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_7711150
_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         'C27 H24 I3 N3 O6'
_chemical_formula_sum            'C27 H24 I3 N3 O6'
_chemical_formula_weight         867.19
_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   geom
_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                 109.522(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6502(4)
_cell_length_b                   9.9201(2)
_cell_length_c                   19.5464(5)
_cell_measurement_reflns_used    5135
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.4410
_cell_measurement_theta_min      3.1180
_cell_volume                     2860.16(13)
_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 0.997
_diffrn_measured_fraction_theta_max 0.993
_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    -82.00  -6.00   1.00    1.50    --  -42.03 125.00  30.00   76
  2  \w    -86.00 -53.00   1.00    1.50    --  -42.03 125.00-180.00   33
  3  \w    -49.00  -9.00   1.00    1.50    --  -42.03 125.00-180.00   40
  4  \w     47.00  74.00   1.00    1.50    --   42.03 -99.00 -60.00   27
  5  \w     26.00 115.00   1.00    1.50    --   42.03  37.00  60.00   89
  6  \w     87.00 178.00   1.00    6.00    --  112.00  45.00  60.00   91
  7  \w     83.00 178.00   1.00    6.00    --  112.00  61.00   0.00   95
  8  \w     41.00 135.00   1.00    6.00    --  112.00 -61.00-150.00   94
  9  \w     83.00 169.00   1.00    6.00    --  112.00  61.00  90.00   86
 10  \w    110.00 145.00   1.00    6.00    --  112.00  77.00 -60.00   35
;
_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      0.0774903000
_diffrn_orient_matrix_UB_12      0.0332454000
_diffrn_orient_matrix_UB_13      -0.0293366000
_diffrn_orient_matrix_UB_21      0.0462632000
_diffrn_orient_matrix_UB_22      -0.1347460000
_diffrn_orient_matrix_UB_23      0.0301097000
_diffrn_orient_matrix_UB_31      -0.0525207000
_diffrn_orient_matrix_UB_32      -0.0696074000
_diffrn_orient_matrix_UB_33      -0.0723250000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10773
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.128
_diffrn_reflns_theta_min         3.151
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    26.136
_exptl_absorpt_correction_T_max  0.420
_exptl_absorpt_correction_T_min  0.130
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/TBME'
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.059
_refine_diff_density_max         1.712
_refine_diff_density_min         -1.297
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+1.2425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4760
_reflns_number_total             5592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01988d2.cif
_cod_data_source_block           4b
_cod_database_code               7711150
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.11
_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 C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C22(H22), C23(H23), C25(H25), C26(H26), C32(H32),
 C33(H33), C35(H35), C36(H36), C42(H42), C43(H43), C45(H45), C46(H46)
2.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C37(H37A,H37B,H37C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              86423
_shelx_hkl_checksum              21005
_ins_header
;
TITL OIK009_numabs in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  15.650236   9.920134  19.546389  90.0000 109.5225  90.0000
ZERR    4.00   0.000378   0.000178   0.000536   0.0000   0.0028   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H N O I
UNIT 108.00 96.00 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 1.215
_oxdiff_exptl_absorpt_empirical_full_min 0.800