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_7046481
_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_moiety         'C54 H72 Ag N4 Se2, 4(C H Cl3), Cl'
_chemical_formula_sum            'C58 H76 Ag Cl13 N4 Se2'
_chemical_formula_weight         1555.87
_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             2017-12-19
_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                 106.086(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4565(4)
_cell_length_b                   20.0342(7)
_cell_length_c                   24.4535(6)
_cell_measurement_reflns_used    19804
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      74.8780
_cell_measurement_theta_min      3.5190
_cell_volume                     7746.5(4)
_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 0.993
_diffrn_measured_fraction_theta_max 0.977
_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    -81.00  22.00   1.00    6.00    --  -41.55  97.00  63.00  103
  2  \w     -1.00  81.00   1.00    6.00    --   41.55 -97.00 -44.00   82
  3  \w    101.00 178.00   1.00   30.00    --  109.13  97.00  63.00   77
  4  \w     28.00  88.00   1.00   30.00    --  109.13 -97.00 -44.00   60
  5  \w    -96.00  -2.00   1.00    6.00    --  -41.55 125.00-150.00   94
  6  \w   -116.00 -17.00   1.00    6.00    --  -41.55 -38.00 120.00   99
  7  \w     26.00 109.00   1.00   30.00    --  109.13 -94.00-180.00   83
  8  \w     36.00 135.00   1.00   30.00    --  109.13 -45.00 150.00   99
  9  \w     33.00 137.00   1.00   30.00    --  109.13 -30.00 120.00  104
 10  \w     36.00 121.00   1.00   30.00    --  109.13-125.00 120.00   85
 11  \w     37.00 138.00   1.00   30.00    --  109.13 -61.00 -60.00  101
 12  \w     94.00 178.00   1.00   30.00    --  109.13 125.00-120.00   84
 13  \w   -114.00 -13.00   1.00    6.00    --  -41.55 -57.00  60.00  101
 14  \w   -114.00 -13.00   1.00    6.00    --  -41.55 -57.00-120.00  101
 15  \w   -118.00  -9.00   1.00    6.00    --  -41.55 -77.00   0.00  109
 16  \w     56.00 178.00   1.00   30.00    --  109.13  15.00  60.00  122
 17  \w     81.00 178.00   1.00   30.00    --  109.13  30.00 -60.00   97
 18  \w     81.00 178.00   1.00   30.00    --  109.13  30.00-120.00   97
 19  \w     77.00 178.00   1.00   30.00    --  109.13  77.00 -60.00  101
 20  \w     83.00 178.00   1.00   30.00    --  109.13  45.00 120.00   95
 21  \w     81.00 178.00   1.00   30.00    --  109.13  30.00-180.00   97
 22  \w   -118.00  -9.00   1.00    6.00    --  -41.55 -77.00 120.00  109
 23  \w   -118.00  -9.00   1.00    6.00    --  -41.55 -77.00-150.00  109
 24  \w    -66.00  33.00   1.00    6.00    --  -41.55  38.00-150.00   99
 25  \w     80.00 174.00   1.00   30.00    --  109.13  61.00-120.00   94
 26  \w     80.00 178.00   1.00   30.00    --  109.13  61.00-180.00   98
 27  \w     80.00 178.00   1.00   30.00    --  109.13  61.00  60.00   98
;
_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      0.0056067000
_diffrn_orient_matrix_UB_12      0.0712877000
_diffrn_orient_matrix_UB_13      -0.0223466000
_diffrn_orient_matrix_UB_21      0.0814443000
_diffrn_orient_matrix_UB_22      0.0120836000
_diffrn_orient_matrix_UB_23      0.0482727000
_diffrn_orient_matrix_UB_31      0.0532047000
_diffrn_orient_matrix_UB_32      -0.0261566000
_diffrn_orient_matrix_UB_33      -0.0383124000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0989
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            119069
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.562
_diffrn_reflns_theta_min         2.899
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.553
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.918
_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    1.334
_exptl_crystal_description       plate
_exptl_crystal_F_000             3152
_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.077
_refine_diff_density_max         1.048
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         15710
_refine_ls_number_restraints     585
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1208
_refine_ls_R_factor_gt           0.0913
_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^)+40.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1653
_refine_ls_wR_factor_ref         0.1786
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9907
_reflns_number_total             15710
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01506f2.cif
_cod_data_source_block           fn018
_cod_depositor_comments
'Adding full bibliography for 7046473--7046483.cif.'
_cod_database_code               7046481
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C58 H76 Ag Cl13 N4 Se2'
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C55-Cl1A = C55-Cl2 = C55-Cl3
 1.75 with sigma of 0.01
 C56-Cl4 = C56-Cl5 = C56-Cl6
 1.75 with sigma of 0.01
 C57-Cl7 = C57-Cl8 = C57-Cl9
 1.75 with sigma of 0.01
 C58-Cl10 = C58-Cl11 = C58-Cl12
 1.75 with sigma of 0.01
 Cl1A-Cl2 = Cl2-Cl3 = Cl3-Cl1A
 2.88 with sigma of 0.02
 Cl4-Cl5 = Cl5-Cl6 = Cl6-Cl4
 2.88 with sigma of 0.02
 Cl7-Cl8 = Cl8-Cl9 = Cl9-Cl7
 2.88 with sigma of 0.02
 Cl10-Cl11 = Cl11-Cl12 = Cl12-Cl10
 2.88 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
4.a Ternary CH refined with riding coordinates:
 C49(H49), C52(H52), C10(H10), C13(H13), C22(H22), C40(H40), C37(H37),
 C25(H25), C55(H55), C57(H57), C58(H58), C56(H56)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C29(H29), C2(H2), C30(H30), C7(H7), C6(H6), C19(H19), C20(H20),
 C8(H8), C46(H46), C47(H47), C34(H34), C35(H35), C33(H33), C45(H45), C18(H18)
4.c Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C11(H11A,H11B,H11C), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C), C12(H12A,
 H12B,H12C), C53(H53A,H53B,H53C), C41(H41A,H41B,H41C), C54(H54A,H54B,H54C),
 C26(H26A,H26B,H26C), C15(H15A,H15B,H15C), C27(H27A,H27B,H27C), C39(H39A,H39B,
 H39C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              23829
_shelx_fab_checksum              29350
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.455
_oxdiff_exptl_absorpt_empirical_full_min 0.248