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_4345794
_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 H55 B1 Cu1 N6 P1 S3'
_chemical_formula_sum            'C45 H55 B Cu N6 P S3'
_chemical_formula_weight         881.45
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2016-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.7346(3)
_cell_length_b                   14.7346(3)
_cell_length_c                   12.1853(3)
_cell_measurement_reflns_used    9785
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.29
_cell_measurement_theta_min      3.46
_cell_volume                     2291.10(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'XS (Sheldrick, 2008)'
_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 0.987
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            38048
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.978
_diffrn_reflns_theta_min         3.463
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.568
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.6051
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1081 before and 0.0717 after correction.
The Ratio of minimum to maximum transmission is 0.8036.
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    1.278
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_recrystallization_method DCM/Hex/Et2O
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.274
_refine_diff_density_min         -2.114
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         2736
_refine_ls_number_restraints     222
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0948
_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^)+(0.1280P)^2^+19.3100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2604
_refine_ls_wR_factor_ref         0.2678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2406
_reflns_number_total             2736
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00226_si_002.cif
_cod_data_source_block           complex_Cu2
_cod_original_cell_volume        2291.10(10)
_cod_database_code               4345794
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.861
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
2. Restrained distances
 C15A-C10A
 1.53 with sigma of 0.02
 C11A-C10A
 1.53 with sigma of 0.02
 C14A-C13A
 1.53 with sigma of 0.02
 C12A-C13A
 1.53 with sigma of 0.02
 C11A-C12A
 1.53 with sigma of 0.02
 C15A-C14A
 1.53 with sigma of 0.02
 C15-C14 = C14-C13 = C15-C10 = C11-C10 = C12-C11 = C12-C13
 1.53 with sigma of 0.02
3. 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
Uanis(C11A) = Uanis(C10A) = Uanis(C15A) = Uanis(C14A) = Uanis(C13A) =
Uanis(C12A)
4. Others
 Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C15A)=
 Sof(H15C)=Sof(H15D)=Sof(C14A)=Sof(H14C)=Sof(H14D)=Sof(C10A)=Sof(H10A)=
 Sof(C13A)=Sof(H13C)=Sof(H13D)=1-FVAR(1)
 Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C13)=Sof(H13A)=Sof(H13B)=
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C14)=Sof(H14A)=
 Sof(H14B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 B1(H1), C10(H10), C10A(H10A)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C12(H12A,H12B), C15(H15A,H15B), C14(H14A,
 H14B), C11A(H11C,H11D), C12A(H12C,H12D), C15A(H15C,H15D), C14A(H14C,H14D),
 C13A(H13C,H13D)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C9(H9), C8(H8), C5(H5), C6(H6), C7(H7)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'