Simple Synthesis of CpNi(NHC)Cl Complexes (Cp = Cyclopentadienyl; NHC = N-Heterocyclic Carbene)
Kelly, Roy A.; Scott, Natalie M.; Díez-González, Silvia; Stevens, Edwin D.; Nolan, Steven P.; Organometallics 24 (2005) 3442–; doi:10.1021/om0501879

data_4075840
_publ_section_title
;
 Simple Synthesis of CpNi(NHC)Cl Complexes (Cp = Cyclopentadienyl; NHC =
 N-Heterocyclic Carbene)
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3442
_journal_paper_doi               10.1021/om0501879
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C26 H31 Cl N2 Ni'
_chemical_formula_weight         465.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.507(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   32.628(4)
_cell_length_b                   8.4750(9)
_cell_length_c                   33.522(4)
_cell_measurement_reflns_used    28904
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      30.921
_cell_measurement_theta_min      2.257
_cell_volume                     9260.7(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            14645
_diffrn_reflns_theta_full        17.50
_diffrn_reflns_theta_max         17.50
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    0.968
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.675400
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3936
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.057
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       0.00005(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         2908
_refine_ls_number_restraints     608
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0915
_refine_ls_shift/su_max          0.167
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+669.0125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2155
_refine_ls_wR_factor_ref         0.2158
_reflns_number_gt                2842
_reflns_number_total             2908
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0501879si20050314_040159.cif
_cod_data_source_block           nol2242m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        9260.6(17)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4075840