Hypervalent organoiodine(v) metal-organic frameworks: syntheses, thermal studies and stoichiometric oxidants.
Bryant, Macguire R.; Richardson, Christopher; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5167–5174; doi:10.1039/d0dt00870b

data_7703866
_publ_section_title
;
 Hypervalent organoiodine(v) metal-organic frameworks: syntheses, thermal
 studies and stoichiometric oxidants.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5167
_journal_page_last               5174
_journal_paper_doi               10.1039/d0dt00870b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C14 H9 I O4, C2 H6 O S'
_chemical_formula_sum            'C16 H15 I O5 S'
_chemical_formula_weight         446.24
_chemical_name_systematic
'2-iodo-[1,1'-biphenyl]-4,4'-dicarboxylic acid dimethylsulfoxide solvate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-16 deposited with the CCDC.	2020-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                86.9929(16)
_cell_angle_beta                 74.1903(17)
_cell_angle_gamma                69.153(2)
_cell_formula_units_Z            2
_cell_length_a                   8.19869(18)
_cell_length_b                   8.27594(19)
_cell_length_c                   13.9191(2)
_cell_measurement_reflns_used    9827
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.5960
_cell_measurement_theta_min      2.6220
_cell_volume                     848.18(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      150.00(10)
_diffrn_detector                 'HyPix Bantam HPC-3000'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.947
_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     45.00  71.00   0.50    7.00    --   20.00  54.00  30.00   52
  2  \w    -73.00  -7.00   0.50    7.00    --   20.00  54.00 -90.00  132
  3  \w     40.00  97.00   0.50    7.00    --   20.00  54.00 -90.00  114
  4  \w    -74.00  87.00   0.50    7.00    --   20.00  54.00 150.00  322
  5  \w    -69.00  42.00   0.50    7.00    --   20.00  54.00-150.00  222
  6  \w    -71.00 109.00   0.50    7.00    --   20.00  54.00  60.00  360
  7  \w    -68.00  68.00   0.50    7.00    --   20.00  54.00 120.00  272
  8  \w    -73.00 -26.00   0.50    7.00    --   20.00  54.00   0.00   94
  9  \w     75.00 100.00   0.50    7.00    --   20.00  54.00   0.00   50
 10  \w    -62.00 -36.00   0.50    7.00    --   20.00  54.00  90.00   52
 11  \w    -21.00  64.00   0.50    7.00    --   20.00  54.00  90.00  170
 12  \w    -66.00   3.00   0.50    7.00    --   20.00  54.00-120.00  138
 13  \w    -26.00  -1.00   0.50    7.00    --   20.00  54.00-180.00   50
 14  \w      6.00  56.00   0.50    7.00    --   20.00  54.00-180.00  100
 15  \w    -66.00 -15.00   0.50    7.00    --   20.00  54.00  30.00  102
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0252457000
_diffrn_orient_matrix_UB_12      -0.0101664000
_diffrn_orient_matrix_UB_13      -0.0528977000
_diffrn_orient_matrix_UB_21      -0.0633443000
_diffrn_orient_matrix_UB_22      0.0839234000
_diffrn_orient_matrix_UB_23      -0.0022959000
_diffrn_orient_matrix_UB_31      0.0678566000
_diffrn_orient_matrix_UB_32      0.0358463000
_diffrn_orient_matrix_UB_33      -0.0029052000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16754
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.703
_diffrn_reflns_theta_min         2.637
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.032
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_description       wedge
_exptl_crystal_F_000             440
_exptl_crystal_recrystallization_method 'slow evaporation from DMSO'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.593
_refine_diff_density_min         -1.393
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4989
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0262
_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^)+(0.0317P)^2^+0.5050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0676
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4151
_reflns_number_total             4989
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00870b2.cif
_cod_data_source_block           exp_81mrb3
_cod_depositor_comments
'Adding full bibliography for 7703865--7703866.cif.'
_cod_database_code               7703866
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C16H15IO5S
_chemical_oxdiff_usercomment     'crystallised from DMSO solution'
_shelx_estimated_absorpt_t_max   0.838
_shelx_estimated_absorpt_t_min   0.512
_reflns_odcompleteness_completeness 95.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Rigid body (RIGU) restrains
 S2, O5, C8, H8A, H8B, H8C, C9, H9A, H9B, H9C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S1, O6, C10, H10A, H10B, H10C, C11, H11A, H11B, H11C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(S1)=Sof(O6)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11)=Sof(H11A)=
 Sof(H11B)=Sof(H11C)=Sof(H2)=1-FVAR(1)
 Sof(S2)=Sof(O5)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=
 Sof(H9C)=Sof(H1)=FVAR(1)
4.a Free rotating group:
 S1(O6,C10,H10A,H10B,H10C,C11,H11A,H11B,H11C), S2(O5,C8,H8A,H8B,H8C,C9,H9A,H9B,
 H9C)
4.b Aromatic/amide H refined with riding coordinates:
 C2'(H2'), C3(H3), C3'(H3'), C5(H5), C5'(H5'), C6(H6), C6'(H6')
4.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O4(H4)
;
_shelx_res_checksum              24335
_olex2_exptl_crystal_mounting_method 'Mitegenmount + Paratone'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.497
_oxdiff_exptl_absorpt_empirical_full_min 0.861