Tuning the redox non-innocence of a phenalenyl ligand toward efficient nickel-assisted catalytic hydrosilylation.
Vijaykumar, Gonela; Pariyar, Anand; Ahmed, Jasimuddin; Shaw, Bikash Kumar; Adhikari, Debashis; Mandal, Swadhin K.; Chemical science 9 (2018) 2817–2825; doi:10.1039/c7sc04687a

data_1548839
_publ_section_title
;
 Tuning the redox non-innocence of a phenalenyl ligand toward efficient
 nickel-assisted catalytic hydrosilylation.
;
_journal_issue                   10
_journal_name_full               'Chemical science'
_journal_page_first              2817
_journal_page_last               2825
_journal_paper_doi               10.1039/c7sc04687a
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C17 H15 Ni0.5 O3, C4 H8 O'
_chemical_formula_sum            'C21 H23 Ni0.5 O4'
_chemical_formula_weight         368.75
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-11-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2016-11-20 deposited with the CCDC.
2018-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.542(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6006(9)
_cell_length_b                   15.4568(16)
_cell_length_c                   11.7534(11)
_cell_measurement_reflns_used    3236
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0190
_cell_measurement_theta_min      4.1660
_cell_volume                     1740.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9160
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -36.00    1.00   1.0000    4.8700
omega____ theta____ kappa____ phi______ frames
    -      -18.1632   38.0000   60.0000 37

  2 omega   31.00   88.00   1.0000    4.8700
omega____ theta____ kappa____ phi______ frames
    -       20.0382   57.0000   90.0000 57

  3 omega   -2.00   91.00   1.0000    4.8700
omega____ theta____ kappa____ phi______ frames
    -       20.0382   38.0000 -120.0000 93

  4 omega   64.00   90.00   1.0000    4.8700
omega____ theta____ kappa____ phi______ frames
    -       20.0382  178.0000 -150.0000 26

  5 omega  -19.00   21.00   1.0000    4.8700
omega____ theta____ kappa____ phi______ frames
    -      -18.1632  -99.0000 -180.0000 40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0278676000
_diffrn_orient_matrix_UB_12      -0.0424969000
_diffrn_orient_matrix_UB_13      -0.0008227000
_diffrn_orient_matrix_UB_21      -0.0681927000
_diffrn_orient_matrix_UB_22      0.0171970000
_diffrn_orient_matrix_UB_23      -0.0099054000
_diffrn_orient_matrix_UB_31      0.0070909000
_diffrn_orient_matrix_UB_32      -0.0023001000
_diffrn_orient_matrix_UB_33      -0.0596352000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6724
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1575
_refine_ls_wR_factor_ref         0.1734
_reflns_number_gt                2478
_reflns_number_total             3066
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7sc04687a2.cif
_cod_data_source_block           skm_ap_niply
_cod_depositor_comments          'Adding full bibliography for 1548839.cif.'
_cod_original_formula_sum        'C21 H23 Ni0.50 O4'
_cod_database_code               1548839
_chemical_oxdiff_formula         C26H14O4Ni
_reflns_odcompleteness_completeness 86.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C10(H10A,H10B), C12(H12A,H12B), C16(H16A,H16B), C13(H13A,
 H13B), C17(H17A,H17B), C14(H14A,H14B), C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C3(H3), C4(H4), C7(H7), C6(H6), C8(H8)
;
_olex2_date_sample_data_collection 2014-03-14
_olex2_submission_special_instructions 'No special instructions were received'