Polyoxometalate-based hydrogen-bonded organic frameworks as a new class of proton conducting materials
Ji, Ning-Ning; Shi, Zhi-Qiang; Xie, Xiao-Xin; Li, Gang; CrystEngComm  (2020) –; doi:10.1039/D0CE01578D

data_7241585
_publ_section_title
;
 Polyoxometalate-based hydrogen-bonded organic frameworks as a new class
 of proton conducting materials
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01578D
_journal_year                    2020
_chemical_formula_moiety         'Mo12 O40 P, 4(H2 O), C9 H8 N2, 3(C9 H9 N2)'
_chemical_formula_sum            'C36 H43 Mo12 N8 O44 P'
_chemical_formula_weight         2474.03
_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
_audit_creation_date             2020-03-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-07 deposited with the CCDC.	2020-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.537(3)
_cell_angle_beta                 104.715(3)
_cell_angle_gamma                109.659(3)
_cell_formula_units_Z            2
_cell_length_a                   13.1882(4)
_cell_length_b                   14.8316(7)
_cell_length_c                   17.8325(7)
_cell_measurement_reflns_used    8003
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.8910
_cell_measurement_theta_min      3.6900
_cell_volume                     3159.8(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   41.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000  -30.0000 29

  2 omega  -68.00  -41.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000  -30.0000 27

  3 omega  -15.00   11.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000  -30.0000 26

  4 omega  -55.00   -5.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -77.0000  -30.0000 50

  5 omega  -89.00  -61.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -77.0000  -30.0000 28

  6 omega   22.00   54.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -57.0000    0.0000 32

  7 omega   -1.00   24.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000   60.0000 25

  8 omega    1.00   50.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -37.0000   30.0000 49

  9 omega   75.00  101.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734    0.0000   30.0000 26

 10 omega    1.00   28.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000    0.0000 27

 11 omega   33.00   69.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000 -180.0000 36

 12 omega   69.00  110.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000    0.0000 41

 13 omega   64.00   90.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000   90.0000 26

 14 omega   14.00  100.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   37.0000  -90.0000 86

 15 omega    1.00   33.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734    0.0000   30.0000 32

 16 omega   41.00   77.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000   60.0000 36

 17 omega  -32.00   11.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -57.0000    0.0000 43

 18 omega   19.00   75.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   37.0000    0.0000 56

 19 omega  -18.00   57.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -37.0000   90.0000 75

 20 omega   57.00   82.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000  -90.0000 25

 21 omega  -32.00   -7.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -37.0000   30.0000 25

 22 omega   42.00   77.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000    0.0000 35

 23 omega   64.00   98.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000  -30.0000 34

 24 omega   46.00   72.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734    0.0000   30.0000 26

 25 omega   40.00  115.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   60.0000 75

 26 omega  101.00  173.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000 -150.0000 72

 27 omega   43.00   87.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 44

 28 omega   38.00   86.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 48

 29 omega   40.00   86.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  120.0000 46

 30 omega   82.00  108.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -60.0000 26

 31 omega   56.00   86.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -180.0000 30

 32 omega  128.00  155.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -180.0000 27

 33 omega  145.00  171.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -30.0000 26

 34 omega  152.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -120.0000 26

 35 omega   94.00  126.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -30.0000 32

 36 omega   46.00   89.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 43

 37 omega   56.00  106.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -120.0000 50

 38 omega   57.00  103.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -180.0000 46

 39 omega   82.00  107.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   90.0000 25

 40 omega   39.00   78.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   90.0000 39

 41 omega   41.00   99.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   60.0000 58

 42 omega   41.00   67.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -180.0000 26

 43 omega   55.00   89.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -150.0000 34

 44 omega   44.00  126.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000 -120.0000 82

 45 omega   63.00  176.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  150.0000 113
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0201159000
_diffrn_orient_matrix_UB_12      -0.1032217000
_diffrn_orient_matrix_UB_13      0.0228366000
_diffrn_orient_matrix_UB_21      0.0599610000
_diffrn_orient_matrix_UB_22      0.0402898000
_diffrn_orient_matrix_UB_23      0.0857935000
_diffrn_orient_matrix_UB_31      -0.1123698000
_diffrn_orient_matrix_UB_32      -0.0046028000
_diffrn_orient_matrix_UB_33      0.0135469000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24001
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.076
_diffrn_reflns_theta_max         67.076
_diffrn_reflns_theta_min         3.700
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.071
_exptl_absorpt_correction_T_max  0.300
_exptl_absorpt_correction_T_min  0.131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.600
_exptl_crystal_description       block
_exptl_crystal_F_000             2372
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.367
_refine_diff_density_min         -1.696
_refine_diff_density_rms         0.267
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         11286
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0621P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1296
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8987
_reflns_number_total             11286
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01578d2.cif
_cod_data_source_block           1
_cod_database_code               7241585
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C36H41O44N8Mo12P1
_shelx_estimated_absorpt_t_max   0.141
_shelx_estimated_absorpt_t_min   0.082
_exptl_absorpt_special_details   block
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O1W) \\sim Ueq, Uanis(O3W) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
3.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB)
3.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), N4(H4), N5(H5), N6(H6), N7(H7), N8(H8), C1(H1), C2(H2A),
 C3(H3A), C4(H4A), C5(H5A), C8(H8A), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
  C23(H23), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C35(H35), C36(H36)
;
_shelx_res_checksum              82206
_olex2_submission_special_instructions 'No special instructions were received'