Tris-decorated multi-iron polyoxotungstates.
Izarova, Natalya V.; Faassen, Fabian; Kögerler, Paul; Dalton transactions (Cambridge, England : 2003) 52 (2023) 546–550; doi:10.1039/d2dt02922g

data_7711914
_publ_section_title
;
 Tris-decorated multi-iron polyoxotungstates.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              546
_journal_page_last               550
_journal_paper_doi               10.1039/d2dt02922g
_journal_volume                  52
_journal_year                    2023
_chemical_formula_sum            'C36 H130 Cl0.5 Fe3 N9 Na0.5 O88 P2 W15'
_chemical_formula_weight         5113.94
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-09-06 deposited with the CCDC.	2022-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.376(2)
_cell_length_b                   16.376(2)
_cell_length_c                   25.646(5)
_cell_measurement_reflns_used    6917
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.89
_cell_measurement_theta_min      1.45
_cell_volume                     5956.2(16)
_computing_cell_refinement
;
X-Area Recipe 1.36.0.0 (STOE, 2020)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.170.0 (STOE, 2020)
;
_computing_data_reduction
;
X-Area Integrate 1.78.3.0 (STOE, 2020)
X-Area LANA 1.83.8.0 (STOE, 2020)
;
_computing_molecular_graphics    'Diamond 4'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.90, Darmstadt 2020
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1158
_diffrn_reflns_av_unetI/netI     0.0769
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            33235
_diffrn_reflns_point_group_measured_fraction_full 0.846
_diffrn_reflns_point_group_measured_fraction_max 0.846
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.141
_diffrn_source                   'Genix Mo'
_exptl_absorpt_coefficient_mu    14.916
_exptl_absorpt_correction_T_max  0.1126
_exptl_absorpt_correction_T_min  0.0414
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration. 
Afterwards scaling of reflection intensities was performed 
within STOE LANA. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.851
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             4690
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.230
_refine_diff_density_max         2.540
_refine_diff_density_min         -3.109
_refine_diff_density_rms         0.340
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
 
;
_refine_ls_abs_structure_Flack   0.33(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         5959
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1213
_refine_ls_R_factor_gt           0.0835
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1811P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2255
_refine_ls_wR_factor_ref         0.2641
_reflns_Friedel_coverage         0.653
_reflns_Friedel_fraction_full    0.685
_reflns_Friedel_fraction_max     0.685
_reflns_number_gt                3856
_reflns_number_total             5959
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02922g2.cif
_cod_data_source_block           fe3_a_sq
_cod_depositor_comments
'Adding full bibliography for 7711914--7711915.cif.'
_cod_original_cell_volume        5956(2)
_cod_original_formula_sum        'C36 H130 Cl0.50 Fe3 N9 Na0.50 O88 P2 W15'
_cod_database_code               7711914
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.091
_shelx_estimated_absorpt_t_max   0.131
_shelx_res_checksum              42378
_shelx_hkl_checksum              41539
_shelx_fab_checksum              24615