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_4085411
_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         'C15 H19 N2 Ni, Br'
_chemical_formula_sum            'C15 H19 Br N2 Ni'
_chemical_formula_weight         365.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-08-19
_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                 90.642(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.26228(16)
_cell_length_b                   12.0198(3)
_cell_length_c                   16.8199(4)
_cell_measurement_reflns_used    12978
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      32.0360
_cell_measurement_theta_min      3.9690
_cell_volume                     1468.14(6)
_computing_cell_refinement
;
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
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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_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      120.0
_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  -84.00  -34.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4946 -179.0000 -180.0000 50

  2 omega   70.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2759  179.0000   90.0000 39

  3 omega   14.00   50.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2759  -57.0000   30.0000 36

  4 omega  -50.00   20.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2759  -19.0000  -30.0000 70

  5 omega  -95.00  -29.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4946  -38.0000  -60.0000 66

  6 omega  -19.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3384   19.0000   90.0000 66

  7 omega  -49.00  -22.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3384   19.0000   90.0000 27

  8 omega   -1.00   96.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1196   77.0000   90.0000 97

  9 omega   56.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1196  179.0000  -90.0000 50

 10 omega  -14.00   35.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1196   77.0000  -60.0000 49

 11 omega  -93.00   10.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3384  -57.0000   30.0000 103

 12 omega  -98.00   14.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3384  -77.0000  150.0000 112

 13 omega  -93.00   10.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3384  -57.0000 -150.0000 103

 14 omega  -49.00   23.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3384   57.0000   90.0000 72

 15 omega    4.00   67.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1196 -108.0000  -36.0000 63

 16 omega   -4.00   62.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1196  -99.0000  120.0000 66

 17 omega  -56.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1196  -38.0000 -180.0000 103
;
_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      -0.0158713000
_diffrn_orient_matrix_UB_12      -0.0146817000
_diffrn_orient_matrix_UB_13      0.0401945000
_diffrn_orient_matrix_UB_21      -0.0232663000
_diffrn_orient_matrix_UB_22      0.0560037000
_diffrn_orient_matrix_UB_23      0.0086210000
_diffrn_orient_matrix_UB_31      -0.0935079000
_diffrn_orient_matrix_UB_32      -0.0114397000
_diffrn_orient_matrix_UB_33      -0.0094336000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38180
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.370
_diffrn_reflns_theta_min         3.278
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.031
_exptl_absorpt_correction_T_max  0.641
_exptl_absorpt_correction_T_min  0.354
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_description       needle
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.4213
_exptl_crystal_size_mid          0.1604
_exptl_crystal_size_min          0.153
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.450(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         6672
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0270P)^2^+1.3280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0649
_reflns_Friedel_coverage         0.909
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6298
_reflns_number_total             6672
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500939s_si_002.cif
_cod_data_source_block           compound_1a
_cod_depositor_comments
'Adding full bibliography for 4085411--4085414.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4085411
_shelxl_version_number           2014-3