RigidN-Phosphino Guanidine P,N Ligands and Their Use in Nickel-Catalyzed Ethylene Oligomerization
Dyer, Philip W.; Fawcett, John; Hanton, Martin J.; Organometallics 27 (2008) 5082–; doi:10.1021/om8005933

data_4072108
_publ_section_title
;
 RigidN-Phosphino Guanidine P,N Ligands and Their Use in Nickel-Catalyzed
 Ethylene Oligomerization
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5082
_journal_paper_doi               10.1021/om8005933
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C19 H22 Br2 N3 Ni P, 0.5(C D2 Cl2)'
_chemical_formula_sum            'C19.5 H22 Br2 Cl D N3 Ni P'
_chemical_formula_weight         585.37
_chemical_name_systematic
; 
 Diphenyl 1,5,7-triazabicyclo[4.4.0]dec-5-ene phosphine nickel 
 dibromide 
;
_chemical_temperature_decomposition_gt 240
_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                 127.2440(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.4597(15)
_cell_length_b                   13.0822(8)
_cell_length_c                   17.0457(11)
_cell_measurement_reflns_used    9035
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.165
_cell_measurement_theta_min      2.405
_cell_volume                     4342.1(5)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16335
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    4.782
_exptl_absorpt_correction_T_max  0.65
_exptl_absorpt_correction_T_min  0.33
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 11008 reflections corrected using SADABS. R(int) = 0.1122 before correction. 
 R(int) = 0.0272 after correction. 
;
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.331
_refine_diff_density_min         -1.316
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         4264
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0710P)^2^+0.4016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1002
_reflns_number_gt                3691
_reflns_number_total             4264
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8005933_si_001.cif
_cod_data_source_block           4a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition_gt' since the value was
specified 'more than' ('>') a certain temperature. The value '> 240
dec.' was changed to '240' - it should be numeric and without a unit
designator.

'_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      C2/c
_cod_original_formula_sum        'C19.50 H22 Br2 Cl D N3 Ni P'
_cod_database_code               4072108