Structural, Spectroscopic, and Electrochemical Studies of the Complexes [Ni2(μ-CNR)(CNR)2(μ-dppm)2]n+ (n= 0, 1, 2): Unusual Examples of Nickel(0)-Nickel(I) and Nickel(0)-Nickel(II) Mixed Valency
Gregory M. Ferrence; Eugenio Simón-Manso; Brian K. Breedlove; Leah Meeuwenberg; Clifford P. Kubiak; Inorganic Chemistry 43 (2004) 1071–1081; doi:10.1021/ic035021j

data_4310545
_publ_section_title
;
 Structural, Spectroscopic, and Electrochemical Studies of the Complexes
 [Ni2(\m-CNR)(CNR)2(\m-dppm)2]n+ (n= 0, 1, 2): Unusual Examples of
 Nickel(0)-Nickel(I) and Nickel(0)-Nickel(II) Mixed Valency
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1071
_journal_page_last               1081
_journal_paper_doi               10.1021/ic035021j
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C65 H71 N3 Ni2 P4'
_chemical_formula_weight         1135.14
_chemical_name_common            Ni2(m-dppm)2(m-CNterBu)(CNterBu)2
_chemical_name_systematic
; 
(\m~2~-terbutylisocianide)bis(terbutylisocianide) 
(bis(\m~2~-bis(diphenylphosphino) 
methane)-di-nickel 
;
_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                 109.16(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.657(5)
_cell_length_b                   11.322(2)
_cell_length_c                   23.208(5)
_cell_measurement_temperature    100(2)
_cell_volume                     5872(2)
_computing_cell_refinement
; 
SAINT PLUS 
;
_computing_data_collection
; 
SAINT PLUS 
;
_computing_data_reduction        'SAINT PLUS'
_computing_publication_material  'SHELXL-97 '
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
; 
Bruker SMART CCD 
;
_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  0.0571
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17682
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.792
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_type   empiric
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
; 
rectangular prism 
;
_exptl_crystal_F_000             2382.7
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.00000(7)
_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   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         4219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          7.663
_refine_ls_shift/su_mean         0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+4.9063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0887
_reflns_number_gt                3721
_reflns_number_total             4219
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035021jsi20030902_015739_1.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_diffrn_ambient_temperature,k' tag replaced with
'_diffrn_ambient_temperature'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_cell_measurement_temperature' value '-173(2)' was changed to
'100(2)' - it was converted from degrees Celsius(C) to
Kelvins(K).

'_diffrn_ambient_temperature' value '-173(2)' was
changed to '100(2)' - it was converted from degrees Celsius(C) to
Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_formula_sum        'C65H71N3Ni2 P4'
_cod_database_code               4310545