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_7046479
_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 H96 Ag Cl N4 Se2'
_chemical_formula_sum            'C54 H96 Ag Cl N4 Se2'
_chemical_formula_weight         1102.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-10
_audit_creation_method
;
Olex2 1.2
(compiled Apr  3 2018 11:26:26 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-04-16 deposited with the CCDC.
2018-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                92.768(2)
_cell_angle_beta                 99.075(2)
_cell_angle_gamma                102.185(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5173(3)
_cell_length_b                   13.8453(2)
_cell_length_c                   16.5647(3)
_cell_measurement_reflns_used    19138
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      28.9580
_cell_measurement_theta_min      2.9700
_cell_volume                     2761.04(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.901
_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    -62.00  38.00   1.00   25.00    --   10.25 -57.00 -60.00  100
  2  \w    -18.00  83.00   1.00   25.00    --   10.25  57.00  90.00  101
  3  \w    -83.00  17.00   1.00   25.00    --  -10.95 -57.00-150.00  100
  4  \w    -83.00  18.00   1.00   25.00    --  -10.95 -59.00 122.40  101
  5  \w    -20.00  51.00   1.00   25.00    --   10.25 -99.00-150.00   71
  6  \w      1.00  66.00   1.00   25.00    --   10.25-124.00 127.00   65
  7  \w    -14.00  85.00   1.00   25.00    --   10.25  38.00   0.00   99
  8  \w    -83.00 -36.00   1.00   25.00    --  -10.95 149.00-110.04   47
  9  \w    -49.00   8.00   1.00   25.00    --  -10.95  91.00-172.70   57
 10  \w    -80.00 -34.00   1.00   25.00    --  -10.95 145.00  33.60   46
;
_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      0.0229422000
_diffrn_orient_matrix_UB_12      0.0088935000
_diffrn_orient_matrix_UB_13      0.0423583000
_diffrn_orient_matrix_UB_21      0.0458114000
_diffrn_orient_matrix_UB_22      0.0348069000
_diffrn_orient_matrix_UB_23      -0.0092917000
_diffrn_orient_matrix_UB_31      -0.0289505000
_diffrn_orient_matrix_UB_32      0.0384199000
_diffrn_orient_matrix_UB_33      0.0036490000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            61661
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.672
_diffrn_reflns_theta_min         2.499
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.769
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.994
_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    1.326
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.282
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.082
_refine_diff_density_max         2.362
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         14091
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0432P)^2^+5.1368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1188
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10517
_reflns_number_total             14091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01506f2.cif
_cod_data_source_block           fn090
_cod_depositor_comments
'Adding full bibliography for 7046473--7046483.cif.'
_cod_database_code               7046479
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C54 H96 Ag Cl N4 Se2'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq,
Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41)
\\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C4(H4), C16(H16), C31(H31), C43(H43)
3.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B),
  C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C26(H26A,H26B), C27(H27A,H27B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
  C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C44(H44A,
 H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B),
 C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B),
  C54(H54A,H54B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C29(H29), C30(H30)
;
_shelx_res_checksum              13840
_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 1.249
_oxdiff_exptl_absorpt_empirical_full_min 0.826