#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/05/4310545.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4310545
loop_
_publ_author_name
'Gregory M. Ferrence'
'Eugenio Simón-Manso'
'Brian K. Breedlove'
'Leah Meeuwenberg'
'Clifford P. Kubiak'
_publ_section_title
;
 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
;
_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
; 
(μ₂-terbutylisocianide)bis(terbutylisocianide) 
(bis(μ₂-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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0489P)²+4.9063P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.444170(12) 0.72330(2) 0.219428(12) 0.01913(13) Uani 1 1 d . . .
P2 P 0.41988(2) 0.61822(5) 0.28672(3) 0.01998(16) Uani 1 1 d . . .
P1 P 0.45019(2) 0.60418(5) 0.14726(3) 0.01936(16) Uani 1 1 d . . .
C21 C 0.40194(9) 0.7028(2) 0.34630(10) 0.0224(5) Uani 1 1 d . . .
C15 C 0.35476(10) 0.5190(2) 0.26285(10) 0.0253(5) Uani 1 1 d . . .
C9 C 0.44736(9) 0.6725(2) 0.07411(10) 0.0210(5) Uani 1 1 d . . .
C35 C 0.47942(9) 0.52004(19) 0.33264(10) 0.0221(5) Uani 1 1 d . . .
H35A H 0.4819 0.4501 0.3095 0.026 Uiso 1 1 calc R . .
H35B H 0.4714 0.4956 0.3692 0.026 Uiso 1 1 calc R . .
C23 C 0.37129(11) 0.7146(2) 0.43550(12) 0.0353(6) Uani 1 1 d . . .
H23 H 0.3590 0.6773 0.4651 0.042 Uiso 1 1 calc R . .
C16 C 0.29837(11) 0.5703(3) 0.23926(12) 0.0395(7) Uani 1 1 d . . .
H16 H 0.2947 0.6522 0.2387 0.047 Uiso 1 1 calc R . .
C3 C 0.39352(10) 0.4877(2) 0.11840(10) 0.0264(6) Uani 1 1 d . . .
N1 N 0.33098(9) 0.85102(18) 0.15368(9) 0.0302(5) Uani 1 1 d . . .
C12 C 0.44533(11) 0.7849(2) -0.03327(12) 0.0353(6) Uani 1 1 d . . .
H12 H 0.4447 0.8224 -0.0691 0.042 Uiso 1 1 calc R . .
C8 C 0.40528(12) 0.3721(2) 0.10705(11) 0.0351(6) Uani 1 1 d . . .
H8 H 0.4445 0.3478 0.1136 0.042 Uiso 1 1 calc R . .
C22 C 0.38288(10) 0.6488(2) 0.39057(11) 0.0294(6) Uani 1 1 d . . .
H22 H 0.3779 0.5673 0.3899 0.035 Uiso 1 1 calc R . .
C20 C 0.35864(11) 0.3974(2) 0.26247(12) 0.0332(6) Uani 1 1 d . . .
H20 H 0.3958 0.3612 0.2782 0.040 Uiso 1 1 calc R . .
C10 C 0.44936(11) 0.7942(2) 0.07093(11) 0.0305(6) Uani 1 1 d . . .
H10 H 0.4513 0.8392 0.1051 0.037 Uiso 1 1 calc R . .
C14 C 0.44397(11) 0.6077(2) 0.02242(11) 0.0312(6) Uani 1 1 d . . .
H14 H 0.4423 0.5257 0.0236 0.037 Uiso 1 1 calc R . .
C11 C 0.44851(12) 0.8500(2) 0.01751(12) 0.0393(7) Uani 1 1 d . . .
H11 H 0.4501 0.9320 0.0161 0.047 Uiso 1 1 calc R . .
C25 C 0.39589(11) 0.8903(2) 0.39247(12) 0.0385(7) Uani 1 1 d . . .
H25 H 0.4001 0.9720 0.3929 0.046 Uiso 1 1 calc R . .
C5 C 0.28824(13) 0.4398(3) 0.08725(13) 0.0503(8) Uani 1 1 d . . .
