An abnormal N-heterocyclic carbene based nickel complex for catalytic reduction of nitroarenes.
Vijaykumar, Gonela; Mandal, Swadhin K.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 7421–7426; doi:10.1039/c6dt00470a

data_7038779
_publ_section_title
;
 An abnormal N-heterocyclic carbene based nickel complex for catalytic
 reduction of nitroarenes.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7421
_journal_page_last               7426
_journal_paper_doi               10.1039/c6dt00470a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C39 H44 Cl N2 Ni0.5'
_chemical_formula_sum            'C39 H44 Cl N2 Ni0.5'
_chemical_formula_weight         605.57
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-12-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-02-01 deposited with the CCDC.
2016-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                66.945(4)
_cell_angle_beta                 85.853(4)
_cell_angle_gamma                71.589(4)
_cell_formula_units_Z            2
_cell_length_a                   11.4154(6)
_cell_length_b                   12.6234(5)
_cell_length_c                   15.3280(8)
_cell_measurement_reflns_used    7420
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      27.8310
_cell_measurement_theta_min      2.1870
_cell_volume                     1925.00(18)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega   -7.00   81.00   1.0000   16.6000
omega____ theta____ kappa____ phi______ frames
    -       27.5074   57.0000  -30.0000 88

  2 omega   65.00  104.00   1.0000   16.6000
omega____ theta____ kappa____ phi______ frames
    -       27.5074   57.0000 -150.0000 39

  3 omega   37.00  121.00   1.0000   16.6000
omega____ theta____ kappa____ phi______ frames
    -       27.5074  178.0000  120.0000 84

  4 omega   67.00   93.00   1.0000   16.6000
omega____ theta____ kappa____ phi______ frames
    -       27.5074   38.0000  120.0000 26

  5 omega  -44.00   62.00   1.0000   16.6000
omega____ theta____ kappa____ phi______ frames
    -       27.5074  -77.0000   90.0000 106

  6 omega  -49.00   69.00   1.0000   16.6000
omega____ theta____ kappa____ phi______ frames
    -       27.5074  -77.0000 -180.0000 118
;
_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      0.0477007000
_diffrn_orient_matrix_UB_12      0.0047442000
_diffrn_orient_matrix_UB_13      -0.0322631000
_diffrn_orient_matrix_UB_21      -0.0368279000
_diffrn_orient_matrix_UB_22      -0.0030529000
_diffrn_orient_matrix_UB_23      -0.0337477000
_diffrn_orient_matrix_UB_31      -0.0259198000
_diffrn_orient_matrix_UB_32      0.0640559000
_diffrn_orient_matrix_UB_33      -0.0189274000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13758
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.85
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.361
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74755
_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 reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.045
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             646
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         8387
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+0.5281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1204
_reflns_number_gt                7097
_reflns_number_total             8387
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt00470a2.cif
_cod_data_source_block           gbnicl2b
_cod_depositor_comments          'Adding full bibliography for 7038779.cif.'
_cod_original_cell_volume        1925.00(15)
_cod_original_formula_sum        'C39 H44 Cl N2 Ni0.50'
_cod_database_code               7038779
_chemical_oxdiff_formula         'C H N Cl Ni'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C13(H13), C37(H37), C34(H34), C10(H10)
2.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C6(H6), C17(H17), C23(H23), C26(H26), C25(H25), C24(H24), C32(H32),
 C31(H31), C30(H30), C20(H20), C8(H8), C7(H7), C18(H18), C21(H21), C19(H19)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C39(H39A,H39B,H39C), C15(H15A,H15B,H15C), C35(H35A,H35B,
 H35C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C38(H38A,H38B,H38C), C36(H36A,
 H36B,H36C)
;
_olex2_date_sample_data_collection 2014-10-25
_olex2_submission_special_instructions 'No special instructions were received'