β-Diketiminato Nickel Imides in Catalytic Nitrene Transfer to Isocyanides
Wiese, Stefan; Aguila, Mae Joanne B.; Kogut, Elzbieta; Warren, Timothy H.; Organometallics 32 (2013) 2300–; doi:10.1021/om300909n

data_4080171
_publ_contact_author             'Timothy H. Warren'
_publ_section_title
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 \b-Diketiminato Nickel Imides in Catalytic Nitrene Transfer to
 Isocyanides
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_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2300
_journal_paper_doi               10.1021/om300909n
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C24 H29 N2 Ni O'
_chemical_formula_weight         420.20
_chemical_name_common            {[Me3NN]Ni}2(m-CO)2
_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                 108.48(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.103(15)
_cell_length_b                   8.942(9)
_cell_length_c                   22.82(2)
_cell_measurement_reflns_used    919
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.699
_cell_measurement_theta_min      2.475
_cell_volume                     4278(6)
_computing_cell_refinement       'Bruker APEXII'
_computing_data_collection       'Bruker APEXII'
_computing_data_reduction        'Bruker APEXII'
_computing_molecular_graphics
'XSEED for Windows with POV-Ray; Barbour L (1999)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0850
_diffrn_reflns_av_sigmaI/netI    0.0781
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            21248
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_T_max  0.8020
_exptl_absorpt_correction_T_min  0.7692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS based on Blessing's method; Blessing, Acta Cryst. (1995) A51 33-38'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.0010(2)
_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   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4423
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0758P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1355
_reflns_number_gt                2656
_reflns_number_total             4423
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300909n_si_002.cif
_cod_data_source_block           cmpd_7
_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 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        4277(6)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4080171