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_4310549
_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            'C81 H79 F12 N3 Ni2 O P6'
_chemical_formula_weight         1630.71
_chemical_name_common
'[Ni2(m-dppm)2(m-CN-Xylyl)(m-CN-Xylyl)2](PF6)2xTHF'
_chemical_name_systematic
; 
(\m~2~-Xylylisocianide)bis(Xylylisocianide) 
(bis(\m~2~-bis(diphenylphosphino) 
methane)-di-nickel bis(hexaflurophosphate) 
;
_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                 100.956(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8173(16)
_cell_length_b                   23.585(3)
_cell_length_c                   23.519(3)
_cell_measurement_temperature    100(2)
_cell_volume                     7524.7(16)
_computing_cell_refinement       'SAINT PLUS'
_computing_data_collection       'SAINT PLUS'
_computing_data_reduction        'SAINT PLUS'
_computing_publication_material  SHELXTL-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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0983
_diffrn_reflns_av_sigmaI/netI    0.0738
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            43737
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_T_max  0.9155
_exptl_absorpt_correction_T_min  0.8922
_exptl_absorpt_correction_type   empiric
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'deep brown'
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3372
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.498
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       0.00000(11)
_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   0.978
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     953
_refine_ls_number_reflns         9838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          5.321
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1165P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1627
_refine_ls_wR_factor_ref         0.1718
_reflns_number_gt                7196
_reflns_number_total             9838
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035021jsi20030902_015739_5.cif
_cod_data_source_block           8(2+)
_cod_depositor_comments
;
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_cell_volume        7524.7(15)
_cod_database_code               4310549