H5 H 0.2489 0.4633 0.0805 0.060 Uiso 1 1 calc R . .
C24 C 0.37788(11) 0.8356(3) 0.43658(12) 0.0369(6) Uani 1 1 d . . .
H24 H 0.3702 0.8801 0.4669 0.044 Uiso 1 1 calc R . .
C17 C 0.24770(12) 0.5011(3) 0.21659(14) 0.0511(8) Uani 1 1 d . . .
H17 H 0.2103 0.5366 0.2017 0.061 Uiso 1 1 calc R . .
C18 C 0.25239(12) 0.3796(3) 0.21592(13) 0.0474(8) Uani 1 1 d . . .
H18 H 0.2184 0.3330 0.2000 0.057 Uiso 1 1 calc R . .
C4 C 0.33407(11) 0.5200(2) 0.10869(12) 0.0382(7) Uani 1 1 d . . .
H4 H 0.3253 0.5970 0.1169 0.046 Uiso 1 1 calc R . .
C19 C 0.30772(13) 0.3284(3) 0.23894(13) 0.0435(7) Uani 1 1 d . . .
H19 H 0.3112 0.2466 0.2388 0.052 Uiso 1 1 calc R . .
C6 C 0.30024(14) 0.3256(3) 0.07583(12) 0.0523(9) Uani 1 1 d . . .
H6 H 0.2692 0.2714 0.0614 0.063 Uiso 1 1 calc R . .
C7 C 0.35827(16) 0.2917(3) 0.08577(12) 0.0497(9) Uani 1 1 d . . .
H7 H 0.3665 0.2139 0.0782 0.060 Uiso 1 1 calc R . .
C13 C 0.44303(12) 0.6637(2) -0.03077(11) 0.0367(6) Uani 1 1 d . . .
H13 H 0.4408 0.6191 -0.0651 0.044 Uiso 1 1 calc R . .
C26 C 0.40784(10) 0.8245(2) 0.34751(11) 0.0306(6) Uani 1 1 d . . .
H26 H 0.4199 0.8623 0.3179 0.037 Uiso 1 1 calc R . .
C31 C 0.22527(13) 0.8261(4) 0.10571(16) 0.0756(11) Uani 1 1 d . . .
H31A H 0.2323 0.7453 0.0975 0.113 Uiso 1 1 calc R . .
H31B H 0.1907 0.8551 0.0741 0.113 Uiso 1 1 calc R . .
H31C H 0.2187 0.8312 0.1443 0.113 Uiso 1 1 calc R . .
C34 C 0.27931(12) 0.8999(4) 0.10762(14) 0.0619(11) Uani 1 1 d . . .
C33 C 0.27078(19) 1.0241(4) 0.1258(3) 0.128(2) Uani 1 1 d . . .
H33A H 0.2575 1.0227 0.1606 0.192 Uiso 1 1 calc R . .
H33B H 0.2414 1.0630 0.0925 0.192 Uiso 1 1 calc R . .
H33C H 0.3080 1.0660 0.1358 0.192 Uiso 1 1 calc R . .
C1 C 0.37619(11) 0.8058(2) 0.18053(11) 0.0245(5) Uani 1 1 d . . .
C2 C 0.5000 0.8505(3) 0.2500 0.0260(8) Uani 1 2 d S . .
N2 N 0.5000 0.9567(3) 0.2500 0.0697(13) Uani 1 2 d S . .
C32 C 0.29290(17) 0.8916(7) 0.04820(18) 0.163(3) Uani 1 1 d . . .
H32A H 0.3234 0.9477 0.0486 0.245 Uiso 1 1 calc R . .
H32B H 0.2573 0.9084 0.0146 0.245 Uiso 1 1 calc R . .
H32C H 0.3066 0.8133 0.0438 0.245 Uiso 1 1 calc R . .
C27 C 0.4813(2) 1.0656(4) 0.2342(3) 0.038(2) Uani 0.495(11) 1 d P . .
C28 C 0.4620(3) 1.0635(5) 0.1651(3) 0.044(3) Uani 0.474(12) 1 d P . .
