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_4074165
_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         'C8 H13 I1 N2 Ni1'
_chemical_formula_sum            'C8 H13 I N2 Ni'
_chemical_formula_weight         322.82
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-03-06
_audit_creation_method           CRYSTALS_ver_12.80
_cell_angle_alpha                90
_cell_angle_beta                 103.351(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.2153(19)
_cell_length_b                   8.362(2)
_cell_length_c                   9.324(3)
_cell_measurement_reflns_used    8193
_cell_measurement_temperature    180
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     547.4(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'Nonius (1997-2001). COLLECT.'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.854
_diffrn_measured_fraction_theta_max 0.757
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.086
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1786
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.321
_diffrn_reflns_theta_min         3.313
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.545
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.959
_exptl_crystal_description       plate
_exptl_crystal_F_000             312
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.76
_refine_diff_density_min         -2.08
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.2114
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         960
_refine_ls_number_restraints     100
_refine_ls_R_factor_all          0.1798
_refine_ls_R_factor_gt           0.1451
_refine_ls_shift/su_max          0.000796
_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: 
 3.47 -1.75 1.59 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1286
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1128
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              10
_reflns_limit_k_min              -10
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                960
_reflns_number_total             1470
_reflns_threshold_expression     I>4.00u(I)
_oxford_diffrn_Wilson_B_factor   3.76
_oxford_diffrn_Wilson_scale      3.94
_oxford_refine_ls_scale          0.955(7)
_oxford_structure_analysis_title '7081523 Compound X'
_cod_data_source_file            om060444psi20060519_032000.cif
_cod_data_source_block           compound_4_(js0407b)
_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      'P 1 21/m 1 '
_cod_original_formula_sum        'C8 H13 I1 N2 Ni1'
_cod_database_code               4074165