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_7705117
_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         'C54 H76 Ag N4 Se2, Ag Cl2, 2(C H2 Cl2)'
_chemical_formula_sum            'C56 H80 Ag2 Cl6 N4 Se2'
_chemical_formula_weight         1395.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                90
_cell_angle_beta                 110.519(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.4825(2)
_cell_length_b                   25.6926(4)
_cell_length_c                   12.1018(2)
_cell_measurement_reflns_used    23005
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      29.4370
_cell_measurement_theta_min      3.1630
_cell_volume                     3052.51(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.887
_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  105.00    --   10.40  38.00 -90.00   99
  2  \w    -64.00  35.00   1.00  105.00    --   10.40 -38.00  90.00   99
  3  \w    -20.00  30.00   1.00  105.00    --  -11.11 -99.00  30.00   50
  4  \w    -66.00  43.00   1.00  105.00    --   10.40 -77.00 -60.00  109
  5  \w    -14.00  11.00   1.00  105.00    --   10.40  38.00  60.00   25
  6  \w    -70.00 -27.00   1.00  105.00    --  -11.11 131.00-153.03   43
;
_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      -0.0017928000
_diffrn_orient_matrix_UB_12      0.0274236000
_diffrn_orient_matrix_UB_13      0.0060147000
_diffrn_orient_matrix_UB_21      -0.0568374000
_diffrn_orient_matrix_UB_22      -0.0024450000
_diffrn_orient_matrix_UB_23      0.0185355000
_diffrn_orient_matrix_UB_31      0.0445581000
_diffrn_orient_matrix_UB_32      -0.0020137000
_diffrn_orient_matrix_UB_33      0.0594850000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36467
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.805
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.751
_diffrn_reflns_theta_min         2.611
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.135
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.720
_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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.444(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     648
_refine_ls_number_reflns         14022
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0252P)^2^+1.3293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0572
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_full    0.928
_reflns_Friedel_fraction_max     0.721
_reflns_number_gt                13186
_reflns_number_total             14022
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02558e2.cif
_cod_data_source_block           ms045
_cod_depositor_comments
'Adding full bibliography for 7705109--7705119.cif.'
_cod_database_code               7705117
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C27 H38 Ag N2 Se Cl2'
_shelx_estimated_absorpt_t_max   0.831
_shelx_estimated_absorpt_t_min   0.729
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.556(6)
 0.444(6)
2. 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
3.a Ternary CH refined with riding coordinates:
 C37(H37), C40(H40), C52(H52), C22(H22), C13(H13), C49(H49), C25(H25), C10(H10)
3.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C3(H3A,H3B), C2(H2A,H2B), C30(H30A,H30B), C56(H56A,H56B),
 C55(H55A,H55B)
3.c Aromatic/amide H refined with riding coordinates:
 C47(H47), C35(H35), C6(H6), C18(H18), C8(H8), C7(H7), C19(H19), C34(H34),
 C33(H33), C20(H20), C46(H46), C45(H45)
3.d Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C54(H54A,H54B,H54C), C12(H12A,H12B,H12C), C26(H26A,H26B,
 H26C), C15(H15A,H15B,H15C), C24(H24B,H24A,H24C), C42(H42A,H42B,H42C), C23(H23A,
 H23B,H23C), C11(H11A,H11B,H11C), C27(H27A,H27B,H27C), C53(H53A,H53B,H53C),
 C39(H39A,H39B,H39C), C50(H50A,H50B,H50C), C14(H14A,H14B,H14C), C38(H38A,H38B,
 H38C), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              73709
_olex2_date_sample_data_collection 2019-03-15
_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 1.156
_oxdiff_exptl_absorpt_empirical_full_min 0.877