Synthesis, Structure, and Solution Dynamic Behavior of Nickel Complexes Bearing a 1,3-Diallyl-Substituted NHC Ligand
Włodarska, Agata; Kozioł, Andrzej; Dranka, Maciej; Gryff-Keller, Adam; Szczeciński, Przemysław; Jurkowski, Jakub; Pietrzykowski, Antoni; Organometallics 34 (2015) 577–; doi:10.1021/om500939s

data_4085413
_publ_section_title
;
 Synthesis, Structure, and Solution Dynamic Behavior of Nickel Complexes
 Bearing a 1,3-Diallyl-Substituted NHC Ligand
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              577
_journal_paper_doi               10.1021/om500939s
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C14 H17 Cl N2 Ni'
_chemical_formula_sum            'C14 H17 Cl N2 Ni'
_chemical_formula_weight         307.45
_chemical_properties_physical    air-sensitive
_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_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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     direct
_audit_creation_date             2014-08-03
_audit_creation_method
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Olex2 1.2-beta
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.532(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7100(3)
_cell_length_b                   15.5306(3)
_cell_length_c                   9.8555(2)
_cell_measurement_reflns_used    12439
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      25.7530
_cell_measurement_theta_min      3.7380
_cell_volume                     1456.23(6)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      120.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3347
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -77.00    3.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3435  125.0000  173.6332 80

  2 omega  -87.00  -25.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3435  142.0000   33.1800 62

  3 omega  -98.00   14.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3435  -77.0000   60.0000 112

  4 omega  -93.00   10.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3435  -57.0000 -180.0000 103

  5 omega  -94.00    7.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3435  -38.0000  -90.0000 101

  6 omega  -45.00   57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3435   38.0000  -30.0000 102

  7 omega  -70.00  -34.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3435 -179.0000   60.0000 36

  8 omega  -47.00   51.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3435   57.0000   60.0000 98

  9 omega   34.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1248 -130.0000   50.6483 47

 10 omega -109.00  -34.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3435 -179.0000  -60.0000 75

 11 omega  -95.00    7.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3435  -38.0000   30.0000 102

 12 omega -108.00  -32.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3435  179.0000   30.0000 76

 13 omega  -93.00   10.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3435  -57.0000  -60.0000 103

 14 omega  -56.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1248  -38.0000  -60.0000 103

 15 omega   22.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1248 -130.0000   50.6483 59

 16 omega   -6.00   96.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1248   38.0000  -90.0000 102

 17 omega  -98.00   14.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3435  -77.0000  150.0000 112

 18 omega  -46.00   57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3435   38.0000 -180.0000 103

 19 omega -109.00  -70.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3435 -179.0000  -30.0000 39

 20 omega   -4.00   62.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1248  -99.0000  -90.0000 66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini A Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0261632000
_diffrn_orient_matrix_UB_12      0.0265661000
_diffrn_orient_matrix_UB_13      0.0476685000
_diffrn_orient_matrix_UB_21      0.0414267000
_diffrn_orient_matrix_UB_22      0.0347064000
_diffrn_orient_matrix_UB_23      -0.0160559000
_diffrn_orient_matrix_UB_31      -0.0561731000
_diffrn_orient_matrix_UB_32      0.0132395000
_diffrn_orient_matrix_UB_33      -0.0535587000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            57136
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.372
_diffrn_reflns_theta_min         3.367
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.499
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       needle
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.3887
_exptl_crystal_size_mid          0.1896
_exptl_crystal_size_min          0.0853
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3297
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+0.4540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0695
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2620
_reflns_number_total             3297
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500939s_si_002.cif
_cod_data_source_block           compound_2
_cod_depositor_comments
'Adding full bibliography for 4085411--4085414.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4085413
_shelxl_version_number           2014-3