Phosphonium zwitterions for lighter and chemically-robust MOFs: highly reversible H2S capture and solvent-triggered release
Reynolds, Joseph E.; Bohnsack, Alisha M.; Kristek, David J.; Gutiérrez-Alejandre, Aída; Dunning, Samuel G.; Waggoner, Nolan W.; Sikma, R. Eric; Ibarra, Ilich A.; Humphrey, Simon M.; Journal of Materials Chemistry A 7 (2019) 16842–; doi:10.1039/C9TA05444H

data_7237678
_publ_section_title
;
 Phosphonium zwitterions for lighter and chemically-robust MOFs: highly
 reversible H2S capture and solvent-triggered release
;
_journal_issue                   28
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              16842
_journal_paper_doi               10.1039/C9TA05444H
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         'C28 H16 In O8 P'
_chemical_formula_sum            'C28 H16 In O8 P'
_chemical_formula_weight         626.20
_chemical_name_common            PCM-66
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2019-03-21 deposited with the CCDC.	2019-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.2729(4)
_cell_length_b                   17.2729(4)
_cell_length_c                   16.1689(6)
_cell_measurement_reflns_used    6342
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.3190
_cell_measurement_theta_min      3.6000
_cell_volume                     4824.0(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'Shelxl-2016/6, Sheldrick, G. M.'
_computing_structure_refinement  'Shelxl-2016/6, Sheldrick, G. M.'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2940
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -74.00  35.00   1.00   10.00    --  -41.34  77.00  30.00  109
  2  \w      9.00 117.00   1.00   10.00    --   41.34  77.00 120.00  108
  3  \w     78.00 178.00   1.00   35.00    --  110.22  77.00-120.00  100
  4  \w     78.00 178.00   1.00   35.00    --  110.22  77.00 -30.00  100
  5  \w     78.00 178.00   1.00   35.00    --  110.22  77.00-150.00  100
  6  \w   -117.00  -9.00   1.00   10.00    --  -41.34 -77.00 -30.00  108
  7  \w   -113.00 -65.00   1.00   10.00    --  -41.34-137.00 123.00   48
  8  \w     94.00 178.00   1.00   35.00    --  110.22 125.00  60.00   84
  9  \w     82.00 178.00   1.00   35.00    --  110.22  30.00  60.00   96
 10  \w     94.00 174.00   1.00   35.00    --  110.22 125.00 -90.00   80
 11  \w     81.00 178.00   1.00   35.00    --  110.22  61.00 150.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0144521000
_diffrn_orient_matrix_UB_12      0.0342923000
_diffrn_orient_matrix_UB_13      -0.0865255000
_diffrn_orient_matrix_UB_21      0.0289608000
_diffrn_orient_matrix_UB_22      0.0756491000
_diffrn_orient_matrix_UB_23      0.0397340000
_diffrn_orient_matrix_UB_31      0.0831450000
_diffrn_orient_matrix_UB_32      -0.0325603000
_diffrn_orient_matrix_UB_33      0.0011342000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0835
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11973
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.3075
_diffrn_reflns_theta_min         3.6189
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.929
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_description       equant
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.937
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details
;
 Flack x determined using 1593 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.035(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         4677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0865P)^2^+15.5215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1345
_reflns_Friedel_coverage         0.831
_reflns_Friedel_fraction_full    0.937
_reflns_Friedel_fraction_max     0.859
_reflns_number_gt                4036
_reflns_number_total             4677
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ta05444h2.cif
_cod_data_source_block           sh17047
_cod_original_cell_volume        4824.0(3)
_cod_database_code               7237678
_chemical_oxdiff_formula         'H20 C28 O10 P1 In2 '
_oxdiff_exptl_absorpt_empirical_full_min 0.637
_oxdiff_exptl_absorpt_empirical_full_max 2.157
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_shelxl_version_number           2013-4
_shelx_res_checksum              73210