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_1508162
_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            'C72 H155 N29 O90 W8'
_chemical_formula_weight         4338.05
_chemical_name_common            'citrate tungsten complex'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                106.524(2)
_cell_angle_beta                 97.523(2)
_cell_angle_gamma                110.994(2)
_cell_formula_units_Z            1
_cell_length_a                   13.6607(3)
_cell_length_b                   13.8904(4)
_cell_length_c                   20.0333(6)
_cell_measurement_temperature    296(2)
_cell_volume                     3285.33(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32101
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    7.099
_exptl_absorpt_correction_T_max  0.3310
_exptl_absorpt_correction_T_min  0.1734
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    2.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2102
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.814
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1030
_refine_ls_number_reflns         12678
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+5.1459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0709
_reflns_number_gt                9378
_reflns_number_total             12678
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            Wcitb.cif
_cod_data_source_block           sad
_cod_original_cell_volume        3285.33(15)
_cod_database_code               1508162