Tripodal S-Ligand Complexes of Copper(I) as Catalysts for Alkene Aziridination, Sulfide Sulfimidation, and C-H Amination.
Lam, Tsz Lung; Tso, Ken Chi-Hang; Cao, Bei; Yang, Chen; Chen, Daqing; Chang, Xiao-Yong; Huang, Jie-Sheng; Che, Chi-Ming; Inorganic chemistry 56 (2017) 4253–4257; doi:10.1021/acs.inorgchem.7b00226

data_4345795
_publ_section_title
;
 Tripodal S-Ligand Complexes of Copper(I) as Catalysts for Alkene
 Aziridination, Sulfide Sulfimidation, and C-H Amination.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4253
_journal_page_last               4257
_journal_paper_doi               10.1021/acs.inorgchem.7b00226
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C45 H37 Au B N6 P S3'
_chemical_formula_sum            'C45 H37 Au B N6 P S3'
_chemical_formula_weight         996.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                74.905(4)
_cell_angle_beta                 85.876(5)
_cell_angle_gamma                89.894(5)
_cell_formula_units_Z            4
_cell_length_a                   9.3602(6)
_cell_length_b                   20.5287(12)
_cell_length_c                   22.3310(14)
_cell_measurement_reflns_used    8209
_cell_measurement_temperature    100
_cell_measurement_theta_max      55.804
_cell_measurement_theta_min      2.608
_cell_volume                     4131.5(4)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1539
_diffrn_reflns_av_unetI/netI     0.1323
_diffrn_reflns_Laue_measured_fraction_full 0.946
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44377
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        57.206
_diffrn_reflns_theta_max         57.206
_diffrn_reflns_theta_min         2.055
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.795
_exptl_absorpt_correction_T_max  0.7513
_exptl_absorpt_correction_T_min  0.4368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1321 before and 0.0976 after correction.
The Ratio of minimum to maximum transmission is 0.5814.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_description       needle
_exptl_crystal_F_000             1984
_exptl_crystal_recrystallization_method DCM/Et2O
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.005
_refine_diff_density_max         4.179
_refine_diff_density_min         -2.586
_refine_diff_density_rms         0.305
_refine_ls_extinction_coef       0.00064(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1028
_refine_ls_number_reflns         10612
_refine_ls_number_restraints     702
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.1694
_refine_ls_R_factor_gt           0.1301
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+495.4560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3116
_refine_ls_wR_factor_ref         0.3305
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7457
_reflns_number_total             10612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00226_si_002.cif
_cod_data_source_block           complex_Au1
_cod_database_code               4345795
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.620
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 B1(H1), B2(H2A)
3.b Aromatic/amide H refined with riding coordinates:
 C35(H35), C45(H45), C43(H43), C82(H82), C32(H32), C23(H23), C44(H44),
 C20(H20), C57(H57), C50(H50), C27(H27), C21(H21), C33(H33), C31(H31), C81(H81),
  C63(H63), C70(H70), C54(H54), C38(H38), C36(H36), C12(H12), C2(H2), C72(H72),
 C83(H83), C14(H14), C62(H62), C30(H30), C15(H15), C59(H59), C68(H68), C16(H16),
  C5(H5), C48(H48), C41(H41), C84(H84), C25(H25), C80(H80), C52(H52), C60(H60),
 C56(H56), C61(H61), C8(H8), C24(H24), C78(H78), C39(H39), C18(H18), C71(H71),
 C65(H65), C11(H11), C37(H37), C88(H88), C3(H3), C69(H69), C7(H7), C42(H42),
 C86(H86), C9(H9), C26(H26), C74(H74), C89(H89), C77(H77), C87(H87), C53(H53),
 C17(H17), C29(H29), C51(H51), C90(H90), C66(H66), C6(H6), C47(H47), C75(H75),
 C76(H76)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'