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_7703865
_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         'C16 H13 I O4'
_chemical_formula_sum            'C16 H13 I O4'
_chemical_formula_weight         396.16
_chemical_melting_point          388.15
_chemical_name_systematic
'dimethyl 2-iodo-[1,1'-biphenyl]-4,4'-dicarboxylate'
_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   geom
_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                105.230(4)
_cell_angle_beta                 107.161(4)
_cell_angle_gamma                102.068(4)
_cell_formula_units_Z            2
_cell_length_a                   7.8767(4)
_cell_length_b                   10.0877(5)
_cell_length_c                   10.6978(5)
_cell_measurement_reflns_used    10803
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      30.6590
_cell_measurement_theta_min      2.1690
_cell_volume                     744.83(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.15 (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      149.99(10)
_diffrn_detector                 'HyPix Bantam HPC-3000'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.944
_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     -2.00  62.00   0.50    7.00    --   20.00  54.00 -30.00  128
  2  \w     43.00  69.00   0.50    7.00    --   20.00  54.00  30.00   52
  3  \w     69.00  95.00   0.50    7.00    --   20.00  54.00  60.00   52
  4  \w     51.00  98.00   0.50    7.00    --   20.00  54.00 116.28   94
  5  \w     14.00  40.00   0.50    7.00    --   20.00  54.00 116.28   52
  6  \w     78.00 104.00   0.50    7.00    --   20.00  54.00-150.00   52
  7  \w    -17.00  60.00   0.50    7.00    --   20.00  54.00-150.00  154
  8  \w    -20.00   6.00   0.50    7.00    --   20.00  54.00  30.00   52
  9  \w    -33.00 108.50   0.50    7.00    --   20.00  54.00 -60.00  283
 10  \w    -35.00  77.50   0.50    7.00    --   20.00  54.00   0.00  225
 11  \w    -65.00  71.50   0.50    7.00    --   20.00  54.00 -90.00  273
 12  \w    -69.00 -43.00   0.50    7.00    --   20.00  54.00   0.00   52
 13  \w    -73.00  52.50   0.50    7.00    --   20.00  54.00  60.00  251
 14  \w    -72.00 -19.00   0.50    7.00    --   20.00  54.00 150.00  106
 15  \w    -66.00 -40.00   0.50    7.00    --   20.00  54.00  90.00   52
 16  \w    -66.00 -23.00   0.50    7.00    --   20.00  54.00  30.00   86
 17  \w    -72.00 -26.00   0.50    7.00    --   20.00  54.00 -30.00   92
 18  \w    -64.00 -39.00   0.50    7.00    --   20.00  54.00-120.00   50
 19  \w    -72.00 -46.00   0.50    7.00    --   20.00  54.00-150.00   52
 20  \w    -65.00  -8.00   0.50    7.00    --   20.00  54.00 116.28  114
;
_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      0.0918221000
_diffrn_orient_matrix_UB_12      0.0089692000
_diffrn_orient_matrix_UB_13      0.0441793000
_diffrn_orient_matrix_UB_21      0.0359116000
_diffrn_orient_matrix_UB_22      0.0575450000
_diffrn_orient_matrix_UB_23      -0.0208263000
_diffrn_orient_matrix_UB_31      -0.0105639000
_diffrn_orient_matrix_UB_32      0.0498657000
_diffrn_orient_matrix_UB_33      0.0555857000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14566
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        29.000
_diffrn_reflns_theta_max         30.660
_diffrn_reflns_theta_min         2.125
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.162
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.15 (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    1.766
_exptl_crystal_description       plate
_exptl_crystal_F_000             388
_exptl_crystal_recrystallization_method 'CH2Cl2 / Pet. Spirit'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         4355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0197
_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^)+(0.0290P)^2^+0.2186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0527
_refine_ls_wR_factor_ref         0.0533
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4087
_reflns_number_total             4355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00870b2.cif
_cod_data_source_block           exp_62me2bpdci
_cod_depositor_comments
'Adding full bibliography for 7703865--7703866.cif.'
_cod_database_code               7703865
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C16H13O4I
_chemical_oxdiff_usercomment
'Iodo biphenyl dicarboxylate from DCM/Pet Spirit'
_shelx_estimated_absorpt_t_max   0.863
_shelx_estimated_absorpt_t_min   0.478
_reflns_odcompleteness_completeness 95.49
_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 C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C2'(H2'), C3'(H3'), C5'(H5'), C6'(H6')
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C8'(H8'A,H8'B,H8'C)
;
_shelx_res_checksum              1497
_olex2_exptl_crystal_mounting_method 'Mitegen mount + 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 1.425
_oxdiff_exptl_absorpt_empirical_full_min 0.839