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_7711149
_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         'C14 H21 I N2 O3'
_chemical_formula_sum            'C14 H21 I N2 O3'
_chemical_formula_weight         392.23
_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             2021-10-06
_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                83.712(3)
_cell_angle_beta                 71.291(3)
_cell_angle_gamma                65.959(3)
_cell_formula_units_Z            4
_cell_length_a                   10.6593(3)
_cell_length_b                   12.9198(4)
_cell_length_c                   13.3925(5)
_cell_measurement_reflns_used    8335
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      76.5610
_cell_measurement_theta_min      3.4640
_cell_volume                     1594.89(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_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   -106.00 -25.00   1.00    1.00    --  -41.90 -37.00-180.00   81
  2  \w    -77.00 -10.00   1.00    1.00    --  -41.90 125.00 -30.00   67
  3  \w    -61.00  24.00   1.00    1.00    --  -41.90  57.00 -30.00   85
  4  \w   -113.00 -18.00   1.00    1.00    --  -41.90 -37.00  90.00   95
  5  \w     53.00  92.00   1.00    1.00    --   41.90-125.00-180.00   39
  6  \w     44.00 109.00   1.00    1.00    --  112.00-111.00  90.00   65
  7  \w     88.00 132.00   1.00    1.00    --  112.00  45.00-150.00   44
  8  \w     92.00 144.00   1.00    1.00    --  112.00 -77.00 -90.00   52
  9  \w     36.00 109.00   1.00    1.00    --  112.00-111.00 -30.00   73
 10  \w     36.00 132.00   1.00    1.00    --  112.00 -30.00 -90.00   96
 11  \w     38.00 140.00   1.00    1.00    --  112.00 -30.00  30.00  102
 12  \w     44.00 109.00   1.00    1.00    --  112.00-111.00 -90.00   65
 13  \w    152.00 178.00   1.00    1.00    --  112.00  45.00-150.00   26
 14  \w     62.00 159.00   1.00    1.00    --  112.00  15.00 -60.00   97
 15  \w     36.00  71.00   1.00    1.00    --  112.00 -77.00 -90.00   35
 16  \w     52.00 145.00   1.00    1.00    --  112.00 -77.00  90.00   93
;
_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      0.0902576000
_diffrn_orient_matrix_UB_12      -0.1076508000
_diffrn_orient_matrix_UB_13      -0.0708397000
_diffrn_orient_matrix_UB_21      -0.0706594000
_diffrn_orient_matrix_UB_22      0.0592427000
_diffrn_orient_matrix_UB_23      -0.0860003000
_diffrn_orient_matrix_UB_31      0.1202469000
_diffrn_orient_matrix_UB_32      0.0442673000
_diffrn_orient_matrix_UB_33      -0.0484175000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10718
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.129
_diffrn_reflns_theta_min         3.485
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.858
_exptl_absorpt_correction_T_max  0.457
_exptl_absorpt_correction_T_min  0.082
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.633
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/DIPE'
_exptl_crystal_size_max          0.427
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.065
_refine_diff_density_max         1.197
_refine_diff_density_min         -1.424
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         6221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0547P)^2^+0.1801P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5820
_reflns_number_total             6221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01988d2.cif
_cod_data_source_block           2d
_cod_database_code               7711149
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.04
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B), C48(H48A,H48B),
 C49(H49A,H49B), C51(H51A,H51B), C52(H52A,H52B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C42(H42), C43(H43), C45(H45), C46(H46)
2.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C65(H65A,H65B,
 H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C)
;
_shelx_res_checksum              46035
_shelx_hkl_checksum              75251
_ins_header
;
TITL OIK019_numabs_ana1 in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  10.659345  12.919778  13.392520  83.7115  71.2915  65.9585
ZERR    4.00   0.000313   0.000376   0.000463   0.0026   0.0030   0.0028
LATT  1
SFAC C H N O I
UNIT 56.00 84.00 8.00 12.00 4.00
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 1.700
_oxdiff_exptl_absorpt_empirical_full_min 0.629