Janus bis(NHCs) tuned by heteroatom-bridge oxidation states.
Naz, Nabila Rauf; Schnakenburg, Gregor; Mikeházi, Antal; Kelemen, Zsolt; Nyulászi, László; Boeré, René T; Streubel, Rainer; Chemical communications (Cambridge, England) 56 (2020) 2646–2649; doi:10.1039/c9cc08468a

data_7125779
_publ_section_title
;
 Janus bis(NHCs) tuned by heteroatom-bridge oxidation states.
;
_journal_issue                   17
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2646
_journal_page_last               2649
_journal_paper_doi               10.1039/c9cc08468a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C30 H57 Au2 Cl2 N6 O2 P2, 2(Cl)'
_chemical_formula_sum            'C30 H57 Au2 Cl4 N6 O2 P2'
_chemical_formula_weight         1131.49
_chemical_name_systematic        NRN-198
_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             2018-06-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2019-05-29 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                103.05(6)
_cell_angle_beta                 97.19(7)
_cell_angle_gamma                116.10(6)
_cell_formula_units_Z            1
_cell_length_a                   10.102(13)
_cell_length_b                   10.857(14)
_cell_length_c                   11.856(13)
_cell_measurement_reflns_used    1958
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.10
_cell_measurement_theta_min      2.21
_cell_volume                     1099(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1058
_diffrn_reflns_av_unetI/netI     0.1060
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_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       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23427
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.824
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.012
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.2655
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1498 before and 0.0808 after correction. The Ratio of minimum to maximum transmission is 0.3966. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_description       block
_exptl_crystal_F_000             551
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         6.077
_refine_diff_density_min         -2.424
_refine_diff_density_rms         0.340
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         5302
_refine_ls_number_restraints     264
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.0773
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0976P)^2^+29.4002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.2138
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3674
_reflns_number_total             5302
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08468a2.cif
_cod_data_source_block           5631g
_cod_depositor_comments
'Adding full bibliography for 7125777--7125780.cif.'
_cod_original_cell_volume        1099(2)
_cod_database_code               7125779
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.513
_shelx_estimated_absorpt_t_min   0.321
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C13S-C12S
 1.5 with sigma of 0.001
 C7S-C6S
 1.5 with sigma of 0.01
 C5-C4
 1.5 with sigma of 0.01
 C12S-N3S
 1.47 with sigma of 0.001
 N3S-C13S
 2.7 with sigma of 0.01
 C7-C6 = C6-C5 = C5-C4 = C5S-C4 = C6S-C5S = C7S-C6S = C9-C8 = C9-C10 = C11-C10
 = C13S-C12S = C13-C12 = C15-C14 = C15S-C14S
 1.5 with sigma of 0.01
 N3-C12 = N3S-C12S = N3-C14 = N3S-C14S
 1.46 with sigma of 0.01
3. Rigid bond restraints
 C10, C11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P, O1S
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C4 \\sim C5 \\sim C5S \\sim C6 \\sim C6S \\sim C7 \\sim C7S: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C15S \\sim C14S \\sim N3S \\sim C14 \\sim C15 \\sim C12S \\sim N3 \\sim C12
\\sim C13 \\sim C13S: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C14S) \\sim Ueq, Uanis(C13S) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 C15S, C14S, N3S, N3, C12, C13, C13S, C12S, C14, C15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(N3S)=Sof(C12S)=Sof(H12C)=Sof(H12D)=Sof(C13S)=Sof(H13D)=Sof(H13E)=
 Sof(H13F)=Sof(C14S)=Sof(H14C)=Sof(H14D)=Sof(C15S)=Sof(H15D)=Sof(H15E)=
 Sof(H15F)=1-FVAR(1)
 Sof(N3)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
 Sof(H4BC)=Sof(H4BD)=Sof(C5S)=Sof(H5SA)=Sof(H5SB)=Sof(C6S)=Sof(H6SA)=Sof(H6SB)=
 Sof(C7S)=Sof(H7SA)=Sof(H7SB)=Sof(H7SC)=1-FVAR(2)
 Sof(H4AA)=Sof(H4AB)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=FVAR(2)
 Fixed Sof: O(0.5) O1S(0.5) H1S(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C4(H4AA,H4AB), C4(H4BC,H4BD), C5(H5A,H5B), C5S(H5SA,H5SB), C6(H6A,H6B),
 C6S(H6SA,H6SB), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B),
 C12S(H12C,H12D), C14(H14A,H14B), C14S(H14C,H14D)
7.b Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C7S(H7SA,H7SB,H7SC), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C13S(H13D,H13E,H13F), C15(H15A,H15B,H15C), C15S(H15D,H15E,H15F)
7.c Idealised tetrahedral OH refined as rotating group:
 O1S(H1S)
;
_shelx_res_checksum              77282
_shelx_hkl_checksum              54460
_shelx_fab_checksum              94869
_olex2_submission_special_instructions 'No special instructions were received'