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_7127588
_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         'C59 H69 Au N4 O2 P2'
_chemical_formula_sum            'C59 H69 Au N4 O2 P2'
_chemical_formula_weight         1125.08
_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                 109.411(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5661(6)
_cell_length_b                   16.4929(5)
_cell_length_c                   18.7879(7)
_cell_measurement_reflns_used    24944
_cell_measurement_temperature    119.97(10)
_cell_measurement_theta_max      28.6120
_cell_measurement_theta_min      2.7110
_cell_volume                     5426.0(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      119.97(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.890
_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     -5.00  36.00   0.50   35.00    --    7.10  46.00  23.00   82
  2  \w    -45.00 -19.00   0.50   35.00    --    7.10 -46.00-125.00   52
  3  \w    -60.00 -35.00   0.50   35.00    --   -7.50 -46.00-125.00   50
  4  \w     13.00  39.00   0.50   35.00    --   -7.50  46.00  23.00   52
  5  \w     51.00  87.00   0.50   35.00    --    7.10  77.00-150.00   72
  6  \w     55.00  96.00   0.50   35.00    --    7.10  77.00 -30.00   82
  7  \w     51.00  76.00   0.50   35.00    --    7.10  77.00 -60.00   50
  8  \w     60.00  95.00   0.50   35.00    --    7.10  77.00 -90.00   70
  9  \w    -76.00  27.00   0.50   35.00    --   -7.50 -77.00 120.00  206
 10  \w    -55.00 -17.00   0.50   35.00    --   -7.50 -77.00 150.00   76
 11  \w    -24.00   2.00   0.50   35.00    --   -7.50 -82.00-180.00   52
 12  \w    -11.00  34.00   0.50   35.00    --   -7.50 -82.00-150.00   90
 13  \w    -56.00 -28.00   0.50   35.00    --   -7.50 -82.00-150.00   56
;
_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      0.0345432000
_diffrn_orient_matrix_UB_12      -0.0154657000
_diffrn_orient_matrix_UB_13      0.0256238000
_diffrn_orient_matrix_UB_21      0.0207589000
_diffrn_orient_matrix_UB_22      0.0189624000
_diffrn_orient_matrix_UB_23      -0.0210031000
_diffrn_orient_matrix_UB_31      0.0040193000
_diffrn_orient_matrix_UB_32      0.0353730000
_diffrn_orient_matrix_UB_33      0.0224732000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1026
_diffrn_reflns_av_unetI/netI     0.0765
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            73725
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.001
_diffrn_reflns_theta_min         2.546
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.815
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68887
_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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.071
_refine_diff_density_min         -2.264
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         12845
_refine_ls_number_restraints     439
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0673
_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^)+(0.0756P)^2^+25.1917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1674
_refine_ls_wR_factor_ref         0.1768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9359
_reflns_number_total             12845
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05461e2.cif
_cod_data_source_block           aj0737
_cod_depositor_comments
'Adding full bibliography for 7127586--7127589.cif.'
_cod_database_code               7127588
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C40 H60 N4 O P2 Au'
_shelx_estimated_absorpt_t_max   0.747
_shelx_estimated_absorpt_t_min   0.711
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C59-C58
 1.54 with sigma of 0.002
 O1-C57
 1.28 with sigma of 0.002
 O2-C57
 1.4 with sigma of 0.002
 N3-N4
 1.45 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C57) = Uanis(C56)
Uanis(O2) = Uanis(C57)
Uanis(C56) = Uanis(N4) = Uanis(N3)
Uanis(O1) = Uanis(C57)
Uanis(C58) = Uanis(O2)
Uanis(C59) = Uanis(C58)
4. Rigid body (RIGU) restrains
 C58, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C58
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C58(H58A,H58B)
5.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C35(H35), C34(H34), C16(H16), C27(H27), C10(H10), C25(H25),
 C18(H18), C40(H40), C42(H42), N3(H3), C12(H12), C49(H49), C11(H11), C51(H51),
 C56(H56)
5.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C53(H53A,H53B,H53C), C7(H7A,H7B,H7C), C22(H22A,H22B,H22C),
 C55(H55A,H55B,H55C), C46(H46A,H46B,H46C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C20(H20A,H20B,H20C), C31(H31A,H31B,H31C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C21(H21A,H21B,H21C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C54(H54A,
 H54B,H54C), C59(H59A,H59B,H59C)
;
_shelx_res_checksum              14214
_shelx_hkl_checksum              14875
_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 1.239
_oxdiff_exptl_absorpt_empirical_full_min 0.824