Synthesis of disubstituted furans catalysed by [(AuCl)2(μ-bis(phosphino)metallocene)] and Na[BArF24]
Gwinn, Reilly K.; Boggess, Anna E.; Winter, Elizabeth P.; Nataro, Chip; Dalton Transactions  (2022) –; doi:10.1039/D2DT02999E

data_7711546
_publ_section_title
;
 Synthesis of disubstituted furans catalysed by
 [(AuCl)2(\m-bis(phosphino)metallocene)] and Na[BArF24]
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02999E
_journal_year                    2022
_chemical_formula_moiety         'C34 H28 Au2 Cl2 P2 Ru'
_chemical_formula_sum            'C34 H28 Au2 Cl2 P2 Ru'
_chemical_formula_weight         1064.41
_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             2021-10-22
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2021-10-22 deposited with the CCDC.	2022-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.805(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7596(7)
_cell_length_b                   16.7100(12)
_cell_length_c                   10.6881(7)
_cell_measurement_reflns_used    9265
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.6500
_cell_measurement_theta_min      2.2830
_cell_volume                     1559.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.945
_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     82.00 110.00   0.50   10.25    --   20.00  54.00   0.00   56
  2  \w    -74.00 101.00   0.50   10.25    --   20.00  54.00 120.00  350
  3  \w    -74.00  -2.00   0.50   10.25    --   20.00  54.00  60.00  144
  4  \w     36.00  64.00   0.50   10.25    --   20.00  54.00  60.00   56
  5  \w     71.00 101.00   0.50   10.25    --   20.00  54.00  60.00   60
  6  \w    -56.00 -31.00   0.50   10.25    --   20.00  54.00-180.00   50
  7  \w     -1.00  24.00   0.50   10.25    --   20.00  54.00-180.00   50
  8  \w    -48.00 -23.00   0.50   10.25    --   20.00  54.00 -90.00   50
  9  \w     20.00  45.00   0.50   10.25    --   20.00  54.00 -90.00   50
 10  \w    -71.00 -46.00   0.50   10.25    --   20.00  54.00  90.00   50
 11  \w    -66.00 -40.00   0.50   10.25    --   20.00  54.00 150.00   52
 12  \w    -71.00  43.00   0.50   10.25    --   20.00  54.00   0.00  228
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0091857000
_diffrn_orient_matrix_UB_12      -0.0420311000
_diffrn_orient_matrix_UB_13      -0.0064366000
_diffrn_orient_matrix_UB_21      -0.0804250000
_diffrn_orient_matrix_UB_22      0.0050904000
_diffrn_orient_matrix_UB_23      -0.0112113000
_diffrn_orient_matrix_UB_31      0.0076922000
_diffrn_orient_matrix_UB_32      0.0032900000
_diffrn_orient_matrix_UB_33      -0.0652726000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15987
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.568
_diffrn_reflns_theta_min         2.268
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.164
_exptl_absorpt_correction_T_max  0.229
_exptl_absorpt_correction_T_min  0.056
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    2.268
_exptl_crystal_description       block
_exptl_crystal_F_000             996
_exptl_crystal_recrystallization_method
'Crystals of the compound were grown by vapor diffusion of diethyl ether in a solution of the compound in methylene chloride at room temperature.'
_exptl_crystal_size_max          0.453
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.214
_refine_diff_density_max         1.247
_refine_diff_density_min         -1.433
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         4527
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+1.9397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3961
_reflns_number_total             4527
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02999e2.cif
_cod_data_source_block           exp_11
_cod_database_code               7711546
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C34H28Au2Cl2P2Ru
_shelx_estimated_absorpt_t_max   0.220
_shelx_estimated_absorpt_t_min   0.091
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17)
;
_olex2_exptl_crystal_mounting_method 'Crystals were mounted using Paratone oil.'
_olex2_submission_original_sample_id C34HH28Au2Cl2P2Ru
_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 2.200
_oxdiff_exptl_absorpt_empirical_full_min 0.528