Carbonyl Hypoiodites from Pivalic and Trimesic Acid and their Silver(I) Intermediates
Ward, Jas S.; Martõnova, Jevgenija; Wilson, Laura M. E.; Kramer, Eric; Aav, Riina; Rissanen, Kari; Dalton Transactions  (2022) –; doi:10.1039/D2DT01988D

data_7711151
_publ_section_title
;
 Carbonyl Hypoiodites from Pivalic and Trimesic Acid and their Silver(I)
 Intermediates
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01988D
_journal_year                    2022
_chemical_formula_moiety         'C24 H18 I3 N3 O6, H2 O'
_chemical_formula_sum            'C24 H20 I3 N3 O7'
_chemical_formula_weight         843.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-18 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.437(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7621(2)
_cell_length_b                   24.2101(5)
_cell_length_c                   11.4785(2)
_cell_measurement_reflns_used    4914
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      75.4470
_cell_measurement_theta_min      4.2400
_cell_volume                     2711.99(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_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    -70.00  29.00   1.00    2.50    --  -42.03  57.00 150.00   99
  2  \w    -29.00  69.00   1.00    2.50    --   42.03 -57.00 -90.00   98
  3  \w     75.00 140.00   1.00   10.00    --  112.00 -30.00-150.00   65
  4  \w     51.00 102.00   1.00   10.00    --  112.00 -30.00 -60.00   51
  5  \w     86.00 173.00   1.00   10.00    --  112.00  30.00-150.00   87
  6  \w     36.00 109.00   1.00   10.00    --  112.00-111.00 -90.00   73
  7  \w     51.00 141.00   1.00   10.00    --  112.00 -77.00 -60.00   90
  8  \w    106.00 140.00   1.00   10.00    --  112.00 -30.00 -60.00   34
  9  \w     36.00  73.00   1.00   10.00    --  112.00 -30.00-150.00   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0140428000
_diffrn_orient_matrix_UB_12      0.0602446000
_diffrn_orient_matrix_UB_13      -0.0415498000
_diffrn_orient_matrix_UB_21      0.0402470000
_diffrn_orient_matrix_UB_22      -0.0176329000
_diffrn_orient_matrix_UB_23      -0.1235276000
_diffrn_orient_matrix_UB_31      -0.1520661000
_diffrn_orient_matrix_UB_32      -0.0102317000
_diffrn_orient_matrix_UB_33      -0.0322700000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10193
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.110
_diffrn_reflns_theta_min         3.651
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    27.569
_exptl_absorpt_correction_T_max  0.564
_exptl_absorpt_correction_T_min  0.088
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.065
_exptl_crystal_description       needle
_exptl_crystal_F_000             1600
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/pentane'
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         5294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0260
_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^)+(0.0302P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0662
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4622
_reflns_number_total             5294
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01988d2.cif
_cod_data_source_block           4a
_cod_database_code               7711151
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O101(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44),
  C45(H45), C46(H46)
;
_shelx_res_checksum              93630
_shelx_hkl_checksum              51560
_ins_header
;
TITL OIK008_numabs_ana2 in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184   9.762113  24.210092  11.478524  90.0000  91.4366  90.0000
ZERR    4.00   0.000152   0.000477   0.000206   0.0000   0.0017   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H N O I
UNIT 96.00 72.00 12.00 24.00 12.00
TREF
HKLF 4
END
;
_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 1.341
_oxdiff_exptl_absorpt_empirical_full_min 0.707