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_7057727
_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         'C42 H43 Co0.97 O P5, 2(C4 H8 O)'
_chemical_formula_sum            'C50 H62 Co O3 P5'
_chemical_formula_weight         924.77
_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     dual
_audit_creation_date             2017-07-10
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.06 svn.r2239, GUI svn.r4109)
;
_audit_update_record
;
2017-07-10 deposited with the CCDC.
2018-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                98.822(2)
_cell_angle_beta                 103.269(3)
_cell_angle_gamma                106.982(3)
_cell_formula_units_Z            2
_cell_length_a                   11.4187(4)
_cell_length_b                   11.7446(4)
_cell_length_c                   18.9017(4)
_cell_measurement_reflns_used    9496
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.5150
_cell_measurement_theta_min      4.2280
_cell_volume                     2292.52(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.22a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.22a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.22a (Rigaku OD, 2015)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.9938
_diffrn_measured_fraction_theta_max 0.9622
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -15.00  12.00   0.50    0.50    --    0.00  37.00   0.00   54
  2  \w    -20.00  17.00   0.50    0.50    --    0.00 -37.00 120.00   74
  3  \w    -88.00 -39.00   0.50    0.50    --    0.00 -37.00 120.00   98
  4  \w     59.00  86.00   0.50    0.50    --    0.00  37.00   0.00   54
  5  \w    140.00 167.00   0.50    6.00    --   94.60  45.00 120.00   54
  6  \w      6.00  31.00   0.50    6.00    --   94.60 -15.00   0.00   50
  7  \w     51.00  78.00   0.50    6.00    --   94.60 -30.00   0.00   54
  8  \w     10.00  37.00   0.50    6.00    --   94.60 -30.00   0.00   54
  9  \w     72.00 100.00   0.50    6.00    --   94.60 -15.00   0.00   56
 10  \w     76.00 121.00   0.50    6.00    --   94.60  45.00 120.00   90
 11  \w     78.00 183.00   0.50    6.00    --   94.60  30.00 -30.00  210
 12  \w     23.00  90.00   0.50    6.00    --   94.60 -77.00  60.00  134
 13  \w    -80.00 -54.00   0.50    0.50    --    0.00 -57.00-120.00   52
 14  \w    -17.00   8.00   0.50    0.50    --    0.00 -19.00  90.00   50
 15  \w    -49.00 -11.00   0.50    0.50    --    0.00 -57.00-120.00   76
 16  \w    -88.00 -59.00   0.50    0.50    --    0.00 -37.00 -60.00   58
 17  \w    -50.00  13.00   0.50    0.50    --    0.00 -37.00   0.00  126
 18  \w     44.00  71.00   0.50    5.00    --   94.60 -82.00  30.00   54
 19  \w     25.00 126.00   0.50    5.00    --   94.60 -82.00 150.00  202
 20  \w    112.00 138.00   0.50    5.00    --   94.60   0.00 -30.00   52
 21  \w     67.00 125.00   0.50    5.00    --   94.60 -82.00   0.00  116
 22  \w      5.00  94.00   0.50    5.00    --   94.60 -61.00 150.00  178
 23  \w     15.00 125.00   0.50    5.00    --   94.60 -82.00-120.00  220
 24  \w      6.00  38.00   0.50    5.00    --   94.60 -15.00 -30.00   64
 25  \w     59.00 103.00   0.50    5.00    --   94.60 -15.00 -30.00   88
 26  \w     84.00 125.00   0.50    5.00    --   94.60 -82.00 -60.00   82
 27  \w     79.00 105.00   0.50    5.00    --   94.60 -82.00  90.00   52
 28  \w     10.00 118.00   0.50    5.00    --   94.60 -61.00-120.00  216
 29  \w     81.00 123.00   0.50    5.00    --   94.60 -82.00  30.00   84
 30  \w    159.00 184.00   0.50    5.00    --   94.60   0.00 -30.00   50
 31  \w      5.00  52.00   0.50    5.00    --   94.60 -30.00 -90.00   94
 32  \w     59.00 102.00   0.50    5.00    --   94.60 -30.00 -90.00   86
 33  \w     77.00 102.00   0.50    5.00    --   94.60   0.00 -30.00   50
 34  \w     21.00  61.00   0.50    5.00    --   94.60   0.00 -30.00   80
 35  \w     64.00  89.00   0.50    0.50    --    0.00   0.00 -90.00   50
 36  \w     -7.00  18.00   0.50    0.50    --    0.00 -19.00  30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0041116000
_diffrn_orient_matrix_UB_12      0.1166832000
_diffrn_orient_matrix_UB_13      -0.0266849000
_diffrn_orient_matrix_UB_21      0.0642204000
_diffrn_orient_matrix_UB_22      0.0769626000
_diffrn_orient_matrix_UB_23      0.0810331000
_diffrn_orient_matrix_UB_31      0.1326254000
_diffrn_orient_matrix_UB_32      0.0197420000
_diffrn_orient_matrix_UB_33      -0.0122593000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23807
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        66.598
_diffrn_reflns_theta_max         66.598
_diffrn_reflns_theta_min         4.217
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.907
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.22a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull dark red'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.577
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         7949
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0651
_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^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1618
_refine_ls_wR_factor_ref         0.1689
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6705
_reflns_number_total             7949
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj03919d2.cif
_cod_data_source_block           20170704-15
_cod_depositor_comments
'Adding full bibliography for 7057725--7057727.cif.'
_cod_original_cell_volume        2292.52(12)
_cod_database_code               7057727
_reflns_odcompleteness_completeness 99.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C43(H43A,H43B), C45(H45A,H45B), C48(H48A,H48B), C47(H47A,
 H47B), C46(H46A,H46B), C49(H49A,H49B), C50(H50A,H50B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C32(H32), C23(H23), C20(H20), C15(H15), C18(H18),
 C11(H11), C36(H36), C33(H33), C5(H5), C22(H22), C21(H21), C35(H35), C10(H10),
 C26(H26), C12(H12), C16(H16), C4(H4), C30(H30), C34(H34), C27(H27), C17(H17),
 C8(H8), C29(H29), C28(H28), C9(H9)
2.c Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C40(H40A,H40B,H40C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.531
_oxdiff_exptl_absorpt_empirical_full_min 0.427
_shelx_shelxl_version_number     2014/7