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_7121625
_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         'C64 H64 Au2 Br Cu N2 O P2'
_chemical_formula_sum            'C64 H64 Au2 Br Cu N2 O P2'
_chemical_formula_weight         1476.49
_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             2016-12-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2017-01-22 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.238(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6441(15)
_cell_length_b                   14.8478(13)
_cell_length_c                   24.590(2)
_cell_measurement_reflns_used    4710
_cell_measurement_temperature    130
_cell_measurement_theta_max      23.410
_cell_measurement_theta_min      2.21
_cell_volume                     6501.3(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1063
_diffrn_reflns_av_unetI/netI     0.1232
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            66695
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.65
_diffrn_reflns_theta_min         0.87
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.528
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1191 before and 0.0576 after correction.
The Ratio of minimum to maximum transmission is 0.6983.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       block
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.031
_refine_diff_density_min         -1.727
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     684
_refine_ls_number_reflns         12760
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0384P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0972
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8934
_reflns_number_total             12760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc02192a2.cif
_cod_data_source_block           mo_dm16837_0m
_cod_depositor_comments
'Adding full bibliography for 7121624--7121626.cif.'
_cod_original_cell_volume        6501.2(9)
_cod_database_code               7121625
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.770
_shelx_estimated_absorpt_t_min   0.608
_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. Uiso/Uaniso restraints and constraints
Br1 \\sim Br1' \\sim Cu1 \\sim Cu1': within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
Uanis(Cu1) \\sim Ueq, Uanis(Br1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Cu1) \\sim Ueq, Uanis(Br1) \\sim Ueq, Uanis(Cu1') \\sim Ueq, Uanis(Br1')
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: Br1(0.75) Br1'(0.25) Cu1(0.75) Cu1'(0.25)
4.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C23(H23), C26(H26)
4.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)
4.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              7799
_shelx_fab_checksum              61312
_olex2_submission_special_instructions 'No special instructions were received'