Hydrogen bonding-controlled assemblies of polymeric and octanuclear tungsten citrates
Zhanga, Rong-Hua; Zhoua, Xin-Wen; Xiaoa, Shu-Zhang; Zhou, Zhao-Hui; Inorganica Chimica Acta 391 (2012) 224–228; doi:10.1016/j.ica.2012.04.025

data_1508161
_publ_section_title
;
 Hydrogen bonding-controlled assemblies of polymeric and octanuclear
 tungsten citrates
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              224
_journal_page_last               228
_journal_paper_doi               10.1016/j.ica.2012.04.025
_journal_volume                  391
_journal_year                    2012
_chemical_formula_sum            'C66 H108 N22 O67 W6'
_chemical_formula_weight         3384.84
_chemical_name_common            'citrate tungsten complex'
_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                 92.278(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.1474(7)
_cell_length_b                   17.7030(5)
_cell_length_c                   19.9701(3)
_cell_measurement_temperature    296(2)
_cell_volume                     10649.6(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34060
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    6.574
_exptl_absorpt_correction_T_max  0.6213
_exptl_absorpt_correction_T_min  0.2068
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    2.111
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6552
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.962
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         10413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0274P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0638
_reflns_number_gt                7121
_reflns_number_total             10413
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            Wcita.cif
_cod_data_source_block           sad
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1508161