A Metal-Organic Framework of Organic Vertices and Polyoxometalate Linkers as a Solid-State Electrolyte.
Xu, Wentao; Pei, Xiaokun; Diercks, Christian S.; Lyu, Hao; Ji, Zhe; Yaghi, Omar M.; Journal of the American Chemical Society 141 (2019) 17522–17526; doi:10.1021/jacs.9b10418

data_4133729
_publ_section_title
;
 A Metal-Organic Framework of Organic Vertices and Polyoxometalate Linkers
 as a Solid-State Electrolyte.
;
_journal_issue                   44
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17522
_journal_page_last               17526
_journal_paper_doi               10.1021/jacs.9b10418
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C11.25 H10.5 Mn0.5 Mo3 N O12'
_chemical_formula_sum            'C11.25 H10.66 Mn0.5 Mo3 N O12'
_chemical_formula_weight         667.16
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-10-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   38.1427(19)
_cell_length_b                   38.1427(19)
_cell_length_c                   13.6269(7)
_cell_measurement_reflns_used    9817
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.89
_cell_measurement_theta_min      3.14
_cell_volume                     19825.3(17)
_computing_cell_refinement       'SAINT V8.38A Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.38A Bruker-AXS, Madison WI'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker PHOTON-II detector'
_diffrn_detector_area_resol_mean 7.39
_diffrn_detector_type            'CMOS detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 with PHOTON-II detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            160428
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        22.552
_diffrn_reflns_theta_max         22.552
_diffrn_reflns_theta_min         1.548
_diffrn_source
;
Advanced Light Source, 12.2.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.895
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.6150
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1028 before and 0.0761 after correction. The Ratio of minimum to maximum transmission is 0.8255. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colorless'
_exptl_crystal_density_diffrn    0.894
_exptl_crystal_description       needle
_exptl_crystal_F_000             5115
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         6041
_refine_ls_number_restraints     200
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0737
_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^)+(0.1482P)^2^+85.9542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2282
_refine_ls_wR_factor_ref         0.2369
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5213
_reflns_number_total             6041
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10418_si_002.cif
_cod_data_source_block           MOF-688
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        19825(2)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'C11.25 H10.66 Mn0.50 Mo3 N O12'
_cod_database_code               4133729
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.841
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N1B-C1 = N1A-C1
 1.46 with sigma of 0.02
 C5B-C6B = C5A-C6A
 1.54 with sigma of 0.02
 N1B-C5B = N1A-C5A
 1.28 with sigma of 0.02
 C9A-C6A \\sim C6B-C9B \\sim C10A-C9A \\sim C9B-C10B \\sim C10B-C11 \\sim
C10A-C11 \\sim C6B-C7B \\sim C7A-
 C6A \\sim C7B-C8B \\sim C8A-C7A \\sim C8A-C11 \\sim C8B-C11
 with sigma of 0.02
 C11-C9B \\sim C10B-C6B \\sim C10A-C6A \\sim C9A-C7A \\sim C10B-C8B \\sim
C8A-C10A
 with sigma of 0.02
 C9B-C5B \\sim C5B-C7B
 with sigma of 0.02
 C10B-C12 \\sim C12-C8B
 with sigma of 0.02
3. Restrained planarity
 C5A, C6A, C9A, C10A, C11, C8A, C7A
 with sigma of 0.1
 C5B, C6B, C9B, C7B, C8B, C10B, C11, C12
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N1A \\sim N1B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C5B \\sim C5A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
Uanis(C9A) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10B) \\sim Ueq, Uanis(C9B)
\\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C6A) \\sim Ueq,
Uanis(C10A) \\sim Ueq, Uanis(C8B) \\sim Ueq, Uanis(C7B) \\sim Ueq, Uanis(C6B)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C5B) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(N1A) \\sim Ueq, Uanis(N1B)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C9A) = Uanis(C11) = Uanis(C10B) = Uanis(C9B) = Uanis(C8A) = Uanis(C7A) =
Uanis(C6A) = Uanis(C10A) = Uanis(C8B) = Uanis(C7B) = Uanis(C6B)
5. Others
 Fixed Sof: C9A(0.5) H9A(0.5) C10B(0.5) H10B(0.5) C9B(0.5) H9B(0.5) C8A(0.5)
 H8A(0.5) C7A(0.5) H7A(0.5) C6A(0.5) C5A(0.5) H5A(0.5) N1A(0.5) C10A(0.5)
 H10A(0.5) C8B(0.5) H8B(0.5) C7B(0.5) H7B(0.5) C6B(0.5) C5B(0.5) N1B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C3(H3A,H3B)
6.b Aromatic/amide H refined with riding coordinates:
 C9A(H9A), C10B(H10B), C9B(H9B), C8A(H8A), C7A(H7A), C5A(H5A), C10A(H10A),
 C8B(H8B), C7B(H7B)
;
_shelx_res_checksum              65058
_shelx_hkl_checksum              52755
_shelx_fab_checksum              59918
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'