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_7127586
_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         'C61 H69 Au N2 O4 P2'
_chemical_formula_sum            'C61 H69 Au N2 O4 P2'
_chemical_formula_weight         1153.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 94.729(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2527(3)
_cell_length_b                   18.7361(5)
_cell_length_c                   25.0944(7)
_cell_measurement_reflns_used    21898
_cell_measurement_temperature    119.99(10)
_cell_measurement_theta_max      27.6620
_cell_measurement_theta_min      2.2210
_cell_volume                     5741.3(3)
_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_environment      N~2~
_diffrn_ambient_temperature      119.99(10)
_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     10.00  35.00   0.50   36.25    --    7.10  71.00 -75.00   50
  2  \w    -20.00   5.00   0.50   36.25    --    7.10 -71.00 153.00   50
  3  \w     -5.00  20.00   0.50   36.25    --   -7.50  71.00 -75.00   50
  4  \w    -59.00 -34.00   0.50   36.25    --   -7.50 -71.00 153.00   50
  5  \w     52.00  96.00   0.50   36.25    --    7.10  77.00 150.00   88
  6  \w     58.00  90.00   0.50   36.25    --    7.10  77.00 120.00   64
  7  \w    -48.00  33.00   0.50   36.25    --   -7.50  38.00 -60.00  162
  8  \w    -38.00   8.00   0.50   36.25    --   -7.50 -57.00  60.00   92
  9  \w    -81.00 -55.00   0.50   36.25    --   -7.50 -57.00  30.00   52
 10  \w    -52.00  -4.00   0.50   36.25    --   -7.50  19.00  90.00   96
 11  \w     18.00  43.00   0.50   36.25    --   -7.50  19.00  90.00   50
 12  \w    -29.00  70.00   0.50   36.25    --   -7.50  57.00-150.00  198
;
_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      0.0293568000
_diffrn_orient_matrix_UB_12      0.0235770000
_diffrn_orient_matrix_UB_13      0.0180651000
_diffrn_orient_matrix_UB_21      0.0192546000
_diffrn_orient_matrix_UB_22      0.0189043000
_diffrn_orient_matrix_UB_23      -0.0218489000
_diffrn_orient_matrix_UB_31      -0.0462670000
_diffrn_orient_matrix_UB_32      0.0228232000
_diffrn_orient_matrix_UB_33      -0.0005550000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            71185
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.098
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.664
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79013
_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    1.334
_exptl_crystal_description       block
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.584
_refine_diff_density_min         -1.850
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         10139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0285P)^2^+31.6748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0979
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8535
_reflns_number_total             10139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05461e2.cif
_cod_data_source_block           aj0690-1
_cod_depositor_comments
'Adding full bibliography for 7127586--7127589.cif.'
_cod_database_code               7127586
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C1H1N1P1O1Au1
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.723
_reflns_odcompleteness_completeness 99.89
_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.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C18(H18), C27(H27), C42(H42), C12(H12), C10(H10), C40(H40),
 C25(H25), C51(H51), C36(H36), C11(H11), C59(H59), C34(H34), C49(H49), C35(H35)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C20(H20A,H20B,H20C), C29(H29A,H29B,H29C), C55(H55A,H55B,
 H55C), C31(H31A,H31B,H31C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C6(H6A,
 H6B,H6C), C4(H4A,H4B,H4C), C46(H46A,H46B,H46C), C5(H5A,H5B,H5C), C53(H53A,H53B,
 H53C), C44(H44A,H44B,H44C), C30(H30A,H30B,H30C), C54(H54A,H54B,H54C), C61(H61A,
 H61B,H61C), C45(H45A,H45B,H45C), C58(H58A,H58B,H58C)
;
_shelx_res_checksum              55552
_shelx_hkl_checksum              78425
_shelx_fab_checksum              33997
_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 1.316
_oxdiff_exptl_absorpt_empirical_full_min 0.778