An ionic organic‒inorganic hybrid: tetrakis[bis(1,10-phenanthroline)copper(I)] dodecatungstophosphate(V)
Meng, Fan-Xia; Liu, Hong-Bo; Chen, Ya-Guang; Acta Crystallographica Section E 64 (2008) m106–m106; doi:10.1107/S1600536807062903

data_2217352
_publ_section_title
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 An ionic organic--inorganic hybrid:
 tetrakis[bis(1,10-phenanthroline)copper(I)] dodecatungstophosphate(V)
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_journal_coeditor_code           WM2165
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m106
_journal_page_last               m106
_journal_paper_doi               10.1107/S1600536807062903
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Cu (C12 H8 N2)2]4 [Si W12 O40]'
_chemical_formula_moiety         '4C24 H16 Cu N4 + , O40 Si W12 4-'
_chemical_formula_sum            'C96 H64 Cu4 N16 O40 Si W12'
_chemical_formula_weight         4570.08
_chemical_name_systematic
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tetrakis[bis(1,10-phenanthroline)copper(I)] dodecatungstophosphate(V)
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.332(3)
_cell_length_b                   21.173(3)
_cell_length_c                   27.901(4)
_cell_measurement_reflns_used    5100
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      1.46
_cell_volume                     10830(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics
'Mercury (Version 1.4.2; Macrae <i>et al.</i>,  2006)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0646
_diffrn_reflns_av_sigmaI/netI    0.0825
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            66617
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.46
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.554
_exptl_absorpt_correction_T_max  0.072
_exptl_absorpt_correction_T_min  0.066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.803
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8360
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.290
_refine_diff_density_min         -1.373
_refine_ls_abs_structure_details 'Flack (1983), with 11091 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.006(6)
_refine_ls_extinction_coef       0.000046(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1523
_refine_ls_number_reflns         24930
_refine_ls_number_restraints     2431
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0109P)^2^] where P= (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0719
_reflns_number_gt                20506
_reflns_number_total             24930
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm2165.cif
_cod_data_source_block           I
_cod_depositor_comments
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The following automatic conversions were performed:

'_diffrn_ambient_temperature' value '293(2) K' was changed to
'293(2)' - the value should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_diffrn_ambient_temperature' value '293(2) K' was changed to
'293(2)' - the value should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2217352
_cod_database_fobs_code          2217352