A stable porphyrinic metal‒organic framework pore-functionalized by high-density carboxylic groups for proton conduction
Wu, Hao; Yang, Fan; Lv, Xiu-Liang; Wang, Bin; Zhang, Yong-Zheng; Zhao, Min-Jian; Li, Jian-Rong; Journal of Materials Chemistry A 5 (2017) 14525–; doi:10.1039/C7TA03917D

data_7236594
_publ_section_title
;
 A stable porphyrinic metal--organic framework pore-functionalized by
 high-density carboxylic groups for proton conduction
;
_journal_issue                   28
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              14525
_journal_paper_doi               10.1039/C7TA03917D
_journal_volume                  5
_journal_year                    2017
_chemical_formula_moiety         '0.11(C396 H216 Co9 N54 O36)'
_chemical_formula_sum            'C44 H24 Co N6 O4'
_chemical_formula_weight         759.62
_chemical_name_systematic        BUT-83
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-12-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-12-22 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   33.0267(5)
_cell_length_b                   33.0267(5)
_cell_length_c                   9.1815(3)
_cell_measurement_reflns_used    3429
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.7660
_cell_measurement_theta_min      4.6180
_cell_volume                     8673.1(3)
_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      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
  1 omega  -74.00   35.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5605   77.0000   60.0000 109

  2 omega   30.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  -30.0000  -60.0000 60

  3 omega   94.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  125.0000   60.0000 84

  4 omega   30.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  -30.0000   30.0000 60

  5 omega   99.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  116.0000   35.0000 79

  6 omega   94.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  125.0000 -150.0000 84

  7 omega -114.00  -75.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5605  -57.0000  150.0000 39

  8 omega -116.00  -17.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5605  -37.0000   30.0000 99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0340341000
_diffrn_orient_matrix_UB_12      0.0186665000
_diffrn_orient_matrix_UB_13      0.0211989000
_diffrn_orient_matrix_UB_21      -0.0415994000
_diffrn_orient_matrix_UB_22      -0.0491584000
_diffrn_orient_matrix_UB_23      -0.0307424000
_diffrn_orient_matrix_UB_31      -0.0034218000
_diffrn_orient_matrix_UB_32      -0.0116609000
_diffrn_orient_matrix_UB_33      0.1635757000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0870
_diffrn_reflns_av_unetI/netI     0.0839
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            10519
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.813
_diffrn_reflns_theta_min         4.638
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.904
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23827
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_F_000             3501
_refine_diff_density_max         1.827
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1240
_refine_ls_R_factor_gt           0.0792
_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^)+(0.1428P)^2^+21.4878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2131
_refine_ls_wR_factor_ref         0.2607
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2417
_reflns_number_total             3792
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ta03917d2.cif
_cod_data_source_block           1
_cod_original_cell_volume        8673.1(4)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7236594
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         CHONCo
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C14(H14), C13(H13), C2(H2), C5(H5), C21(H21), C1(H1),
 C18(H18), C4(H4), C17(H17), C20(H20)
;
_shelx_res_checksum              5376
_shelx_fab_checksum              55965
_olex2_submission_special_instructions 'No special instructions were received'