Synthesis and catalytic application of [PPP]-pincer iron, nickel and cobalt complexes for the hydrosilylation of aldehydes and ketones
Qi, Xinghao; Zhao, Hua; Sun, Hongjian; Li, Xiaoyan; Fuhr, Olaf; Fenske, Dieter; New Journal of Chemistry 42 (2018) 16583–; doi:10.1039/C8NJ03919D

data_7057725
_publ_section_title
;
 Synthesis and catalytic application of [PPP]-pincer iron, nickel and
 cobalt complexes for the hydrosilylation of aldehydes and ketones
;
_journal_issue                   20
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16583
_journal_paper_doi               10.1039/C8NJ03919D
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C39 H38 Ni P4'
_chemical_formula_sum            'C39 H38 Ni P4'
_chemical_formula_weight         689.28
_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     direct
_audit_creation_date             2014-08-28
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2015-05-12 deposited with the CCDC.
2018-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                110.387(3)
_cell_angle_beta                 99.425(3)
_cell_angle_gamma                97.279(3)
_cell_formula_units_Z            4
_cell_length_a                   11.6219(5)
_cell_length_b                   15.7590(6)
_cell_length_c                   20.5250(8)
_cell_measurement_temperature    180.15
_cell_volume                     3406.8(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.15
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0709
_diffrn_reflns_Laue_measured_fraction_full 0.945
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25600
_diffrn_reflns_point_group_measured_fraction_full 0.945
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.667
_diffrn_reflns_theta_min         2.172
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_target            Mo
_diffrn_source_type              'sealed X-ray tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_T_max  0.9528
_exptl_absorpt_correction_T_min  0.7268
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       plate
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.006
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.00161(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.890
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     800
_refine_ls_number_reflns         12667
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.890
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0357P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0746
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8482
_reflns_number_total             12667
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj03919d2.cif
_cod_data_source_block           2014sun-07
_cod_depositor_comments
'Adding full bibliography for 7057725--7057727.cif.'
_cod_original_cell_volume        3406.8(2)
_cod_database_code               7057725
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All P(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 P2(H2P), P6(H6P)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
  C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C41(H41), C42(H42), C43(H43), C44(H44),
  C45(H45), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C54(H54),
 C55(H55), C56(H56), C57(H57), C60(H60), C61(H61), C62(H62), C63(H63), C65(H65),
  C66(H66), C67(H67), C68(H68), C69(H69), C71(H71), C72(H72), C73(H73),
 C74(H74), C75(H75)
2.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C76(H76A,H76B,
 H76C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C)
;
_shelx_res_checksum              81303
_olex2_submission_special_instructions 'No special instructions were received'