A "directed precursor self-assembly" strategy for the facile synthesis of heteropoly blues: crystal structures, formation mechanism and electron distribution.
Wang, Yuchao; Li, Fengyan; Jiang, Ning; Liu, Xizheng; Xu, Lin; Dalton transactions (Cambridge, England : 2003) 48 (2019) 14347–14353; doi:10.1039/c9dt02789k

data_7701000
_publ_section_title
;
 A &quot;directed precursor self-assembly&quot; strategy for the facile
 synthesis of heteropoly blues: crystal structures, formation mechanism
 and electron distribution.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14347
_journal_page_last               14353
_journal_paper_doi               10.1039/c9dt02789k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C56 H254 Mo18 N14 Na2 O222 P6 W36'
_chemical_formula_weight         13254.05
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-05-16 deposited with the CCDC.    2019-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 110.62
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   66.961
_cell_length_b                   18.432
_cell_length_c                   23.971
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.030
_cell_measurement_theta_min      0.013
_cell_volume                     27690.258
_computing_cell_refinement       'SMART (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0818
_diffrn_reflns_limit_h_max       79
_diffrn_reflns_limit_h_min       -74
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            51096
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    15.812
_exptl_absorpt_correction_T_max  0.206
_exptl_absorpt_correction_T_min  0.050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Sheldrick, 1996)'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    3.179
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             23984
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.047
_refine_diff_density_min         -3.804
_refine_diff_density_rms         0.373
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1550
_refine_ls_number_reflns         24197
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0599P)^2^+2517.7314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1570
_refine_ls_wR_factor_ref         0.1727
_reflns_number_gt                17902
_reflns_number_total             24197
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9dt02789k2.cif
_cod_data_source_block           4#
_cod_depositor_comments
'Adding full bibliography for 7700997--7701000.cif.'
_cod_original_cell_volume        27689.7
_cod_original_sg_symbol_Hall     'c 2yc'
_cod_original_sg_symbol_H-M      'c 2/c'
_cod_database_code               7701000