H28A H 0.4448 1.1384 0.1492 0.067 Uiso 0.55(6) 1 calc PR . .
H28B H 0.4329 1.0023 0.1497 0.067 Uiso 0.44(6) 1 calc PR . .
H28C H 0.4962 1.0486 0.1525 0.067 Uiso 0.59(6) 1 calc PR . .
C30 C 0.4267(3) 1.0844(5) 0.2549(4) 0.066(3) Uani 0.583(14) 1 d P . .
H30A H 0.4300 1.0670 0.2968 0.079 Uiso 0.44(7) 1 calc PR . .
H30B H 0.3869 1.0795 0.2249 0.079 Uiso 0.32(6) 1 calc PR . .
C29 C 0.4738(3) 1.1667(5) 0.2421(4) 0.091(3) Uani 0.614(12) 1 d P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Ni1 C2 100.72(10) . . ?
C1 Ni1 P2 103.71(8) . . ?
C2 Ni1 P2 116.96(4) . . ?
C1 Ni1 P1 101.83(8) . . ?
C2 Ni1 P1 122.23(4) . . ?
P2 Ni1 P1 108.03(3) . . ?
C1 Ni1 Ni1 149.12(7) . 2_655 ?
C2 Ni1 Ni1 48.42(7) . 2_655 ?
P2 Ni1 Ni1 93.99(3) . 2_655 ?
P1 Ni1 Ni1 96.31(3) . 2_655 ?
C35 P2 C15 102.25(11) . . ?
C35 P2 C21 101.58(10) . . ?
C15 P2 C21 99.62(10) . . ?
C35 P2 Ni1 114.39(8) . . ?
C15 P2 Ni1 120.54(8) . . ?
C21 P2 Ni1 115.66(8) . . ?
C35 P1 C3 102.22(11) 2_655 . ?
C35 P1 C9 101.92(10) 2_655 . ?
C3 P1 C9 99.39(10) . . ?
C35 P1 Ni1 113.90(8) 2_655 . ?
C3 P1 Ni1 119.76(8) . . ?
C9 P1 Ni1 116.94(8) . . ?
C26 C21 C22 118.5(2) . . ?
C26 C21 P2 119.07(18) . . ?
C22 C21 P2 122.45(18) . . ?
C20 C15 C16 118.1(2) . . ?
C20 C15 P2 124.09(19) . . ?
C16 C15 P2 117.60(19) . . ?
C10 C9 C14 118.3(2) . . ?
C10 C9 P1 118.39(17) . . ?
C14 C9 P1 123.26(18) . . ?
P2 C35 P1 106.96(11) . 2_655 ?
C24 C23 C22 120.1(2) . . ?
C17 C16 C15 120.8(3) . . ?
C8 C3 C4 118.1(2) . . ?
C8 C3 P1 125.42(19) . . ?
C4 C3 P1 116.44(19) . . ?
C1 N1 C34 165.9(2) . . ?
C11 C12 C13 119.5(2) . . ?
C3 C8 C7 119.9(3) . . ?
C23 C22 C21 120.9(2) . . ?
C15 C20 C19 120.9(3) . . ?
C9 C10 C11 120.8(2) . . ?
C13 C14 C9 120.7(2) . . ?
C12 C11 C10 120.3(2) . . ?
C24 C25 C26 120.5(3) . . ?
C6 C5 C4 120.3(3) . . ?
C23 C24 C25 119.6(2) . . ?
C18 C17 C16 120.4(3) . . ?
C19 C18 C17 119.2(3) . . ?
C5 C4 C3 121.2(3) . . ?
C18 C19 C20 120.7(3) . . ?
C5 C6 C7 119.5(3) . . ?
C6 C7 C8 121.0(3) . . ?
C12 C13 C14 120.4(2) . . ?
C21 C26 C25 120.4(2) . . ?
N1 C34 C33 108.1(3) . . ?
N1 C34 C31 108.1(3) . . ?
C33 C34 C31 109.6(3) . . ?
N1 C34 C32 105.6(2) . . ?
