Synthesis, Structure, and Solution Dynamics of Neutral Allylnickel Complexes of N-Heterocyclic Carbenes
Silva, Leonel C.; Gomes, Pedro T.; Veiros, Luis F.; Pascu, Sofia I.; Duarte, M. Teresa; Namorado, Sónia; Ascenso, José R.; Dias, Alberto R.; Organometallics 25 (2006) 4391–; doi:10.1021/om060444p

data_4074164
_publ_section_title
;
 Synthesis, Structure, and Solution Dynamics of Neutral Allylnickel
 Complexes of N-Heterocyclic Carbenes
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4391
_journal_paper_doi               10.1021/om060444p
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C10 H17 Br1 N2 Ni1'
_chemical_formula_sum            'C10 H17 Br N2 Ni'
_chemical_formula_weight         303.87
_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
_audit_creation_date             06-03-07
_audit_creation_method           CRYSTALS_ver_12.82
_cell_angle_alpha                90
_cell_angle_beta                 93.703(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.265(5)
_cell_length_b                   8.471(2)
_cell_length_c                   14.144(4)
_cell_measurement_reflns_used    13420
_cell_measurement_temperature    150
_cell_measurement_theta_max      30
_cell_measurement_theta_min      0
_cell_volume                     2423.0(11)
_computing_cell_refinement
; 
Bruker SAINT version 6.36a (Bruker, 2002)
;
_computing_data_collection
; 
SMART (Siemens, 1993) 
;
_computing_data_reduction
; 
 Bruker SAINT version 6.36a (Bruker, 2002) 
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution
; 
 SHELXS 86 (Sheldrick, 1986) 
;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type
; 
Bruker AXS SMART 1K CCD diffractometer
;
_diffrn_measurement_method       'thin slice \w-scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS Station 9.8'
_diffrn_radiation_type           'synchrotron '
_diffrn_radiation_wavelength     0.6904
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13420
_diffrn_reflns_theta_full        28.344
_diffrn_reflns_theta_max         28.923
_diffrn_reflns_theta_min         1.919
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.865
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS (Siemens, 1996) 
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_description       shard
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.24
_refine_diff_density_min         -0.65
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0257
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2769
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.025204
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.771 0.156 0.584 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0444
_refine_ls_wR_factor_gt          0.0434
_refine_ls_wR_factor_ref         0.0434
_reflns_limit_h_max              28
_reflns_limit_h_min              -28
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                2769
_reflns_number_total             3558
_reflns_threshold_expression     I>3.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.1765(4)
_cod_data_source_file            om060444psi20060519_032000.cif
_cod_data_source_block           compound_2_(cam205)
_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_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        'C10 H17 Br1 N2 Ni1'
_cod_database_code               4074164