Mechanochemical synthesis of (hetero)aryl Au(i) complexes
Ingner, Fredric J. L.; Giustra, Zachary X.; Novosedlik, Sebastian; Orthaber, Andreas; Gates, Paul J.; Dyrager, Christine; Pilarski, Lukasz T.; Green Chemistry 22 (2020) 5648–5655; doi:10.1039/D0GC02263B

data_7241038
_publ_section_title
;
 Mechanochemical synthesis of (hetero)aryl Au(i) complexes
;
_journal_issue                   17
_journal_name_full               'Green Chemistry'
_journal_page_first              5648
_journal_page_last               5655
_journal_paper_doi               10.1039/D0GC02263B
_journal_volume                  22
_journal_year                    2020
_chemical_formula_moiety         'C18 H30 Au Cl2 P'
_chemical_formula_sum            'C18 H30 Au Cl2 P'
_chemical_formula_weight         545.25
_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             2020-05-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-06-04 deposited with the CCDC.	2020-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                65.9950(10)
_cell_angle_beta                 87.9480(10)
_cell_angle_gamma                71.8100(10)
_cell_formula_units_Z            2
_cell_length_a                   8.63460(10)
_cell_length_b                   11.49630(10)
_cell_length_c                   11.8740(2)
_cell_measurement_reflns_used    37688
_cell_measurement_temperature    170
_cell_measurement_theta_max      34.6030
_cell_measurement_theta_min      2.4750
_cell_volume                     1017.27(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      170
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.955
_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    -75.28 130.22   0.50    7.00    --  -36.52  73.79 109.24  411
  2  \w    -77.38 130.62   0.50    7.00    --  -37.62  73.79-124.87  416
  3  \w    -75.28 130.22   0.50    7.00    --  -36.52  73.79 -25.76  411
  4  \w    -75.28 130.22   0.50    7.00    --  -36.52  73.79  19.24  411
  5  \w    -75.28 130.22   0.50    7.00    --  -36.52  73.79 154.24  411
  6  \w    -75.28 130.22   0.50    7.00    --  -36.52  73.79 -70.76  411
  7  \w    -75.28 130.22   0.50    7.00    --  -36.52  73.79  64.24  411
  8  \w    -75.28 130.22   0.50    7.00    --  -36.52  73.79-160.76  411
  9  \w    -15.68 190.32   0.50    7.00    --   23.08  73.79  25.24  412
 10  \w    -15.68 190.32   0.50    7.00    --   23.08  73.79-130.76  412
 11  \f    -25.76 334.24   0.50    7.00 -26.68  13.08  73.79    --   720
 12  \f    -25.76 334.24   0.50    7.00 -76.28 -36.52  73.79    --   720
 13  \w    -15.68 190.32   0.50    7.00    --   23.08  73.79 127.24  412
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker-APEX II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0311900000
_diffrn_orient_matrix_UB_12      -0.0546095000
_diffrn_orient_matrix_UB_13      0.0194994000
_diffrn_orient_matrix_UB_21      0.0752057000
_diffrn_orient_matrix_UB_22      -0.0438505000
_diffrn_orient_matrix_UB_23      0.0367410000
_diffrn_orient_matrix_UB_31      -0.0305186000
_diffrn_orient_matrix_UB_32      0.0141056000
_diffrn_orient_matrix_UB_33      0.0509272000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0100
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14472
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.655
_diffrn_reflns_theta_min         2.051
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.568
_exptl_absorpt_correction_T_max  0.05685
_exptl_absorpt_correction_T_min  0.02553
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
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    1.780
_exptl_crystal_description       plate
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_crystal_size_rad          0.05
_refine_diff_density_max         2.537
_refine_diff_density_min         -2.471
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         14472
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0727P)^2^+3.8824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14087
_reflns_number_total             14472
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9837\% 
 around [-0.00 0.00 1.00] (reciprocal) or [0.13 -0.41 0.90] (direct)
;
_cod_data_source_file            d0gc02263b2.cif
_cod_data_source_block           ao_2_twin1_hklf5
_cod_depositor_comments
;Adding full bibliography for 7241038--7241039.cif.

 Adding full bibliography for 7241038--7241039.cif.
;
_cod_original_cell_volume        1017.27(2)
_cod_database_code               7241038
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C18H30AuCl2P
_shelx_estimated_absorpt_t_max   0.805
_shelx_estimated_absorpt_t_min   0.518
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7458(7)
 0.2542(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C4(H4)
3.b Idealised Me refined as rotating group:
 C9(H9a,H9b,H9c), C12(H12a,H12b,H12c), C16(H16a,H16b,H16c), C8(H8a,H8b,H8c),
 C17(H17a,H17b,H17c), C14(H14a,H14b,H14c), C10(H10a,H10b,H10c), C18(H18a,H18b,
 H18c), C13(H13a,H13b,H13c)
;
_shelx_res_checksum              38648
_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 1.794
_oxdiff_exptl_absorpt_empirical_full_min 0.485
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2