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_7711145
_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         'C10 H18 Ag2 O4'
_chemical_formula_sum            'C10 H18 Ag2 O4'
_chemical_formula_weight         417.98
_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             2022-03-17
_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                108.220(7)
_cell_angle_beta                 90.240(5)
_cell_angle_gamma                94.770(6)
_cell_formula_units_Z            4
_cell_length_a                   5.7752(4)
_cell_length_b                   13.4830(10)
_cell_length_c                   16.9347(12)
_cell_measurement_reflns_used    2398
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      76.6360
_cell_measurement_theta_min      3.6450
_cell_volume                     1247.57(16)
_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      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.989
_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   -115.00 -14.00   1.00    1.00    --  -41.40 -57.00  90.00  101
  2  \w    -55.00  35.00   1.00    1.00    --  -41.40  77.00-150.00   90
  3  \w     28.00  97.00   1.00    1.00    --   41.40-125.00  60.00   69
  4  \w     14.00 115.00   1.00    1.00    --   41.40  57.00 -30.00  101
  5  \w     39.00 118.00   1.00    2.00    --  112.00 -45.00  60.00   79
  6  \w     40.00 140.00   1.00    2.00    --  112.00 -61.00-180.00  100
  7  \w     60.00 145.00   1.00    2.00    --  112.00 -77.00 -30.00   85
  8  \w     38.00 109.00   1.00    2.00    --  112.00-111.00   0.00   71
  9  \w     39.00 109.00   1.00    2.00    --  112.00-111.00 150.00   70
 10  \w     37.00 139.00   1.00    2.00    --  112.00 -30.00 -60.00  102
 11  \w    124.00 175.00   1.00    2.00    --  112.00  45.00   0.00   51
 12  \w     37.00 109.00   1.00    2.00    --  112.00-111.00-150.00   72
 13  \w     31.00 165.00   1.00    2.00    --  112.00 -15.00-180.00  134
;
_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      0.0484401000
_diffrn_orient_matrix_UB_12      0.1199043000
_diffrn_orient_matrix_UB_13      0.0367489000
_diffrn_orient_matrix_UB_21      -0.2386811000
_diffrn_orient_matrix_UB_22      0.0139712000
_diffrn_orient_matrix_UB_23      -0.0340886000
_diffrn_orient_matrix_UB_31      -0.1114056000
_diffrn_orient_matrix_UB_32      -0.0036137000
_diffrn_orient_matrix_UB_33      0.0816656000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0716
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8322
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.125
_diffrn_reflns_theta_min         3.465
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    25.178
_exptl_absorpt_correction_T_max  0.829
_exptl_absorpt_correction_T_min  0.164
_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    2.225
_exptl_crystal_description       needle
_exptl_crystal_F_000             816
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/DIPE'
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.008
_refine_diff_density_max         1.261
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         4849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0225P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3314
_reflns_number_total             4849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01988d2.cif
_cod_data_source_block           1
_cod_database_code               7711145
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 98.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C37(H37A,H37B,H37C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C),
 C47(H47A,H47B,H47C)
;
_shelx_res_checksum              61185
_shelx_hkl_checksum              21471
_ins_header
;
TITL OIS-016_numabs_ana1 in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   5.775206  13.482956  16.934656 108.2203  90.2400  94.7698
ZERR    8.00   0.000367   0.001024   0.001184   0.0065   0.0055   0.0057
LATT  1
SFAC C H O Ag
UNIT 40.00 72.00 16.00 8.00
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 1.270
_oxdiff_exptl_absorpt_empirical_full_min 0.747