Reactivity of NHC/diphosphene-coordinated Au(I)-hydride.
Dhara, Debabrata; Scheschkewitz, David; Chandrasekhar, Vadapalli; Yildiz, Cem B.; Jana, Anukul; Chemical communications (Cambridge, England) 57 (2021) 809–812; doi:10.1039/d0cc05461e

data_7127587
_publ_section_title
;
 Reactivity of NHC/diphosphene-coordinated Au(I)-hydride.
;
_journal_issue                   6
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              809
_journal_page_last               812
_journal_paper_doi               10.1039/d0cc05461e
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C63 H67 Au N2 P2'
_chemical_formula_sum            'C63 H67 Au N2 P2'
_chemical_formula_weight         1111.09
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-29 deposited with the CCDC.	2020-12-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.320(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3820(9)
_cell_length_b                   17.2777(7)
_cell_length_c                   20.8054(11)
_cell_measurement_reflns_used    7579
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.7870
_cell_measurement_theta_min      2.6850
_cell_volume                     5780.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     50.00  91.00   0.50  120.00    --    7.10  77.00-150.00   82
  2  \w    -75.00   7.00   0.50  120.00    --   -7.50 -77.00 -60.00  164
  3  \w    -39.00 -11.00   0.50  120.00    --   -7.50 -82.00   0.00   56
  4  \w    -25.00  51.00   0.50  120.00    --   -7.50  38.00-150.00  152
  5  \w    -75.00  28.00   0.50  120.00    --   -7.50 -77.00  60.00  206
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0004692000
_diffrn_orient_matrix_UB_12      -0.0235795000
_diffrn_orient_matrix_UB_13      0.0280443000
_diffrn_orient_matrix_UB_21      0.0224139000
_diffrn_orient_matrix_UB_22      0.0290505000
_diffrn_orient_matrix_UB_23      0.0238449000
_diffrn_orient_matrix_UB_31      -0.0380186000
_diffrn_orient_matrix_UB_32      0.0168433000
_diffrn_orient_matrix_UB_33      -0.0018646000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0845
_diffrn_reflns_av_unetI/netI     0.0782
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            47511
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.533
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.638
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       block
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.630
_refine_diff_density_min         -1.007
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         10163
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0478P)^2^+11.2257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7518
_reflns_number_total             10163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05461e2.cif
_cod_data_source_block           aj0664
_cod_depositor_comments
'Adding full bibliography for 7127586--7127589.cif.'
_cod_database_code               7127587
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H N P Au'
_shelx_estimated_absorpt_t_max   0.742
_shelx_estimated_absorpt_t_min   0.709
_reflns_odcompleteness_completeness 99.84
_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
 C1-C2
 1.14 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C2)
Uanis(C38) = Uanis(C34)
4.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C19(H19), C57(H57), C18(H18), C44(H44), C42(H42), C59(H59),
 C43(H43), C24(H24), C48(H48), C26(H26), C35(H35), C33(H33), C50(H50), C4(H4),
 C5(H5), C6(H6), C8(H8), C7(H7)
4.b Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C), C15(H15A,H15B,H15C), C28(H28A,H28B,H28C), C12(H12A,H12B,
 H12C), C61(H61A,H61B,H61C), C54(H54A,H54B,H54C), C52(H52A,H52B,H52C), C14(H14A,
 H14B,H14C), C30(H30A,H30B,H30C), C37(H37A,H37B,H37C), C62(H62A,H62B,H62C),
 C39(H39A,H39B,H39C), C13(H13A,H13B,H13C), C29(H29A,H29B,H29C), C53(H53A,H53B,
 H53C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              34501
_shelx_hkl_checksum              17828
_shelx_fab_checksum              45984
_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 1.114
_oxdiff_exptl_absorpt_empirical_full_min 0.905