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_4085412
_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 Br N2 Ni'
_chemical_formula_sum            'C15 H19 Br N2 Ni'
_chemical_formula_weight         365.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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)
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_cell_angle_alpha                90
_cell_angle_beta                 92.4415(15)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.99221(20)
_cell_length_b                   16.0882(2)
_cell_length_c                   15.8008(3)
_cell_measurement_reflns_used    13192
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      30.1230
_cell_measurement_theta_min      3.5990
_cell_volume                     3045.73(9)
_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
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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)
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_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)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_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  -73.00   -1.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.0909  127.0000  162.0860 72

  2 omega  -76.00   -1.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.0909  132.0000 -137.4367 75

  3 omega  -92.00   17.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.0909  -77.0000   90.0000 109

  4 omega  -90.00   -6.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.0909  -38.0000  -30.0000 84

  5 omega  -40.00   58.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.0909   38.0000   30.0000 98

  6 omega  -44.00   60.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.0909   57.0000  120.0000 104

  7 omega  -86.00   17.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.0909  -77.0000 -120.0000 103

  8 omega   26.00   76.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       14.7159 -131.0000   83.1582 50
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_11      -0.0211503000
_diffrn_orient_matrix_UB_12      0.0279507000
_diffrn_orient_matrix_UB_13      -0.0314901000
_diffrn_orient_matrix_UB_21      0.0475993000
_diffrn_orient_matrix_UB_22      -0.0072307000
_diffrn_orient_matrix_UB_23      -0.0241075000
_diffrn_orient_matrix_UB_31      -0.0280872000
_diffrn_orient_matrix_UB_32      -0.0333201000
_diffrn_orient_matrix_UB_33      -0.0211556000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            52519
_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         27.374
_diffrn_reflns_theta_min         3.284
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.886
_exptl_absorpt_correction_T_max  0.886
_exptl_absorpt_correction_T_min  0.464
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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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)
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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       plate
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.282
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         6899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0275
_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^)+(0.0230P)^2^+1.6610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0632
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5551
_reflns_number_total             6899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500939s_si_002.cif
_cod_data_source_block           compound_1b
_cod_depositor_comments
'Adding full bibliography for 4085411--4085414.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4085412
_shelxl_version_number           2014-3