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

data_7709580
_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_formula_moiety
'Na3, 4(H2 O), 4(C3 H7 N O), 2(C H3 C N), Mn Mo6 O24 (C22 H21 N2 O2)2'
_chemical_formula_sum            'C60 H84 Mn Mo6 N10 Na3 O36'
_chemical_formula_weight         2220.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_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                90.088(4)
_cell_angle_beta                 95.059(4)
_cell_angle_gamma                99.731(4)
_cell_formula_units_Z            1
_cell_length_a                   9.3899(9)
_cell_length_b                   13.0933(13)
_cell_length_c                   16.5155(16)
_cell_measurement_reflns_used    9864
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      27.477
_cell_measurement_theta_min      2.628
_cell_volume                     1993.2(3)
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker D8 Venture'
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0764
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47040
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.551
_diffrn_reflns_theta_min         2.628
_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
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.178
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6222
_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    1.850
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.023
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         8969
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0236P)^2^+5.2567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6794
_reflns_number_total             8969
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00093h2.cif
_cod_data_source_block           aa
_cod_database_code               7709580
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.757
_shelx_estimated_absorpt_t_min   0.538
_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, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
O15 \\sim N4 \\sim C25 \\sim C26 \\sim C27: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002 within 2A
O16 \\sim N5 \\sim C28 \\sim C29 \\sim C30: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004 within 2A
O16A \\sim N5A \\sim C28A \\sim C29A \\sim C30A: within 2A with sigma of 0.002
and sigma for terminal atoms of 0.004 within 2A
3. Others
 Sof(O16A)=Sof(N5A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29D)=Sof(H29E)=
 Sof(H29F)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(O16)=Sof(N5)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
 Fixed Sof: Na2(0.5)
4.a Free rotating group:
 O18(H18A,H18B)
4.b Rotating group:
 O17(H17A,H17B)
4.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B)
4.d Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C18(H18),
 C19(H19), C20(H20), C21(H21), C25(H25), C28(H28), C28A(H28A)
4.e Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C29A(H29D,H29E,H29F), C30A(H30D,H30E,H30F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              60265
_olex2_submission_special_instructions 'No special instructions were received'