Chiral hexamers of organically modified polyoxometalates via ionic complexation
Guan, Weiming; Li, Bao; Wu, Lixin; Dalton Transactions  (2022) –; doi:10.1039/D2DT00093H

data_7709579
_publ_section_title
;
 Chiral hexamers of organically modified polyoxometalates via ionic
 complexation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00093H
_journal_year                    2022
_chemical_absolute_configuration rmad
_chemical_formula_moiety
'C276 H316 Mn6 Mo36 N24 Na16 O188, 3(H3O), 1(Cl1), 16(C2 H3 N), 26.35[CH3CN], 15.6[C3H7NO], 30.3[H2O]'
_chemical_formula_sum
'C407.5 H621.85 Cl Mn6 Mo36 N81.95 Na16 O236.9'
_chemical_formula_weight         14646.15
_space_group_crystal_system      cubic
_space_group_IT_number           197
_space_group_name_Hall           'I 2 2 3'
_space_group_name_H-M_alt        'I 2 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-09
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-02-10 deposited with the CCDC.	2022-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   30.8142(9)
_cell_length_b                   30.8142(9)
_cell_length_c                   30.8142(9)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      27.491
_cell_measurement_theta_min      2.644
_cell_volume                     29258.5(15)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker D8 Venture'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Bruker APEX-II CCD'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'equatorial mounted graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            221521
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_min         2.644
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.978
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       cube
_exptl_crystal_F_000             14781
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Flack x determined using 4189 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.028(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         11223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+113.0501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1049
_reflns_Friedel_coverage         0.894
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                9694
_reflns_number_total             11223
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00093h2.cif
_cod_data_source_block           as_sq
_cod_original_cell_volume        29259(3)
_cod_original_formula_sum
'C407.50 H621.85 Cl Mn6 Mo36 N81.95 Na16 O236.90'
_cod_database_code               7709579
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.751
_shelx_estimated_absorpt_t_min   0.635
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: O18(0.25) H25A(0.33333) H25B(0.33333) H25C(0.33333)
3.a Ternary CH refined with riding coordinates:
 C7(H7)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B)
3.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C19(H19),
 C20(H20), C21(H21), C22(H22)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              94175
_shelx_fab_checksum              11752
_platon_squeeze_special_details
;
A solvent mask was calculated and 3013 electrons were 
found in a volume of 10924\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
52.7 [CH3CN], 31.2[C3H7NO], 60.6 [H2O] per Unit Cell 
which account for 3014 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'