One-step introduction of terminal sulfonic groups into a proton-conducting metal-organic framework by concerted deprotonation-metalation-hydrolysis reaction.
Szufla, Monika; Roztocki, Kornel; Krawczuk, Anna; Matoga, Dariusz; Dalton transactions (Cambridge, England : 2003) 49 (2020) 9953–9956; doi:10.1039/d0dt02017f

data_7704833
_publ_section_title
;
 One-step introduction of terminal sulfonic groups into a
 proton-conducting metal-organic framework by concerted
 deprotonation-metalation-hydrolysis reaction.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9953
_journal_page_last               9956
_journal_paper_doi               10.1039/d0dt02017f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C34 H23.5 Cd N6 O10 S'
_chemical_formula_weight         820.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2020-05-21 deposited with the CCDC.	2020-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.4070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   39.3542(4)
_cell_length_b                   8.97070(10)
_cell_length_c                   30.3706(2)
_cell_measurement_reflns_used    136113
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      32.9910
_cell_measurement_theta_min      2.5070
_cell_volume                     10112.68(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_molecular_graphics
;
  ORTEP-3 for Windows (Farrugia, 2012); MERCURY (Version
  4.0; Macrae et al., 2020)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            293179
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.195
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.519
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_description       prism
_exptl_crystal_F_000             3308
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.180
_refine_diff_density_max         3.515
_refine_diff_density_min         -1.623
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     920
_refine_ls_number_reflns         24379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0882
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1163P)^2^+35.6298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2577
_refine_ls_wR_factor_ref         0.2644
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18901
_reflns_number_total             24379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02017f2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7704833.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C34 H23.50 Cd N6 O10 S'
_cod_database_code               7704833
_shelx_estimated_absorpt_t_min   0.864
_shelx_estimated_absorpt_t_max   0.912
_shelxl_version_number           2013-4
_shelx_res_checksum              10917