Coinage metal complexes of selenoureas derived from N-heterocyclic carbenes.
Nahra, Fady; Van Hecke, Kristof; Kennedy, Alan R.; Nelson, David J.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 10671–10684; doi:10.1039/c8dt01506f

data_7046475
_publ_section_title
;
 Coinage metal complexes of selenoureas derived from N-heterocyclic
 carbenes.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10671
_journal_page_last               10684
_journal_paper_doi               10.1039/c8dt01506f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C45.5 H73 Ag Cl2 N6 O Se3'
_chemical_formula_weight         1135.74
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-19
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-16 deposited with the CCDC.
2018-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.277(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.3848(4)
_cell_length_b                   15.0419(2)
_cell_length_c                   27.9825(4)
_cell_measurement_reflns_used    31188
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      74.5980
_cell_measurement_theta_min      3.3270
_cell_volume                     11064.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.970
_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   -119.00  42.00   1.00    4.00    --  -41.68  11.00 135.00  161
  2  \w   -125.00  36.00   1.00    4.00    --  -41.68 -11.00 -37.00  161
  3  \w    -36.00 125.00   1.00    4.00    --   41.68  11.00 135.00  161
  4  \w    -42.00 119.00   1.00    4.00    --   41.68 -11.00 -37.00  161
  5  \w     31.00 178.00   1.00   25.00    --  109.13  11.00 135.00  147
  6  \w     26.00 178.00   1.00   25.00    --  109.13 -11.00 -37.00  152
  7  \w      1.00  83.00   1.00    4.00    --   41.68 -99.00  60.00   82
  8  \w     23.00  98.00   1.00    4.00    --   41.68-125.00-150.00   75
  9  \w     36.00 121.00   1.00   25.00    --  109.13-125.00 -90.00   85
 10  \w     36.00 135.00   1.00   25.00    --  109.13 -45.00-180.00   99
 11  \w     83.00 178.00   1.00   25.00    --  109.13  45.00  30.00   95
 12  \w     26.00  96.00   1.00   25.00    --  109.13 -94.00 120.00   70
 13  \w     80.00 178.00   1.00   25.00    --  109.13  61.00 -30.00   98
 14  \w     29.00 108.00   1.00   25.00    --  109.13 -94.00   0.00   79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0017103000
_diffrn_orient_matrix_UB_12      -0.0099496000
_diffrn_orient_matrix_UB_13      0.0543249000
_diffrn_orient_matrix_UB_21      0.0582200000
_diffrn_orient_matrix_UB_22      -0.0115242000
_diffrn_orient_matrix_UB_23      0.0169054000
_diffrn_orient_matrix_UB_31      0.0066118000
_diffrn_orient_matrix_UB_32      0.1012274000
_diffrn_orient_matrix_UB_33      0.0072347000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            103069
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.598
_diffrn_reflns_theta_min         3.291
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.338
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       block
_exptl_crystal_F_000             4632
_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.063
_refine_diff_density_max         2.081
_refine_diff_density_min         -1.352
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1054
_refine_ls_number_reflns         22282
_refine_ls_number_restraints     735
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1018P)^2^+15.3061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1750
_refine_ls_wR_factor_ref         0.1895
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17427
_reflns_number_total             22282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01506f2.cif
_cod_data_source_block           fn021
_cod_depositor_comments
'Adding full bibliography for 7046473--7046483.cif.'
_cod_database_code               7046475
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.691
_shelx_estimated_absorpt_t_min   0.348
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C91-Cl4
 1.746 with sigma of 0.01
 C91-Cl3
 1.746 with sigma of 0.01
 Cl3-Cl4
 2.897 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C4(H4), C10(H10), C19(H19), C25(H25), C34(H34), C40(H40), C49(H49), C55(H55),
 C64(H64), C70(H70), C79(H79), C85(H85)
4.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C11(H11A,
 H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B),
  C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,
 H30B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
 C39(H39A,H39B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B),
  C45(H45A,H45B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,
 H53B), C54(H54A,H54B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B),
 C59(H59A,H59B), C60(H60A,H60B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B),
  C68(H68A,H68B), C69(H69A,H69B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,
 H73B), C74(H74A,H74B), C75(H75A,H75B), C80(H80A,H80B), C81(H81A,H81B),
 C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B), C86(H86A,H86B), C87(H87A,H87B),
  C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B), C91(H91A,H91B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C17(H17), C18(H18), C32(H32), C33(H33), C47(H47), C48(H48),
 C62(H62), C63(H63), C77(H77), C78(H78)
;
_shelx_res_checksum              29805
_shelx_fab_checksum              56277
_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop'
_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 1.824
_oxdiff_exptl_absorpt_empirical_full_min 0.725