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_7044861
_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
'C12.8 H14.4 Cu6.4 N19.2 Nb2.4 O41.6 P0.8 W7.2'
_chemical_formula_weight         3080.97
_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            10
_cell_length_a                   17.5009(8)
_cell_length_b                   17.5009(8)
_cell_length_c                   47.384(4)
_cell_measurement_reflns_used    4405
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.29
_cell_measurement_theta_min      2.33
_cell_volume                     14512.8(15)
_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 0.998
_diffrn_measured_fraction_theta_max 0.999
_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  0.0969
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            42896
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.384
_diffrn_reflns_theta_min         1.719
_exptl_absorpt_coefficient_mu    17.077
_exptl_absorpt_correction_T_max  0.711
_exptl_absorpt_correction_T_min  0.443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/1,(Bruker AXS)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.525
_exptl_crystal_density_meas      ?
_exptl_crystal_description       slice
_exptl_crystal_F_000             13872
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.770
_refine_diff_density_min         -4.832
_refine_diff_density_rms         0.427
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3334
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0668
_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^)+(0.0510P)^2^+3596.5210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.1706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2624
_reflns_number_total             3334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03968a2.cif
_cod_data_source_block           142
_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        14513.0(19)
_cod_original_formula_sum
'C12.80 H14.40 Cu6.40 N19.20 Nb2.40 O41.60 P0.80 W7.20'
_cod_database_code               7044861
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.4780
_shelx_estimated_absorpt_t_max   0.7452
_exptl_absorpt_special_details
'wR2(int)=0.1130 before and 0.0607 after the adsorption correction process.'
_shelx_res_checksum              12190