The assembly of [Mo2O2S2]2+ based on polydentate phosphonate templates and their proton conductivity
Li, Bo; Meng, Yuxi; Liu, Qianqian; Chen, Xinyu; Liu, Xin; Zang, Hong-Ying; Chemical Communications  (2023) –; doi:10.1039/D3CC04114J

data_7132233
_publ_section_title
;
 The assembly of [Mo2O2S2]2+ based on polydentate phosphonate templates
 and their proton conductivity
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC04114J
_journal_year                    2023
_chemical_formula_moiety         'C12 H48 K12 Mo16 N4 O90 P8 S16, 2(H2 O)'
_chemical_formula_sum            'C12 H52 K12 Mo16 N4 O92 P8 S16'
_chemical_formula_weight         4489.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-10-16
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-10-16 deposited with the CCDC.	2023-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.514(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.5373(16)
_cell_length_b                   17.6293(10)
_cell_length_c                   25.0402(13)
_cell_measurement_reflns_used    9758
_cell_measurement_temperature    173.01
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     12954.8(12)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.01
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            76815
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.110
_diffrn_reflns_theta_max         25.110
_diffrn_reflns_theta_min         2.451
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.9
_diffrn_source_power             0.0405
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    2.335
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8656
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.806
_refine_diff_density_min         -1.398
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         11505
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0495P)^2^+478.1135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1317
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9496
_reflns_number_total             11505
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04114j2.cif
_cod_data_source_block           2
_cod_database_code               7132233
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.652
_shelx_estimated_absorpt_t_min   0.604
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H29-O29 = O44-H44
 0.85 with sigma of 0.02
 H44-O44
 0.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
K7 \\sim K12 \\sim O17 \\sim O18: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
K3 \\sim K12 \\sim K14 \\sim K15 \\sim O23 \\sim O36: within 4A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 4A
Uanis(O18) \\sim Ueq, Uanis(K7) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(K14) \\sim Ueq, Uanis(K15) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O40) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(K7) \\sim Ueq, Uanis(O17) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O5) = Uanis(O3)
4. Others
 Sof(O3)=1-FVAR(1)
 Sof(O5)=FVAR(1)
 Fixed Sof: K2(0.4) K3(0.15) K5(0.5) K11(0.7) K12(0.15) K13(0.35) K14(0.5)
 K15(0.25) O2(0.5) O10(0.5)
5.a Riding coordinates:
 O4(H4), O21(H21A,H21B), O24(H24A,H24B), O25(H25A,H25B), O30(H30A,H30B),
 O45(H45), O1(H1C,H1D)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1B,H1A), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5B,H5A), C6(H6B,H6A)
;
_shelx_res_checksum              45014
_shelx_hkl_checksum              32777
_olex2_submission_special_instructions 'No special instructions were received'