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_7711146
_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 H38 Ag2 N4 O4'
_chemical_formula_sum            'C24 H38 Ag2 N4 O4'
_chemical_formula_weight         662.32
_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             2022-04-26
_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                82.991(14)
_cell_angle_beta                 72.900(14)
_cell_angle_gamma                73.381(15)
_cell_formula_units_Z            1
_cell_length_a                   6.8349(11)
_cell_length_b                   9.4356(18)
_cell_length_c                   11.4549(19)
_cell_measurement_reflns_used    1211
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      23.8550
_cell_measurement_theta_min      2.9650
_cell_volume                     676.0(2)
_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      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0107
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.987
_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    -87.00   0.00   1.00    2.00    --  -18.29 -57.00  60.00   87
  2  \w    -48.00  41.00   1.00    2.00    --  -18.29  77.00-150.00   89
  3  \w    -22.00  10.00   1.00    2.00    --  -18.29 -77.00  90.00   32
  4  \w    -20.00  10.00   1.00    2.00    --  -18.29 -77.00 -30.00   30
  5  \w    -39.00  -6.00   1.00    2.00    --  -18.29  57.00 -30.00   33
  6  \w    -50.00  40.00   1.00    2.00    --   19.23 -37.00 -60.00   90
  7  \w      3.00  31.00   1.00    2.00    --   19.23  77.00 -60.00   28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0993176000
_diffrn_orient_matrix_UB_12      -0.0152506000
_diffrn_orient_matrix_UB_13      0.0288682000
_diffrn_orient_matrix_UB_21      0.0336579000
_diffrn_orient_matrix_UB_22      -0.0660197000
_diffrn_orient_matrix_UB_23      -0.0324200000
_diffrn_orient_matrix_UB_31      0.0408966000
_diffrn_orient_matrix_UB_32      -0.0396794000
_diffrn_orient_matrix_UB_33      0.0481609000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.1168
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4536
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.864
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.483
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             336
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetone+DMSO'
_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.053
_refine_diff_density_max         1.648
_refine_diff_density_min         -1.608
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         2745
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0514P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1124
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1914
_reflns_number_total             2745
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 6.4240\% 
around [0.09 -0.62 0.78] (reciprocal) or [0.20 -0.78 0.59] (direct)
;
_cod_data_source_file            d2dt01988d2.cif
_cod_data_source_block           1c
_cod_database_code               7711146
_shelxl_version_number           2014/6
_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), C3(H3), C5(H5), C6(H6)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C)
;
_shelx_res_checksum              72998
_shelx_hkl_checksum              2892
_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 1.293
_oxdiff_exptl_absorpt_empirical_full_min 0.736
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2