A polyoxometalate supported copper dimeric complex: Synthesis, structure and electrocatalysis
Kumar, N. Tanmaya; Bhoi, Umashis; Naulakha, Pragya; Das, Samar K.; Inorganica Chimica Acta 506 (2020) 119554–; doi:10.1016/j.ica.2020.119554

data_1565198
_publ_section_title
;
 A polyoxometalate supported copper dimeric complex: Synthesis, structure
 and electrocatalysis
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119554
_journal_paper_doi               10.1016/j.ica.2020.119554
_journal_volume                  506
_journal_year                    2020
_chemical_formula_sum            'C48 H76 Cu4 Mo16 N8 O78'
_chemical_formula_weight         3802.16
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.490(8)
_cell_angle_beta                 98.770(9)
_cell_angle_gamma                111.063(8)
_cell_formula_units_Z            1
_cell_length_a                   12.135(3)
_cell_length_b                   12.766(3)
_cell_length_c                   19.016(5)
_cell_measurement_reflns_used    8542
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      26.92
_cell_measurement_theta_min      2.96
_cell_volume                     2564.0(11)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 0.709
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            53273
_diffrn_reflns_theta_full        29.49
_diffrn_reflns_theta_max         29.49
_diffrn_reflns_theta_min         2.30
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.809
_exptl_absorpt_correction_T_max  0.1625
_exptl_absorpt_correction_T_min  0.0658
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    2.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Grain
_exptl_crystal_F_000             2139
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         3.377
_refine_diff_density_min         -5.443
_refine_diff_density_rms         0.887
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.426
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         10129
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.426
_refine_ls_R_factor_all          0.1110
_refine_ls_R_factor_gt           0.0748
_refine_ls_shift/su_max          0.182
_refine_ls_shift/su_mean         0.042
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2394
_refine_ls_wR_factor_ref         0.3043
_reflns_number_gt                8559
_reflns_number_total             10129
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ICA-2020-506-119554.cif
_cod_data_source_block           skd343_0m_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

data item '_exptl_crystal_density_meas' value 'none' was changed to
'?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1565198