Coordination chemistry of gold with N-Phosphine Oxide-Substituted Imidazolylidenes (POxIms)
Branzi, Lorenzo; Baron, Marco; Armelao, Lidia; Rancan, Marzio; Sgarbossa, Paolo; Graiff, Claudia; Pöthig, Alexander; Biffis, Andrea; New Journal of Chemistry 43 (2019) 17275–17283; doi:10.1039/C9NJ04911H

data_7058885
_publ_section_title
;
 Coordination chemistry of gold with N-Phosphine Oxide-Substituted
 Imidazolylidenes (POxIms)
;
_journal_issue                   44
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17275
_journal_page_last               17283
_journal_paper_doi               10.1039/C9NJ04911H
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         '2(C20 H31 Au Br1.95 Cl1.05 N2 O P), C2 H3 N'
_chemical_formula_sum            'C42 H65 Au2 Br3.88 Cl2.12 N5 O2 P2'
_chemical_formula_weight         1513.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-27 deposited with the CCDC.    2019-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.602(2)
_cell_length_b                   15.0955(14)
_cell_length_c                   15.1623(15)
_cell_measurement_reflns_used    9363
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.62
_cell_volume                     5173.2(8)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'APEX3 (Bruker, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0872
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            62675
_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         27.874
_diffrn_reflns_theta_min         2.622
_exptl_absorpt_coefficient_mu    8.872
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7023
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1278 before and 0.0765 after correction.
The Ratio of minimum to maximum transmission is 0.4260.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_description       prism
_exptl_crystal_F_000             2911
_exptl_crystal_size_max          0.464
_exptl_crystal_size_mid          0.354
_exptl_crystal_size_min          0.215
_refine_diff_density_max         1.400
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.164
_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     320
_refine_ls_number_reflns         6166
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0092P)^2^+16.6386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4860
_reflns_number_total             6166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj04911h2.cif
_cod_data_source_block           pseudo-10
_cod_original_cell_volume        5173.1(8)
_cod_database_code               7058885
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.251
_shelx_estimated_absorpt_t_min   0.105
_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
Au1 \\sim Br2 \\sim Br3 \\sim Br1 \\sim Cl2 \\sim Cl3 \\sim Cl1: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Cl2) \\sim Ueq, Uanis(Cl3) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(Br2)
\\sim Ueq, Uanis(Br3) \\sim Ueq, Uanis(Br1) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
3. Others
 Sof(Cl2)=1-FVAR(1)
 Sof(Br2)=FVAR(1)
 Sof(Cl3)=1-FVAR(2)
 Sof(Br3)=FVAR(2)
 Sof(Cl1)=1-FVAR(3)
 Sof(Br1)=FVAR(3)
 Fixed Sof: N3(0.5) C22(0.5) H22A(0.5) H22B(0.5) H22C(0.5) C21(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C2(H2), C3(H3), C6(H6)
4.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C12(H12A,H12B,
 H12C), C16(H16A,H16B,H16C), C11(H11A,H11B,H11C), C18(H18A,H18B,H18C), C20(H20A,
 H20B,H20C), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              24566
_olex2_submission_special_instructions 'No special instructions were received'