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_7711152
_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         'C44 H38 Ag3 N7 O6'
_chemical_formula_sum            'C44 H38 Ag3 N7 O6'
_chemical_formula_weight         1084.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-17
_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                90
_cell_angle_beta                 91.048(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8504(9)
_cell_length_b                   10.5290(3)
_cell_length_c                   19.2520(4)
_cell_measurement_reflns_used    6022
_cell_measurement_temperature    119.96(19)
_cell_measurement_theta_max      27.2700
_cell_measurement_theta_min      2.7410
_cell_volume                     4225.8(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      119.96(19)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0053
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -42.00  12.00   1.00   50.00    --  -18.29 -77.00  90.00   54
  2  \w    -42.00  12.00   1.00   50.00    --  -18.29 -77.00 -60.00   54
  3  \w    -53.00  45.00   1.00   50.00    --   19.23 -37.00 -60.00   98
  4  \w    -50.00  41.00   1.00   50.00    --   19.23 -57.00  30.00   91
  5  \w     39.00  95.00   1.00   50.00    --   19.23 178.00   0.00   56
  6  \w    -50.00  41.00   1.00   50.00    --   19.23 -57.00 150.00   91
  7  \w    -11.00  42.00   1.00   50.00    --   19.23  77.00 -90.00   53
  8  \w     15.00  92.00   1.00   50.00    --   19.23  37.00 120.00   77
;
_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      0.0314925000
_diffrn_orient_matrix_UB_12      -0.0181438000
_diffrn_orient_matrix_UB_13      0.0104991000
_diffrn_orient_matrix_UB_21      0.0129206000
_diffrn_orient_matrix_UB_22      0.0447381000
_diffrn_orient_matrix_UB_23      -0.0234317000
_diffrn_orient_matrix_UB_31      -0.0001891000
_diffrn_orient_matrix_UB_32      0.0469579000
_diffrn_orient_matrix_UB_33      0.0264205000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_unetI/netI     0.0758
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43231
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.116
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.433
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90540
_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    1.705
_exptl_crystal_description       plate
_exptl_crystal_F_000             2160
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pyridine+DMSO/TBME'
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.009
_refine_diff_density_max         2.161
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         8637
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.209
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0794
_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^)+(0.0312P)^2^+16.7942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1319
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6802
_reflns_number_total             8637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01988d2.cif
_cod_data_source_block           3a_py_4
_cod_database_code               7711152
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 N51, C52, C53, C54, C55, C56
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a 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), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56),
 C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C72(H72), C73(H73), C74(H74),
  C75(H75), C76(H76), C82(H82), C83(H83), C84(H84), C85(H85), C86(H86)
;
_shelx_res_checksum              56126
_shelx_hkl_checksum              44191
_ins_header
;
TITL OIK096_scale1 in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073  20.850443  10.528970  19.251987  90.0000  91.0477  90.0000
ZERR    4.00   0.000931   0.000340   0.000442   0.0000   0.0029   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H N O Ag
UNIT 176.00 152.00 28.00 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 1.164
_oxdiff_exptl_absorpt_empirical_full_min 0.887