A tritopic carbanionic N-heterocyclic dicarbene and its homo- and heterometallic coinage metal complexes.
Zhang, Fan; Cao, Xiao-Ming; Wang, Jiwei; Jiao, Jiajun; Huang, Yongming; Shi, Min; Braunstein, Pierre; Zhang, Jun; Chemical communications (Cambridge, England) 54 (2018) 5736–5739; doi:10.1039/c8cc02192a

data_7121626
_publ_section_title
;
 A tritopic carbanionic N-heterocyclic dicarbene and its homo- and
 heterometallic coinage metal complexes.
;
_journal_issue                   45
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5736
_journal_page_last               5739
_journal_paper_doi               10.1039/c8cc02192a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C82 H79 Au3 N2 O P3, Cl'
_chemical_formula_sum            'C82 H79 Au3 Cl0.25 N2 O P3'
_chemical_formula_weight         1801.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-11-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2017-01-22 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.166(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9827(9)
_cell_length_b                   14.8116(11)
_cell_length_c                   36.774(2)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    130
_cell_measurement_theta_max      66.397
_cell_measurement_theta_min      3.832
_cell_volume                     7616.1(9)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_Laue_measured_fraction_full 0.936
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            37074
_diffrn_reflns_point_group_measured_fraction_full 0.936
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.673
_diffrn_reflns_theta_min         2.403
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.658
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1069 before and 0.0501 after correction.
The Ratio of minimum to maximum transmission is 0.5622.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       block
_exptl_crystal_F_000             3517
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.648
_refine_diff_density_min         -1.913
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     837
_refine_ls_number_reflns         12906
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0816P)^2^+17.6753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1390
_refine_ls_wR_factor_ref         0.1464
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11057
_reflns_number_total             12906
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc02192a2.cif
_cod_data_source_block           cu_dm16773_0m
_cod_depositor_comments
'Adding full bibliography for 7121624--7121626.cif.'
_cod_database_code               7121626
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.800
_shelx_estimated_absorpt_t_min   0.593
_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.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C23(H23), C26(H26)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C19(H19), C20(H20), C21(H21), C30(H30), C31(H31),
 C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40),
  C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49),
 C50(H50), C51(H51), C52(H52), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58),
  C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C66(H66), C67(H67),
 C68(H68), C69(H69), C70(H70), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76),
  C78(H78), C79(H79), C80(H80), C81(H81), C82(H82)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C)
;
_shelx_res_checksum              35873
_shelx_fab_checksum              70139
_olex2_submission_special_instructions 'No special instructions were received'