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_7700676
_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_formula_moiety         'C3 H6 In3 O26 P5, C4 H14 N2, 2(H2 O)'
_chemical_formula_sum            'C7 H27 In3 N2 O29 P5'
_chemical_formula_weight         1102.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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                107.688(2)
_cell_angle_beta                 95.217(2)
_cell_angle_gamma                99.513(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7933(3)
_cell_length_b                   11.9038(3)
_cell_length_c                   13.2892(3)
_cell_measurement_reflns_used    9204
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9150
_cell_measurement_theta_min      3.7290
_cell_volume                     1586.12(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   -1.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7256   57.0000  -90.0000 84

  2 omega  -52.00   42.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7256  -77.0000  150.0000 94

  3 omega   -1.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7256   57.0000  -30.0000 84

  4 omega  -56.00   45.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7256  -19.0000 -180.0000 101

  5 omega   -1.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7256   57.0000   30.0000 84

  6 omega  -84.00   10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.6631  -77.0000   30.0000 94

  7 omega  -36.00   28.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.6631   38.0000    0.0000 64
;
_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      -0.0528350000
_diffrn_orient_matrix_UB_12      0.0276018000
_diffrn_orient_matrix_UB_13      -0.0040339000
_diffrn_orient_matrix_UB_21      0.0413933000
_diffrn_orient_matrix_UB_22      0.0530551000
_diffrn_orient_matrix_UB_23      0.0003414000
_diffrn_orient_matrix_UB_31      -0.0061294000
_diffrn_orient_matrix_UB_32      -0.0224401000
_diffrn_orient_matrix_UB_33      -0.0565209000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19292
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.498
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.524
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1074
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         6488
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+0.8181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0565
_refine_ls_wR_factor_ref         0.0585
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5861
_reflns_number_total             6488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02703c2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7700675--7700676.cif.'
_cod_original_cell_volume        1586.11(8)
_cod_database_code               7700676
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.538
_shelx_estimated_absorpt_t_min   0.481
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O27(H27A,H27B), O28(H28A,H28B)
2.b Ternary CH refined with riding coordinates:
 N1(H1)
2.c Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), N2(H2A,H2B,H2C)
2.e Idealised tetrahedral OH refined as rotating group:
 O4(H4), O8(H8), O12(H12), O16(H16), O19(H19), O20(H20)
;
_olex2_submission_special_instructions 'No special instructions were received'