Group-Transfer Reactions of Ni(II)−Ni(II) Bridging Imido Complexes. Catalytic Formation of Carbodiimides and Isocyanates via Nitrene Transfer from Organoazides
Laskowski, Carl A.; Hillhouse, Gregory L.; Organometallics 28 (2009) 6114–; doi:10.1021/om900783u

data_4070395
_publ_section_title
;
 Group-Transfer Reactions of Ni(II)&#x2212;Ni(II) Bridging Imido
 Complexes. Catalytic Formation of Carbodiimides and Isocyanates via
 Nitrene Transfer from Organoazides
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              6114
_journal_paper_doi               10.1021/om900783u
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C95 H95 B Cl F24 N5 Ni2'
_chemical_formula_weight         1926.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.122(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.107(3)
_cell_length_b                   12.354(2)
_cell_length_c                   41.418(7)
_cell_measurement_temperature    100(2)
_cell_volume                     9121(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w 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  0.1698
_diffrn_reflns_av_sigmaI/netI    0.1583
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            46463
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_T_max  0.3356
_exptl_absorpt_correction_T_min  0.1918
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'Norton et. al.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3976
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.364
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1172
_refine_ls_number_reflns         16047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0724
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.1687
_reflns_number_gt                9717
_reflns_number_total             16047
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900783u_si_002.cif
_cod_data_source_block           4
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        9120(3)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4070395