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_7241039
_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         'C17 H29 Au Cl F N P'
_chemical_formula_sum            'C17 H29 Au Cl F N P'
_chemical_formula_weight         529.80
_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             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                90
_cell_angle_beta                 90.975(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6986(10)
_cell_length_b                   18.586(2)
_cell_length_c                   12.1084(13)
_cell_measurement_reflns_used    9389
_cell_measurement_temperature    170
_cell_measurement_theta_max      30.082
_cell_measurement_theta_min      2.586
_cell_volume                     1957.3(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28991
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.705
_diffrn_reflns_theta_min         2.008
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.740
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1333 before and 0.0713 after correction.
The Ratio of minimum to maximum transmission is 0.6018.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_description       plate
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.598
_refine_diff_density_min         -1.597
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         6049
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0322
_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^)+2.1711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0745
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4792
_reflns_number_total             6049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0gc02263b2.cif
_cod_data_source_block           1
_cod_depositor_comments
;Adding full bibliography for 7241038--7241039.cif.

 Adding full bibliography for 7241038--7241039.cif.
;
_cod_database_code               7241039
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.512
_shelx_estimated_absorpt_t_min   0.457
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C5, F1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
3.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C8(H8A,H8B,H8C), C17(H17A,H17B,
 H17C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              3341
_olex2_submission_special_instructions 'No special instructions were received'