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_7058882
_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         'C40 H62 Au Br2 N4 O2 P2, C F3 O3 S'
_chemical_formula_sum            'C41 H62 Au Br2 F3 N4 O5 P2 S'
_chemical_formula_weight         1198.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-10-07 deposited with the CCDC.    2019-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.269(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5747(3)
_cell_length_b                   28.8162(6)
_cell_length_c                   14.7781(3)
_cell_measurement_reflns_used    5027
_cell_measurement_temperature    303.1(8)
_cell_measurement_theta_max      29.1150
_cell_measurement_theta_min      3.1220
_cell_volume                     4864.71(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 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 (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      303.1(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1274
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.838
_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    -25.00   4.00   0.10   10.00    --  -18.52 -99.00 150.00  290
  2  \w    -48.00  63.00   0.10   10.00    --   18.52 -19.00  90.00 1110
  3  \w    -47.00  32.00   0.10   10.00    --   18.52 -57.00  30.00  790
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0153638000
_diffrn_orient_matrix_UB_12      -0.0141026000
_diffrn_orient_matrix_UB_13      -0.0394610000
_diffrn_orient_matrix_UB_21      0.0172240000
_diffrn_orient_matrix_UB_22      0.0179877000
_diffrn_orient_matrix_UB_23      -0.0277637000
_diffrn_orient_matrix_UB_31      0.0576331000
_diffrn_orient_matrix_UB_32      -0.0091204000
_diffrn_orient_matrix_UB_33      0.0062212000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.838
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10660
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.838
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.293
_diffrn_reflns_theta_min         2.515
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.831
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_description       block
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5570
_refine_ls_number_restraints     242
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+7.6409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5199
_reflns_number_total             5570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj04911h2.cif
_cod_data_source_block           9-otf
_cod_original_cell_volume        4864.69(19)
_cod_database_code               7058882
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Au Br2 C20 N2 H20 F3 S1 O3'
_chemical_oxdiff_usercomment     'Mes2AuBr2OTf da ACN/Et2O'
_shelx_estimated_absorpt_t_max   0.644
_shelx_estimated_absorpt_t_min   0.283
_reflns_odcompleteness_completeness 99.15
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Restrained distances
 C17A-C13 \\sim C17B-C13 \\sim C13-C16A \\sim C13-C16B \\sim C15A-C13 \\sim
C15B-C13
 with sigma of 0.02
 C18A-C14 \\sim C18B-C14 \\sim C20A-C14 \\sim C20B-C14 \\sim C19B-C14 \\sim
C19A-C14
 with sigma of 0.02
 C20B-C19B \\sim C20B-C18B \\sim C19B-C18B \\sim C18A-C19A \\sim C18A-C20A
\\sim C19A-C20A
 with sigma of 0.04
 C14-P1 \\sim C14-C20B \\sim C14-C19B \\sim C14-C18B \\sim C14-C18A \\sim
C14-C19A \\sim C14-C20A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C19B) = Uanis(C19A) = Uanis(C20B) = Uanis(C20A) = Uanis(C18B) =
Uanis(C18A)
4. Rigid body (RIGU) restrains
 C1, C2, C3, C9, C10, C8, C7, C13, C12, C5, C6, C11, C14, C16B, C17B, C4, C20B,
  C19B, C18B, C15B, C17A, C16A, C15A, C18A, C19A, C20A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, S2, O3, O4, C15, F7, F8, F9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C16B)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17B)=Sof(H17A)=Sof(H17B)=
 Sof(H17C)=Sof(C15B)=Sof(H15A)=Sof(H15B)=Sof(H15C)=1-FVAR(1)
 Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C16A)=Sof(H16D)=Sof(H16E)=
 Sof(H16F)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=FVAR(1)
 Sof(C20B)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C18B)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=1-FVAR(2)
 Sof(C19B)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C18A)=Sof(H18D)=Sof(H18E)=
 Sof(H18F)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=FVAR(2)
 Fixed Sof: S2(0.5) O3(0.5) O4(0.5) O5(0.5) C15(0.5) F7(0.5) F8(0.5) F9(0.5)
6.a Free rotating group:
 S2(O3,O4,O5,C15,F7,F8,F9)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C12(H12), C6(H6)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C16B(H16A,H16B,H16C), C17B(H17A,H17B,
 H17C), C4(H4A,H4B,H4C), C20B(H20A,H20B,H20C), C19B(H19A,H19B,H19C), C18B(H18A,
 H18B,H18C), C15B(H15A,H15B,H15C), C17A(H17D,H17E,H17F), C16A(H16D,H16E,H16F),
 C15A(H15D,H15E,H15F), C18A(H18D,H18E,H18F), C19A(H19D,H19E,H19F), C20A(H20D,
 H20E,H20F)
;
_shelx_res_checksum              22626
_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 1.468
_oxdiff_exptl_absorpt_empirical_full_min 0.753