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_7124395
_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         'C42 H52 Cu N3 S2'
_chemical_formula_sum            'C42 H52 Cu N3 S2'
_chemical_formula_weight         726.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-08-22
_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                 116.562(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.471(8)
_cell_length_b                   13.794(9)
_cell_length_c                   13.094(8)
_cell_measurement_temperature    200(2)
_cell_volume                     2015(2)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      200.05
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26692
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.082
_diffrn_reflns_theta_min         1.739
_exptl_absorpt_coefficient_mu    0.677
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.463(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         9542
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0405P)^2^+0.0707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0730
_reflns_Friedel_coverage         0.899
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.960
_reflns_number_gt                8728
_reflns_number_total             9542
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07266g2.cif
_cod_data_source_block           ipr-cu-amido
_cod_database_code               7124395
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.935
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.537(9)
 0.463(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C40-C42B \\sim C40-C42A
 with sigma of 0.02
 C40-C41B \\sim C40-C41A
 with sigma of 0.02
 C42A-C40 \\sim C40-C41A
 with sigma of 0.02
 C41B-C40 \\sim C40-C42B
 with sigma of 0.02
4. Rigid body (RIGU) restrains
 C36, C41A, C41B, C40, C42A, C42B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H40A)=Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C42A)=Sof(H42D)=
 Sof(H42E)=Sof(H42F)=1-FVAR(1)
 Sof(H40)=Sof(C42B)=Sof(H42A)=Sof(H42B)=Sof(H42C)=Sof(C41B)=Sof(H41A)=
 Sof(H41B)=Sof(H41C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C25(H25), C37(H37), C40(H40), C40(H40A), C28(H28)
6.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
6.c Aromatic/amide H refined with riding coordinates:
 C35(H35), C3(H3), C18(H18), C17(H17), C33(H33), C34(H34), C10(H10), C21(H21),
 C23(H23), C22(H22), C11(H11), C4(H4), C6(H6), C5(H5), C13(H13), C12(H12)
6.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C1(H1A,H1B,
 H1C), C26(H26A,H26B,H26C), C15(H15A,H15B,H15C), C29(H29A,H29B,H29C), C38(H38A,
 H38B,H38C), C42B(H42A,H42B,H42C), C41B(H41A,H41B,H41C), C41A(H41D,H41E,H41F),
 C42A(H42D,H42E,H42F)
;
_shelx_res_checksum              29367
_olex2_submission_special_instructions 'No special instructions were received'