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_4310546
_publ_contact_author_address
; 
9500 gilman drive 
La Jolla CA 92093-0358 
USA 
;
_publ_contact_author_email       ckubiak@ucsd.edu
_publ_contact_author_name        'Clifford P. Kubiak'
_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            'C66 H73 Cl2 F6 N3 Ni2 P5'
_chemical_formula_weight         1365.52
_chemical_name_systematic
; 
(\m~2~-terbutylisocianide)bis(terbutylisocianide) 
(bis(\m~2~-bis(diphenylphosphino) 
methane)-di-nickel hexafluorophosphate 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.439(3)
_cell_angle_beta                 101.316(3)
_cell_angle_gamma                110.051(3)
_cell_formula_units_Z            1
_cell_length_a                   10.6578(7)
_cell_length_b                   13.3188(9)
_cell_length_c                   13.5122(6)
_cell_measurement_reflns_used    13500
_cell_measurement_temperature    193
_cell_measurement_theta_max      27
_cell_measurement_theta_min      4
_cell_volume                     1670.64(18)
_computing_cell_refinement       DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_data_collection       Collect_(Nonius,_1998)
_computing_data_reduction        DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_molecular_graphics
; 
ORTEP (Johnson, 1976) 
Xtal_GX (Hall, 1995) 
PLUTON (Spek, 1991) 
;
_computing_publication_material  CIF_VAX_MolEN_(Fair,_1990)
_computing_structure_refinement  SHELX97_(Sheldrick,_1997)
_computing_structure_solution    PATTY_(DIRDIF92,_Beurskins,_1992)
_diffrn_ambient_temperature      193
_diffrn_radiation_type           MO-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13500
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         4.00
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_T_max  0.7351
_exptl_absorpt_correction_T_min  0.3706
_exptl_absorpt_correction_type   sempirical
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.36
_exptl_crystal_description       chunk
_exptl_crystal_F_000             709
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.81
_refine_diff_density_min         -0.55
_refine_ls_abs_structure_details
; 
refinement results for the other absolute structure: 
R = 0.000 Rw = 0.000 goodness_of_fit = 0.000 
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         8374
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.047
_refine_ls_shift/su_max          0.046
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+1.9721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.115
_reflns_number_gt                7788
_reflns_number_total             8374
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            ic035021jsi20030902_015739_2.cif
_cod_data_source_block           6(+)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc' 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_cell_volume        1670.6(4)
_cod_database_code               4310546