Half-sandwich Ni(II) complexes bearing enantiopure bidentate NHC-carboxylate ligands: efficient catalysts for the hydrosilylative reduction of acetophenones.
Sanz-Garrido, Jorge; Martin, Avelino; González-Arellano, Camino; Flores, Juan C.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 1460–1468; doi:10.1039/d3dt03739h

data_7714731
_publ_section_title
;
 Half-sandwich Ni(II) complexes bearing enantiopure bidentate
 NHC-carboxylate ligands: efficient catalysts for the hydrosilylative
 reduction of acetophenones.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1460
_journal_page_last               1468
_journal_paper_doi               10.1039/d3dt03739h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C25 H24 N2 Ni O2'
_chemical_formula_sum            'C25 H24 N2 Ni O2'
_chemical_formula_weight         443.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-22
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-23 deposited with the CCDC.	2023-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.807(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3904(10)
_cell_length_b                   11.4363(9)
_cell_length_c                   16.0226(11)
_cell_measurement_reflns_used    7863
_cell_measurement_temperature    200.00
_cell_measurement_theta_max      27.470
_cell_measurement_theta_min      2.571
_cell_volume                     2184.6(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Apex3 v2019.11-0 (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200.00
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type
;
Bruker AXS D8 Venture diffractometer with PhotonIII_C14 charge-integrating and 
photon counting pixel array detector
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1328
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            48749
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         3.258
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.911
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1278 before and 0.0797 after correction.
The Ratio of minimum to maximum transmission is 0.8378.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.044
_refine_diff_density_max         1.692
_refine_diff_density_min         -0.943
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         3855
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0788
_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^)+(0.0582P)^2^+7.7195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1667
_refine_ls_wR_factor_ref         0.1739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3231
_reflns_number_total             3855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03739h2.cif
_cod_data_source_block           pgsphgni_0m_a
_cod_depositor_comments
'Adding full bibliography for 7714726--7714736.cif.'
_cod_database_code               7714731
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.833
_olex2_refinement_description
;
1. 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
2. Uiso/Uaniso restraints and constraints
C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 1.7A
C31 \\sim C36 \\sim C35 \\sim C34 \\sim C33 \\sim C32: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C31) \\sim Ueq, Uanis(C32A) \\sim Ueq, Uanis(C33A) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C35A) \\sim Ueq, Uanis(C36A) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24)
\\sim Ueq, Uanis(C25) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
3. Rigid body (RIGU) restrains
 C31, C34, C32, C33, C35, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C31, C34, C32A, C33A, C35A, C36A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H34A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C35A)=Sof(H35A)=
 Sof(C36A)=Sof(H36A)=1-FVAR(1)
 Sof(H34)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C35)=Sof(H35)=Sof(C36)=
 Sof(H36)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C5(H5)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C8(H8), C10(H10), C21(H21), C22(H22), C23(H23), C24(H24),
 C25(H25), C34(H34), C34(H34A), C32(H32), C33(H33), C35(H35), C36(H36),
 C32A(H32A), C33A(H33A), C35A(H35A), C36A(H36A)
5.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              73802
_shelx_hkl_checksum              19641
_olex2_submission_special_instructions 'No special instructions were received'