An unprecedented [{Fe5O5(OH)2(OAc)2}2{W2O2(OH)}] cluster sandwiched in the tetravacant tungstophosphate
Niu, Jingyang; Yang, Zongfei; Wang, Yaping; Liang, Zhijie; Lu, Jingkun; Ma, Pengtao; Wang, Jingping; Dalton Transactions  (2019) –; doi:10.1039/C9DT03524A

data_7701451
_publ_section_title
;
 An unprecedented [{Fe5O5(OH)2(OAc)2}2{W2O2(OH)}] cluster sandwiched in
 the tetravacant tungstophosphate
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03524A
_journal_year                    2019
_chemical_formula_moiety         'C8 H12 Fe10 K3 Na4 O149 P4 W30, 13(O)'
_chemical_formula_sum            'C8 H12 Fe10 K3 Na4 O162 P4 W30'
_chemical_formula_weight         9107.32
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_block_doi                 10.5517/ccdc.csd.cc20wgn1
_audit_creation_date             2017-08-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2018-10-16 deposited with the CCDC.    2019-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                114.9234(6)
_cell_angle_beta                 95.2570(7)
_cell_angle_gamma                96.9183(7)
_cell_formula_units_Z            2
_cell_length_a                   13.4742(6)
_cell_length_b                   26.3391(11)
_cell_length_c                   31.1489(13)
_cell_measurement_reflns_used    8740
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.924
_cell_measurement_theta_min      2.285
_cell_volume                     9826.9(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0974
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            51307
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         1.558
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.389
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1352 before and 0.0452 after correction.
The Ratio of minimum to maximum transmission is 0.4082.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.078
_exptl_crystal_description       block
_exptl_crystal_F_000             7994
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.554
_refine_diff_density_min         -2.370
_refine_diff_density_rms         0.410
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1140
_refine_ls_number_reflns         34716
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0787P)^2^+21.7659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1711
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22407
_reflns_number_total             34716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03524a2.cif
_cod_data_source_block           1
_cod_database_code               7701451
_shelx_estimated_absorpt_t_max   0.183
_shelx_estimated_absorpt_t_min   0.064
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O3W-O17W = O14W-O19W
 2.65 with sigma of 0.04
3. Others
 Fixed Sof: Na4(0.5) Na5(0.5) Na6(0.5)
4.a Me refined with riding coordinates:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'