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_4310547
_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 H74 Cl2 F12 N3 Ni2 P6'
_chemical_formula_weight         1511.42
_chemical_name_common            Ni2(m-dppm)2(m-CNterBu)(CNterBu)2(PF6)2
_chemical_name_systematic
; 
(\m~2~-terbutylisocianide)bis(terbutylisocianide) 
(bis(\m~2~-bis(diphenylphosphino) 
methane)-di-nickel bis(hexafluorophosphate) 
;
_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                 102.58(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.050(10)
_cell_length_b                   16.340(10)
_cell_length_c                   40.280(30)
_cell_measurement_temperature    186(2)
_cell_volume                     14164(15)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      186(2)
_diffrn_measurement_device       'Siemens 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  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            12114
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.56
_diffrn_standards_interval_count 197
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_T_max  0.8203
_exptl_absorpt_correction_T_min  0.6722
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_F_000             6232
_exptl_crystal_size_max          2.00
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.049
_refine_ls_goodness_of_fit_obs   1.091
_refine_ls_matrix_type           full
_refine_ls_number_parameters     743
_refine_ls_number_reflns         11938
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_restrained_S_obs      1.091
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_obs          0.0601
_refine_ls_shift/esd_max         1.097
_refine_ls_shift/esd_mean        0.080
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+90.8432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1679
_refine_ls_wR_factor_obs         0.1417
_reflns_number_observed          9380
_reflns_number_total             11948
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic035021jsi20030902_015739_3.cif
_cod_data_source_block           6(2+)
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+90.8432P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+90.8432P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        14164.4(151)
_cod_database_code               4310547