Cluster-oxalate frameworks with extra-large channels: solvent-free synthesis, chemical stability, and proton conduction.
Luan, Lindong; Zhang, Ying; Zeng, Hongmei; Zou, Guohong; Dai, Yong; Zhou, Xiaoying; Lin, Zhien; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13130–13134; doi:10.1039/c9dt02703c

data_7700675
_publ_section_title
;
 Cluster-oxalate frameworks with extra-large channels: solvent-free
 synthesis, chemical stability, and proton conduction.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13130
_journal_page_last               13134
_journal_paper_doi               10.1039/c9dt02703c
_journal_volume                  48
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C2 H2 Mn2 O13 S2, C10 H10 N2'
_chemical_formula_sum            'C12 H12 Mn2 N2 O13 S2'
_chemical_formula_weight         566.24
_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_Hall           'I 4bw -2c'
_space_group_name_H-M_alt        'I 41 c d'
_symmetry_space_group_name_Hall  'I 4bw -2c'
_symmetry_space_group_name_H-M   'I 41 c d'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-06-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-27 deposited with the CCDC.    2019-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   23.10844(15)
_cell_length_b                   23.10844(15)
_cell_length_c                   13.18166(15)
_cell_measurement_reflns_used    4984
_cell_measurement_temperature    292.06(10)
_cell_measurement_theta_max      72.3160
_cell_measurement_theta_min      4.2850
_cell_volume                     7039.01(10)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.06(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -31.00   63.00   1.0000    5.5100
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -77.0000  -90.0000 94

  2 omega    1.00   75.00   1.0000    5.5100
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000   60.0000 74

  3 omega  -31.00   53.00   1.0000    5.5100
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -57.0000  150.0000 84

  4 omega    1.00   75.00   1.0000    5.5100
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000  120.0000 74

  5 omega   38.00   91.00   1.0000   22.0300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -180.0000 53

  6 omega   39.00  109.00   1.0000   22.0300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -150.0000 70

  7 omega   40.00   98.00   1.0000   22.0300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -120.0000 58

  8 omega   39.00  163.00   1.0000   22.0300
omega____ theta____ kappa____ phi______ frames
    -      108.0000    0.0000    0.0000 124
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0399153000
_diffrn_orient_matrix_UB_12      -0.0517241000
_diffrn_orient_matrix_UB_13      0.0232008000
_diffrn_orient_matrix_UB_21      0.0500200000
_diffrn_orient_matrix_UB_22      -0.0419990000
_diffrn_orient_matrix_UB_23      -0.0235196000
_diffrn_orient_matrix_UB_31      0.0187203000
_diffrn_orient_matrix_UB_32      0.0018729000
_diffrn_orient_matrix_UB_33      0.1121101000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            9332
_diffrn_reflns_point_group_measured_fraction_full 0.755
_diffrn_reflns_point_group_measured_fraction_max 0.755
_diffrn_reflns_theta_full        67.044
_diffrn_reflns_theta_max         67.044
_diffrn_reflns_theta_min         5.414
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.667
_exptl_absorpt_correction_T_max  0.227
_exptl_absorpt_correction_T_min  0.081
_exptl_absorpt_correction_type   gaussian
_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            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.137
_exptl_crystal_description       block
_exptl_crystal_F_000             4544
_exptl_crystal_size_max          0.3449
_exptl_crystal_size_mid          0.2513
_exptl_crystal_size_min          0.1903
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.005(6)
_refine_ls_extinction_coef       0.00012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         2371
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0835P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1012
_reflns_Friedel_coverage         0.439
_reflns_Friedel_fraction_full    0.484
_reflns_Friedel_fraction_max     0.484
_reflns_number_gt                2293
_reflns_number_total             2371
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02703c2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7700675--7700676.cif.'
_cod_original_cell_volume        7039.01(12)
_cod_database_code               7700675
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C192  H192  Mn32  N32  O208  S32  '
_reflns_odcompleteness_completeness 99.83
_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
 At 1.5 times of:
  All O(H,H) groups
2.a Riding coordinates:
 OW1(HW1A,HW1B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), N1(H1),
 N2(H2)
;
_olex2_submission_special_instructions 'No special instructions were received'