell_length_c                   47.567(12)
_cell_measurement_reflns_used    36495
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.999
_cell_measurement_theta_min      1.848
_cell_volume                     14714(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1048
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            36495
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.848
_exptl_absorpt_coefficient_mu    16.843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2012/1 (Bruker AXS)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.417
_exptl_crystal_density_meas      ?
_exptl_crystal_description       slice
_exptl_crystal_F_000             13584
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   0.603
_exptl_transmission_factor_min   0.320
_refine_diff_density_max         3.880
_refine_diff_density_min         -1.829
_refine_diff_density_rms         0.372
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3616
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+1412.7617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1363
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2793
_reflns_number_total             3616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03968a2.cif
_cod_data_source_block           mo_60722b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        14714(5)
_cod_original_formula_sum        'C12 H12 Cu8 N18 Nb3 O56.50 P W9'
_cod_database_code               7044860
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.3962
_shelx_estimated_absorpt_t_max   0.5635
_exptl_absorpt_special_details
'wR2(int)=0.1014 before and 0.0662 after the adsorption correction process.'
_shelx_res_checksum              60713