Oxygen-Induced Ligand Dehydrogenation of a Planar Bis-μ-Chloronickel(I) Dimer Featuring an NHC Ligand
Benjamin R. Dible; Matthew S. Sigman; Atta M. Arif; Inorganic Chemistry 44 (2005) 3774–3776; doi:10.1021/ic050445u

data_4308944
_publ_contact_author_address
;Department of Chemistry
University of Utah
315 South 1400 East
Salt Lake City, Utah 84112-8500
;
_publ_contact_author_email       sigman@chem.utah.edu
_publ_contact_author_name        'Matthew S. Sigman'
_publ_contact_author_phone       801-585-0774
_publ_section_title
;
Oxygen-Induced Ligand Dehydrogenation of a Planar Bis-\m-Chloronickel(I)
Dimer Featuring an NHC Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3774
_journal_page_last               3776
_journal_paper_doi               10.1021/ic050445u
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C54 H72 Cl2 N4 Ni2'
_chemical_formula_weight         965.48
_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                 94.4164(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.2379(3)
_cell_length_b                   15.2877(3)
_cell_length_c                   18.8278(4)
_cell_measurement_reflns_used    11247
_cell_measurement_temperature    150(1)
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_cell_measurement_theta_min      1.018
_cell_volume                     5233.90(17)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'WinGX, Ortep3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method       'Phi plus Omega scan'
_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  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0905
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21301
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  0.9345
_exptl_absorpt_correction_T_min  0.7826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.0026(3)
_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   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     826
_refine_ls_number_reflns         11935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0483P)^2^+1.3902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1339
_reflns_number_gt                7772
_reflns_number_total             11935
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050445usi20050420_115959_2.cif
_cod_data_source_block           mss012
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4308944