Cu(i)-SNS complexes for outer-sphere hydroboration and hydrosilylation of carbonyls.
Elsby, Matthew R.; Baker, R. Tom; Chemical communications (Cambridge, England)  (2019) –; doi:10.1039/c9cc07266g

data_7124396
_publ_section_title
;
 Cu(i)-SNS complexes for outer-sphere hydroboration and hydrosilylation of
 carbonyls.
;
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/c9cc07266g
_journal_year                    2019
_chemical_formula_moiety         'C41 H48 Cu N3 S2'
_chemical_formula_sum            'C41 H48 Cu N3 S2'
_chemical_formula_weight         710.48
_chemical_name_systematic        C41H48CuN3S2
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-09 deposited with the CCDC.    2019-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.175(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.955(3)
_cell_length_b                   15.654(3)
_cell_length_c                   19.260(4)
_cell_measurement_reflns_used    7969
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.88
_cell_measurement_theta_min      2.49
_cell_volume                     3890.0(14)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      298.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_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  0.0405
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36950
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.649
_diffrn_reflns_theta_min         1.679
_exptl_absorpt_coefficient_mu    0.700
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0520 before and 0.0436 after correction. The Ratio of minimum to maximum transmission is 0.9058. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.382
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.179
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         8089
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0539P)^2^+1.0339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1161
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5413
_reflns_number_total             8089
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07266g2.cif
_cod_data_source_block           me_k0458_0m
_cod_original_cell_volume        3889.8(15)
_cod_database_code               7124396
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.776
_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.a Ternary CH refined with riding coordinates:
 C39(H39), C24(H24), C36(H36), C27(H27)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C16(H16), C7(H7), C5(H5), C12(H12), C20(H20), C2(H2), C9(H9),
 C34(H34), C32(H32), C10(H10), C11(H11), C22(H22), C4(H4), C33(H33), C3(H3),
 C21(H21)
2.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C28(H28A,H28B,H28C), C38(H38A,H38B,H38C), C25(H25A,H25B,
 H25C), C41(H41A,H41B,H41C), C29(H29A,H29B,H29C), C37(H37A,H37B,H37C), C26(H26A,
 H26B,H26C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              79735
_olex2_submission_special_instructions 'No special instructions were received'