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_7700998
_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            'C21 H76 Mo2 N14 O82 P2 W16'
_chemical_formula_weight         5032.38
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_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                 92.02
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
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_cell_length_b                   13.887
_cell_length_c                   21.170
_cell_measurement_temperature    293(2)
_cell_volume                     4391.211
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0674
_diffrn_reflns_av_sigmaI/netI    0.0802
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21565
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    21.299
_exptl_absorpt_correction_T_max  0.051
_exptl_absorpt_correction_T_min  0.023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Sheldrick, 1996)'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    3.806
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4508
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.180
_refine_diff_density_min         -3.847
_refine_diff_density_rms         0.422
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.71(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         11383
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1361
_reflns_number_gt                10226
_reflns_number_total             11383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9dt02789k2.cif
_cod_data_source_block           3#
_cod_depositor_comments
'Adding full bibliography for 7700997--7701000.cif.'
_cod_original_cell_volume        4391.2
_cod_original_sg_symbol_H-M      'p n'
_cod_database_code               7700998