C33 C34 C32 113.7(4) . . ?
C31 C34 C32 111.5(4) . . ?
N1 C1 Ni1 175.1(2) . . ?
N2 C2 Ni1 138.42(7) . . ?
N2 C2 Ni1 138.42(7) . 2_655 ?
Ni1 C2 Ni1 83.16(14) . 2_655 ?
C2 N2 C27 159.0(2) . 2_655 ?
C2 N2 C27 159.0(2) . . ?
C27 N2 C27 41.9(5) 2_655 . ?
C27 C27 C29 91.7(5) 2_655 . ?
C27 C27 N2 69.0(2) 2_655 . ?
C29 C27 N2 156.1(7) . . ?
C27 C27 C28 134.6(10) 2_655 . ?
C29 C27 C28 99.9(6) . . ?
N2 C27 C28 103.7(4) . . ?
C27 C27 C29 50.4(3) 2_655 2_655 ?
C29 C27 C29 49.0(6) . 2_655 ?
N2 C27 C29 117.9(4) . 2_655 ?
C28 C27 C29 108.9(5) . 2_655 ?
C27 C27 C30 115.1(10) 2_655 . ?
C29 C27 C30 68.3(5) . . ?
N2 C27 C30 106.4(4) . . ?
C28 C27 C30 109.9(5) . . ?
C29 C27 C30 109.8(5) 2_655 . ?
C27 C30 C29 45.0(3) . . ?
C29 C29 C27 81.4(5) 2_655 . ?
C29 C29 C27 49.6(3) 2_655 2_655 ?
C27 C29 C27 38.0(4) . 2_655 ?
C29 C29 C30 133.8(7) 2_655 . ?
C27 C29 C30 66.7(5) . . ?
C27 C29 C30 86.6(4) 2_655 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C1 1.823(2) . ?
Ni1 C2 1.925(3) . ?
Ni1 P2 2.1849(7) . ?
Ni1 P1 2.1911(7) . ?
Ni1 Ni1 2.5555(10) 2_655 ?
P2 C35 1.836(2) . ?
P2 C15 1.839(2) . ?
P2 C21 1.842(2) . ?
P1 C35 1.841(2) 2_655 ?
P1 C3 1.842(2) . ?
P1 C9 1.847(2) . ?
C21 C26 1.384(3) . ?
C21 C22 1.391(3) . ?
C15 C20 1.380(4) . ?
C15 C16 1.392(4) . ?
C9 C10 1.381(3) . ?
C9 C14 1.386(3) . ?
C35 P1 1.841(2) 2_655 ?
C23 C24 1.378(4) . ?
C23 C22 1.380(4) . ?
C16 C17 1.384(4) . ?
C3 C8 1.382(4) . ?
C3 C4 1.398(4) . ?
N1 C1 1.165(3) . ?
N1 C34 1.444(3) . ?
C12 C11 1.371(4) . ?
C12 C13 1.375(4) . ?
C8 C7 1.396(4) . ?
C20 C19 1.389(4) . ?
C10 C11 1.386(3) . ?
C14 C13 1.381(3) . ?
C25 C24 1.378(4) . ?
C25 C26 1.385(4) . ?
C5 C6 1.368(5) . ?
C5 C4 1.376(4) . ?
C17 C18 1.381(4) . ?
C18 C19 1.369(4) . ?
C6 C7 1.370(5) . ?
C31 C34 1.516(5) . ?
C34 C33 1.500(6) . ?
C34 C32 1.518(5) . ?
C2 N2 1.202(5) . ?
C2 Ni1 1.925(3) 2_655 ?
N2 C27 1.321(6) 2_655 ?
N2 C27 1.321(6) . ?
C27 C27 0.945(10) 2_655 ?
C27 C29 1.182(7) . ?
C27 C28 1.517(9) . ?
C27 C29 1.535(7) 2_655 ?
C27 C30 1.536(9) . ?
C30 C29 1.554(9) . ?
C29 C29 1.172(13) 2_655 ?
C29 C27 1.535(7) 2_655 ?
