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_7705111
_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_formula_moiety         'C29 H40 Au Cl N2 Se, C H2 Cl2'
_chemical_formula_sum            'C30 H42 Au Cl3 N2 Se'
_chemical_formula_weight         812.94
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 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                79.757(2)
_cell_angle_beta                 73.610(2)
_cell_angle_gamma                74.505(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9301(3)
_cell_length_b                   10.5160(4)
_cell_length_c                   17.0134(4)
_cell_measurement_reflns_used    20964
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      29.5580
_cell_measurement_theta_min      2.8980
_cell_volume                     1632.36(9)
_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_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 0.897
_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    -14.00  85.00   1.00   18.55    --   10.40  38.00 120.00   99
  2  \w    -20.00  51.00   1.00   18.55    --   10.40 -99.00  30.00   71
  3  \w    -20.00  51.00   1.00   18.55    --   10.40 -99.00 -90.00   71
  4  \w    -18.00  84.00   1.00   18.55    --   10.40  57.00-150.00  102
  5  \w    -39.00  62.00   1.00   18.55    --  -11.11  57.00 -30.00  101
  6  \w    -20.00  30.00   1.00   18.55    --  -11.11 -99.00-150.00   50
  7  \w    -64.00  35.00   1.00   18.55    --   10.40 -38.00 120.00   99
  8  \w    -20.00  26.00   1.00   18.55    --   10.40 -99.00-180.00   46
  9  \w    -20.00  30.00   1.00   18.55    --  -11.11 -99.00 -60.00   50
 10  \w    -36.00  63.00   1.00   18.55    --  -11.11  38.00 120.00   99
;
_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      0.0133123000
_diffrn_orient_matrix_UB_12      -0.0679225000
_diffrn_orient_matrix_UB_13      -0.0055571000
_diffrn_orient_matrix_UB_21      -0.0744842000
_diffrn_orient_matrix_UB_22      0.0070956000
_diffrn_orient_matrix_UB_23      0.0035669000
_diffrn_orient_matrix_UB_31      0.0112933000
_diffrn_orient_matrix_UB_32      0.0172125000
_diffrn_orient_matrix_UB_33      -0.0432246000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36446
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.712
_diffrn_reflns_theta_min         2.511
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.888
_exptl_absorpt_correction_T_max  0.621
_exptl_absorpt_correction_T_min  0.350
_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            'light colourless'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_description       irregular
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.117
_refine_diff_density_max         1.498
_refine_diff_density_min         -1.271
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         8332
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0270
_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^)+(0.0206P)^2^+1.2012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0574
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7582
_reflns_number_total             8332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02558e2.cif
_cod_data_source_block           ms030
_cod_depositor_comments
'Adding full bibliography for 7705109--7705119.cif.'
_cod_database_code               7705111
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C29 H40 Au Cl N2 Se'
_shelx_estimated_absorpt_t_max   0.546
_shelx_estimated_absorpt_t_min   0.453
_reflns_odcompleteness_completeness 99.91
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl2A-C30A = Cl3A-C30A
 1.746 with sigma of 0.01
 Cl2B-C30B = Cl3B-C30B
 1.746 with sigma of 0.01
 Cl2A-Cl3A
 2.9 with sigma of 0.01
 Cl2B-Cl3B
 2.9 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(Cl2A) = Uanis(Cl2B)
Uanis(Cl3A) = Uanis(Cl3B)
Uanis(C30A) = Uanis(C30B)
4. Others
 Sof(Cl2B)=Sof(Cl3B)=Sof(C30B)=Sof(H30C)=Sof(H30D)=1-FVAR(1)
 Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(Cl3A)=Sof(Cl2A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27)
5.b Secondary CH2 refined with riding coordinates:
 C30A(H30A,H30B), C30B(H30C,H30D)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22)
5.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              10763
_olex2_date_sample_data_collection 2019-01-30
_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 1.286
_oxdiff_exptl_absorpt_empirical_full_min 0.819