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_7132232
_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 H24 K2 Mo20 N4 O70 P12 S20, 60[H2O]'
_chemical_formula_sum            'C12 H144 K2 Mo20 N4 O130 P12 S20'
_chemical_formula_weight         5435.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           71
_space_group_name_Hall           '-I 2 2'
_space_group_name_H-M_alt        'I m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-15
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.155(7)
_cell_length_b                   28.056(19)
_cell_length_c                   28.151(15)
_cell_measurement_reflns_used    6779
_cell_measurement_temperature    280.31
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     8810(9)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      280.31
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.1037
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            25350
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.105
_diffrn_reflns_theta_max         25.105
_diffrn_reflns_theta_min         2.289
_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    1.866
_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            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.049
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5324
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.400
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         4258
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0537P)^2^+49.8415P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1207
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3114
_reflns_number_total             4258
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04114j2.cif
_cod_data_source_block           22
_cod_database_code               7132232
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.707
_shelx_estimated_absorpt_t_min   0.663
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 P1-C3
 1.75 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim O4 \\sim O6 \\sim O8 \\sim O10 \\sim O12 \\sim O14 \\sim O16 \\sim O18
\\sim O20 \\sim O22 \\sim O24 \\sim O26: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.03 within 3.8A
C1 \\sim C2 \\sim C3: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.03 within 3.8A
Uanis(O24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: S2(0.25) S3(0.25) P2(0.5) O22(0.25) O24(0.25) O26(0.5) H1A(0.5)
 H1B(0.5) C2(0.5) H2A(0.5) H2B(0.5) C3(0.5) H3A(0.5) H3B(0.5) O7(0.5) O27(0.5)
 O22A(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              3008
_shelx_hkl_checksum              56962
_shelx_fab_checksum              89719
_olex2_submission_special_instructions 'No special instructions were received'