Straightforward access to chalcogenoureas derived from N-heterocyclic carbenes and their coordination chemistry.
Saab, Marina; Nelson, David J.; Tzouras, Nikolaos V.; A C A Bayrakdar, Tahani; Nolan, Steven P.; Nahra, Fady; Van Hecke, Kristof; Dalton transactions (Cambridge, England : 2003) 49 (2020) 12068–12081; doi:10.1039/d0dt02558e

data_7705115
_publ_section_title
;
 Straightforward access to chalcogenoureas derived from N-heterocyclic
 carbenes and their coordination chemistry.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12068
_journal_page_last               12081
_journal_paper_doi               10.1039/d0dt02558e
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C46 H64 Au N4 Se2, Au Cl2'
_chemical_formula_sum            'C46 H64 Au2 Cl2 N4 Se2'
_chemical_formula_weight         1295.77
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-16
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-17 deposited with the CCDC.	2020-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.16904(12)
_cell_length_b                   20.9451(4)
_cell_length_c                   28.7144(4)
_cell_measurement_reflns_used    17905
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      73.7650
_cell_measurement_theta_min      3.0450
_cell_volume                     4311.65(12)
_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      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -87.00  -6.00   1.00    1.00    --  -41.68 125.00 -30.00   81
  2  \w    -70.00  31.00   1.00    1.00    --  -41.68  57.00 -60.00  101
  3  \w      6.00  83.00   1.00    1.00    --   41.68 -99.00-120.00   77
  4  \w    103.00 178.00   1.00    3.50    --  106.01  77.00-150.00   75
  5  \w     23.00 107.00   1.00    3.50    --  106.01 -94.00 -30.00   84
  6  \w    109.00 112.00   1.00    3.50    --  106.01-125.00-180.00    3
  7  \w    104.00 105.00   1.00    3.50    --  106.01  97.00 -78.00    1
  8  \w    103.00 178.00   1.00    3.50    --  106.01  77.00  60.00   75
  9  \w     33.00 132.00   1.00    3.50    --  106.01 -45.00 150.00   99
 10  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00 -60.00  101
 11  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00-180.00  101
 12  \w     80.00 178.00   1.00    3.50    --  106.01  45.00 150.00   98
 13  \w     78.00 178.00   1.00    3.50    --  106.01  30.00 -60.00  100
 14  \w     77.00 178.00   1.00    3.50    --  106.01  61.00-180.00  101
 15  \w     78.00 178.00   1.00    3.50    --  106.01  30.00  30.00  100
 16  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00  60.00  101
 17  \w    -30.00  70.00   1.00    1.00    --   41.68 -57.00 120.00  100
 18  \w     77.00 178.00   1.00    3.50    --  106.01  61.00  90.00  101
 19  \w     80.00 178.00   1.00    3.50    --  106.01  45.00 -30.00   98
 20  \w     23.00 107.00   1.00    3.50    --  106.01 -94.00-150.00   84
 21  \w     80.00 178.00   1.00    3.50    --  106.01  45.00-120.00   98
 22  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00 120.00  101
 23  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00-120.00  101
 24  \w     23.00  48.00   1.00    3.50    --  106.01 -94.00  30.00   25
;
_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      0.1378788000
_diffrn_orient_matrix_UB_12      -0.0355076000
_diffrn_orient_matrix_UB_13      0.0320263000
_diffrn_orient_matrix_UB_21      0.1478890000
_diffrn_orient_matrix_UB_22      0.0012403000
_diffrn_orient_matrix_UB_23      -0.0388749000
_diffrn_orient_matrix_UB_31      0.0731221000
_diffrn_orient_matrix_UB_32      0.0643914000
_diffrn_orient_matrix_UB_33      0.0184150000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            52642
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.942
_diffrn_reflns_theta_min         2.611
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.971
_exptl_absorpt_correction_T_max  0.710
_exptl_absorpt_correction_T_min  0.142
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.996
_exptl_crystal_description       cube
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.046
_refine_diff_density_max         2.595
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.145
_refine_ls_abs_structure_details
;
 Flack x determined using 3008 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.013(6)
_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     505
_refine_ls_number_reflns         8640
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0443P)^2^+7.6568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0965
_reflns_Friedel_coverage         0.763
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                7762
_reflns_number_total             8640
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02558e2.cif
_cod_data_source_block           ms34-6
_cod_depositor_comments
'Adding full bibliography for 7705109--7705119.cif.'
_cod_database_code               7705115
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C46 H64 Au2 Cl2 N4 Se2'
_reflns_odcompleteness_completeness 99.93
_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.a Ternary CH refined with riding coordinates:
 C8(H8), C10(H10), C12(H12), C18(H18), C20(H20), C22(H22), C31(H31), C33(H33),
 C35(H35), C41(H41), C45(H45), C43(H43)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B), C11(H11A,H11B), C13(H13A,
 H13B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B),
 C21(H21A,H21B), C23(H23A,H23B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
  C32(H32A,H32B), C34(H34A,H34B), C36(H36A,H36B), C38(H38A,H38B), C40(H40A,
 H40B), C39(H39A,H39B), C46(H46A,H46B), C44(H44A,H44B), C42(H42A,H42B)
2.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C2(H2), C3(H3)
;
_shelx_res_checksum              52760
_olex2_date_sample_data_collection 2020-01-21
_olex2_exptl_crystal_mounting_method 'mounted on a LithoLoop'
_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 2.237
_oxdiff_exptl_absorpt_empirical_full_min 0.546