Hydronium μ-chloro-bis[bis(1,10-phenanthroline)copper(I)] hexatungstate monohydrate
Ma, Peng-Tao; Hu, Fu-Xin; Li, Ming-Xue; Wang, Jing-Ping; Acta Crystallographica Section E 62 (2006) m2241–m2243; doi:10.1107/S160053680603220X

data_2210082
_publ_section_title
;
 Hydronium \m-chloro-bis[bis(1,10-phenanthroline)copper(I)]
 hexatungstate monohydrate
;
_journal_coeditor_code           BI2028
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2241
_journal_page_last               m2243
_journal_paper_doi               10.1107/S160053680603220X
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(H3 O) [Cu2 Cl (C12 H8 N2)4] [W6 O19], H2 O'
_chemical_formula_moiety
'H3 O +, C48 H32 Cl Cu2 N8 +, W6 O19 2-, H2 O'
_chemical_formula_sum            'C48 H37 Cl Cu2 N8 O21 W6'
_chemical_formula_weight         2327.48
_chemical_name_systematic
;
hydronium \m-chloro-bis[bis(1,10-phenanthroline)copper(I)] hexatungstate
monohydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 118.1380(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.135(2)
_cell_length_b                   16.2883(14)
_cell_length_c                   14.1273(13)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.5
_cell_volume                     5303.2(8)
_computing_cell_refinement       RAXIS
_computing_data_collection
;
RAXIS (Molecular Structure Corporation, 1992)
;
_computing_data_reduction
;
TEXSAN (Molecular Structure Corporation, 1995)
;
_computing_molecular_graphics    TEXSAN
_computing_publication_material  TEXSAN
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS IV'
_diffrn_measurement_method       \f
_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  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13441
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.882
_exptl_absorpt_correction_T_max  0.287
_exptl_absorpt_correction_T_min  0.242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.914
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4268
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.685
_refine_diff_density_min         -3.804
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         4659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+13.1567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1232
_reflns_number_gt                3729
_reflns_number_total             4659
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bi2028.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2210082
_cod_database_fobs_code          2210082