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_7127589
_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         'C67 H73 Au N4 P2, C6 H6'
_chemical_formula_sum            'C73 H79 Au N4 P2'
_chemical_formula_weight         1271.30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                80.844(2)
_cell_angle_beta                 81.813(2)
_cell_angle_gamma                86.997(2)
_cell_formula_units_Z            4
_cell_length_a                   11.8644(2)
_cell_length_b                   21.3145(4)
_cell_length_c                   26.4459(6)
_cell_measurement_reflns_used    24650
_cell_measurement_temperature    120.02(10)
_cell_measurement_theta_max      28.6570
_cell_measurement_theta_min      2.2160
_cell_volume                     6532.2(2)
_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      120.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.870
_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    -35.00  46.00   0.50  124.61    --    7.10 -82.00 -90.00  162
  2  \w     50.00  77.00   0.50  124.61    --    7.10  77.00-120.00   54
  3  \w     51.00  95.00   0.50  124.61    --    7.10  77.00 -30.00   88
  4  \w    -26.00  35.00   0.50  124.61    --    7.10 -82.00-180.00  122
  5  \w    -34.00  64.00   0.50  124.61    --    7.10  38.00  90.00  196
  6  \w     67.00  95.00   0.50  124.61    --    7.10  77.00  60.00   56
  7  \w    -52.00  20.00   0.50  124.61    --   -7.50 -82.00 150.00  144
  8  \w    -28.00  34.00   0.50  124.61    --   -7.50 -82.00  30.00  124
  9  \w      7.00  75.00   0.50  124.61    --   -7.50 -19.00 -90.00  136
 10  \w    -93.00 -24.00   0.50  124.61    --   -7.50 -19.00 -90.00  138
;
_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      0.0033589000
_diffrn_orient_matrix_UB_12      0.0289058000
_diffrn_orient_matrix_UB_13      -0.0175600000
_diffrn_orient_matrix_UB_21      -0.0112114000
_diffrn_orient_matrix_UB_22      0.0173581000
_diffrn_orient_matrix_UB_23      0.0210279000
_diffrn_orient_matrix_UB_31      0.0592830000
_diffrn_orient_matrix_UB_32      0.0005990000
_diffrn_orient_matrix_UB_33      0.0011716000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.0777
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.870
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            113322
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.870
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.023
_diffrn_reflns_theta_min         1.805
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.345
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80994
_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    1.293
_exptl_crystal_description       plate
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1473
_refine_ls_number_reflns         30284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+3.4810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22156
_reflns_number_total             30284
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05461e2.cif
_cod_data_source_block           aj0721-1
_cod_depositor_comments
;
Adding full bibliography for 7127586--7127589.cif.

2024-11-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C146 H158 Au2 N8 P4'
_cod_original_formula_weight         2542.61
_cod_original_formula_moiety         '2(C67 H73 Au N4 P2), 2(C6 H6)'
_cod_original_formula_units_Z            2
_cod_database_code               7127589
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         CHPNAu
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.750
_reflns_odcompleteness_completeness 99.77
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N4(H4), C101(H101), C35(H35), C12(H12), C11(H11), C36(H36), N8(H8), C92(H92),
 C25(H25), C40(H40), C109(H109), C10(H10), C102(H102), C103(H103), C27(H27),
 C77(H77), C144(H144), C107(H107), C42(H42), C34(H34), C118(H118), C49(H49),
 C143(H143), C146(H146), C83(H83), C142(H142), C57(H57), C18(H18), C60(H60),
 C116(H116), C51(H51), C16(H16), C85(H85), C133(H133), C61(H61), C79(H79),
 C125(H125), C124(H124), C145(H145), C67(H67), C134(H134), C141(H141), C66(H66),
  C94(H94), C78(H78), C65(H65), C63(H63), C58(H58), C59(H59), C131(H131),
 C128(H128), C64(H64), C132(H132), C135(H135), C130(H130), C139(H139),
 C137(H137), C136(H136), C138(H138), C140(H140), C126(H126), C127(H127)
2.b Idealised Me refined as rotating group:
 C74(H74A,H74B,H74C), C31(H31A,H31B,H31C), C55(H55A,H55B,H55C), C46(H46A,H46B,
 H46C), C22(H22A,H22B,H22C), C98(H98A,H98B,H98C), C71(H71A,H71B,H71C),
 C120(H12A,H12B,H12C), C113(H11A,H11B,H11C), C6(H6A,H6B,H6C), C87(H87A,H87B,
 H87C), C122(H12D,H12E,H12F), C45(H45A,H45B,H45C), C7(H7A,H7B,H7C), C29(H29A,
 H29B,H29C), C5(H5A,H5B,H5C), C111(H11D,H11E,H11F), C4(H4A,H4B,H4C), C30(H30A,
 H30B,H30C), C89(H89A,H89B,H89C), C73(H73A,H73B,H73C), C44(H44A,H44B,H44C),
 C96(H96A,H96B,H96C), C54(H54A,H54B,H54C), C121(H12G,H12H,H12I), C72(H72A,H72B,
 H72C), C97(H97A,H97B,H97C), C112(H11G,H11H,H11I), C20(H20A,H20B,H20C),
 C53(H53A,H53B,H53C), C21(H21A,H21B,H21C), C88(H88A,H88B,H88C)
;
_shelx_res_checksum              68195
_shelx_hkl_checksum              33142
_shelx_fab_checksum              30758
_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 1.284
_oxdiff_exptl_absorpt_empirical_full_min 0.780