Synthesis, reactivity and catalytic activity of Au-PAd<sub>3</sub> complexes.
Voloshkin, Vladislav A.; Saab, Marina; Van Hecke, Kristof; Lau, Sii Hong; Carrow, Bradley P.; Nolan, Steven P.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 13872–13879; doi:10.1039/d0dt03330h

data_7705580
_publ_section_title
;
 Synthesis, reactivity and catalytic activity of Au-PAd<sub>3</sub>
 complexes.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13872
_journal_page_last               13879
_journal_paper_doi               10.1039/d0dt03330h
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C60 H90 Au P2, C2 F6 N O4 S2, 2(C H2 Cl2)'
_chemical_formula_sum            'C64 H94 Au Cl4 F6 N O4 P2 S2'
_chemical_formula_weight         1520.23
_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             2020-04-05
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-16 deposited with the CCDC.	2020-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.125(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3017(3)
_cell_length_b                   21.3897(4)
_cell_length_c                   27.2421(7)
_cell_measurement_reflns_used    11339
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      73.4800
_cell_measurement_theta_min      3.6470
_cell_volume                     6379.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.912
_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    -66.00  33.00   1.00    1.75    --  -41.68  38.00  30.00   99
  2  \w    -30.00  70.00   1.00    1.75    --   41.68 -57.00 150.00  100
  3  \w     80.00 178.00   1.00    6.00    --  106.01  45.00-120.00   98
  4  \w     33.00 112.00   1.00    6.00    --  106.01-125.00-120.00   79
  5  \w    104.00 178.00   1.00    6.00    --  106.01 107.00 -99.00   74
  6  \w    103.00 178.00   1.00    6.00    --  106.01  77.00-180.00   75
  7  \w     33.00 112.00   1.00    6.00    --  106.01-125.00 -30.00   79
  8  \w   -115.00 -14.00   1.00    1.75    --  -41.68 -57.00  60.00  101
  9  \w   -115.00 -14.00   1.00    1.75    --  -41.68 -57.00 -90.00  101
 10  \w     53.00 120.00   1.00    6.00    --  106.01  15.00  60.00   67
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0116893000
_diffrn_orient_matrix_UB_12      -0.0380030000
_diffrn_orient_matrix_UB_13      0.1156248000
_diffrn_orient_matrix_UB_21      0.0108403000
_diffrn_orient_matrix_UB_22      0.0610563000
_diffrn_orient_matrix_UB_23      0.0738603000
_diffrn_orient_matrix_UB_31      -0.0615345000
_diffrn_orient_matrix_UB_32      0.0034903000
_diffrn_orient_matrix_UB_33      -0.0314377000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0979
_diffrn_reflns_av_unetI/netI     0.0947
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            31902
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.997
_diffrn_reflns_theta_min         2.755
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.508
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.787
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       needle
_exptl_crystal_F_000             3120
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.044
_refine_diff_density_max         3.492
_refine_diff_density_min         -4.811
_refine_diff_density_rms         0.219
_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     764
_refine_ls_number_reflns         11815
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0856
_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^)+180.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1850
_refine_ls_wR_factor_ref         0.1924
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9847
_reflns_number_total             11815
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03330h2.cif
_cod_data_source_block           vl147
_cod_depositor_comments
'Adding full bibliography for 7705580--7705581.cif.'
_cod_database_code               7705580
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C10 H10 N2 O2 Au1 Cl1 P1 S1'
_shelx_estimated_absorpt_t_max   0.734
_shelx_estimated_absorpt_t_min   0.362
_reflns_odcompleteness_completeness 95.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C63-Cl1A = C63-Cl2A
 1.75 with sigma of 0.01
 C63-Cl1B = C63-Cl2B
 1.75 with sigma of 0.01
 Cl1A-Cl2A
 2.9 with sigma of 0.01
 Cl1B-Cl2B
 2.9 with sigma of 0.01
3. Rigid bond restraints
 C63, Cl1A, Cl1B, Cl2A, Cl2B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C63 \\sim Cl1A \\sim Cl1B \\sim Cl2A \\sim Cl2B: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.04
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C29) \\sim
Ueq, Uanis(C43) \\sim Ueq, Uanis(C51) \\sim Ueq: with sigma of 0.005 and sigma
for terminal atoms of 0.01
Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C21) \\sim Ueq, Uanis(P1) \\sim Ueq, Uanis(P2) \\sim Ueq: with sigma of
0.003 and sigma for terminal atoms of 0.006
Uanis(Cl1A) = Uanis(Cl1B)
Uanis(Cl2A) = Uanis(Cl2B)
5. Others
 Sof(H63C)=Sof(H63D)=Sof(Cl2B)=Sof(Cl1B)=1-FVAR(1)
 Sof(H63A)=Sof(H63B)=Sof(Cl1A)=Sof(Cl2A)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C44(H44), C17(H17), C38(H38), C54(H54), C29(H29), C7(H7), C23(H23), C56(H56),
 C34(H34), C48(H48), C13(H13), C46(H46), C58(H58), C3(H3), C31(H31), C5(H5),
 C15(H15), C36(H36)
6.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C25(H25A,H25B), C49(H49A,H49B), C61(H61A,H61B), C33(H33A,
 H33B), C59(H59A,H59B), C30(H30A,H30B), C2(H2A,H2B), C4(H4A,H4B), C39(H39A,
 H39B), C60(H60A,H60B), C28(H28A,H28B), C53(H53A,H53B), C10(H10A,H10B),
 C35(H35A,H35B), C57(H57A,H57B), C9(H9A,H9B), C12(H12A,H12B), C8(H8A,H8B),
 C41(H41A,H41B), C43(H43A,H43B), C19(H19A,H19B), C45(H45A,H45B), C24(H24A,H24B),
  C37(H37A,H37B), C16(H16A,H16B), C6(H6A,H6B), C51(H51A,H51B), C47(H47A,H47B),
 C18(H18A,H18B), C55(H55A,H55B), C20(H20A,H20B), C40(H40A,H40B), C27(H27A,H27B),
  C50(H50A,H50B), C14(H14A,H14B), C62(H62A,H62B), C63(H63A,H63B), C63(H63C,H63D)
;
_shelx_res_checksum              1355
_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop'
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 55.710
_oxdiff_exptl_absorpt_empirical_full_min 0.096