#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:09:21 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178937 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/66/4116632.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_4116632
loop_
_publ_author_name
'Douglas E. Berning'
'Bruce C. Noll'
'Daniel L. DuBois'
_publ_section_title
;
 Relative Hydride, Proton, and Hydrogen Atom Transfer Abilities of
 [HM(diphosphine)2]PF6 Complexes (M = Pt, Ni)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11432
_journal_page_last               11447
_journal_paper_doi               10.1021/ja991888y
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C20 H50 B2 F8 Ni O P4'
_chemical_formula_weight         662.81
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7301(2)
_cell_length_b                   10.91290(10)
_cell_length_c                   15.77990(10)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    162(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.19
_cell_volume                     3053.20(5)
_computing_cell_refinement       'SAINT v4.05 (Siemens, 1995)'
_computing_data_collection       'SMART v4.05 (Siemens, 1995)'
_computing_data_reduction        'SAINT v4.05 (Siemens, 1995)'
_computing_molecular_graphics    'SHELXTL XP v5.03 (Siemens, 1994)'
_computing_publication_material  'CIFTAB 97-2 (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      162(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22340
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_T_max  0.9309
_exptl_absorpt_correction_T_min  0.5610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3798
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0398P)²+1.4490P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0731
_reflns_number_gt                3145
_reflns_number_total             3798
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja991888y_3.cif
_cod_data_source_block           '[Ni(depe)2](BF4)2'
_cod_database_code               4116632
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, 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
Ni Ni 0.5000 0.5000 0.5000 0.01247(8) Uani 1 2 d S
P1 P 0.46361(2) 0.30778(3) 0.47297(2) 0.01449(9) Uani 1 1 d .
P2 P 0.37826(2) 0.53317(3) 0.52673(2) 0.01501(9) Uani 1 1 d .
C1 C 0.51104(11) 0.19901(14) 0.54327(10) 0.0219(3) Uani 1 1 d .
H1A H 0.4872(12) 0.1196(19) 0.5343(13) 0.026(5) Uiso 1 1 d .
H1B H 0.5616(13) 0.1928(18) 0.5224(13) 0.027(5) Uiso 1 1 d .
C2 C 0.50543(12) 0.23612(18) 0.63659(11) 0.0294(4) Uani 1 1 d .
H2A H 0.5335(14) 0.181(2) 0.6696(15) 0.040(6) Uiso 1 1 d .
H2B H 0.4548(14) 0.234(2) 0.6539(14) 0.034(6) Uiso 1 1 d .
H2C H 0.5245(12) 0.317(2) 0.6458(13) 0.028(5) Uiso 1 1 d .
C3 C 0.47257(10) 0.24611(15) 0.36563(9) 0.0194(3) Uani 1 1 d .
H3A H 0.4545(13) 0.3082(19) 0.3264(13) 0.032(5) Uiso 1 1 d .
H3B H 0.5248(13) 0.2382(19) 0.3536(12) 0.026(5) Uiso 1 1 d .
C4 C 0.43085(11) 0.12479(16) 0.35183(12) 0.0272(4) Uani 1 1 d .
H4A H 0.4431(14) 0.095(2) 0.2962(17) 0.051(7) Uiso 1 1 d .
H4B H 0.3758(13) 0.137(2) 0.3528(13) 0.033(6) Uiso 1 1 d .
H4C H 0.4433(13) 0.068(2) 0.3939(15) 0.038(6) Uiso 1 1 d .
C5 C 0.36225(10) 0.28847(14) 0.49713(10) 0.0212(3) Uani 1 1 d .
H5A H 0.3359(13) 0.2966(18) 0.4431(13) 0.030(5) Uiso 1 1 d .
H5B H 0.3523(13) 0.207(2) 0.5207(13) 0.033(6) Uiso 1 1 d .
C6 C 0.33658(10) 0.38703(14) 0.55967(10) 0.0211(3) Uani 1 1 d .
H6A H 0.3549(11) 0.3702(16) 0.6156(12) 0.018(4) Uiso 1 1 d .
H6B H 0.2829(12) 0.3976(17) 0.5649(12) 0.022(5) Uiso 1 1 d .
C7 C 0.34174(10) 0.64138(14) 0.60494(9) 0.0186(3) Uani 1 1 d .
H7A H 0.3602(12) 0.7202(18) 0.5924(13) 0.026(5) Uiso 1 1 d .
H7B H 0.2886(12) 0.6448(17) 0.5976(12) 0.021(5) Uiso 1 1 d .
C8 C 0.36129(11) 0.60434(16) 0.69629(10) 0.0241(3) Uani 1 1 d .
H8A H 0.3492(14) 0.669(2) 0.7344(15) 0.042(6) Uiso 1 1 d .
H8B H 0.4131(14) 0.5833(19) 0.7019(13) 0.034(5) Uiso 1 1 d .
H8C H 0.3330(13) 0.534(2) 0.7142(14) 0.031(5) Uiso 1 1 d .
C9 C 0.33129(10) 0.57387(16) 0.42673(10) 0.0237(3) Uani 1 1 d .
H9A H 0.3452(13) 0.656(2) 0.4175(13) 0.035(6) Uiso 1 1 d .
H9B H 0.3535(13) 0.5247(19) 0.3832(14) 0.031(5) Uiso 1 1 d .
C10 C 0.24563(12) 0.5597(2) 0.42557(13) 0.0361(4) Uani 1 1 d .
H10A H 0.2267(13) 0.590(2) 0.3744(15) 0.042(6) Uiso 1 1 d .
H10B H 0.2216(16) 0.605(2) 0.4683(18) 0.054(7) Uiso 1 1 d .
H10C H 0.2319(17) 0.472(2) 0.4340(17) 0.058(8) Uiso 1 1 d .
B B 0.36307(12) 0.50604(16) 0.18569(13) 0.0250(4) Uani 1 1 d .
F1 F 0.31647(7) 0.59906(11) 0.21318(8) 0.0458(3) Uani 1 1 d .
F2 F 0.32360(9) 0.39505(12) 0.18319(9) 0.0577(4) Uani 1 1 d .
F3 F 0.38820(8) 0.53136(12) 0.10370(7) 0.0446(3) Uani 1 1 d .
F4 F 0.42359(7) 0.49455(10) 0.24034(7) 0.0357(3) Uani 1 1 d .
O O 0.2500 0.2500 0.30825(15) 0.0484(6) Uani 1 2 d S
H1O H 0.2678(18) 0.295(3) 0.2765(17) 0.059(9) Uiso 1 1 d .
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
P2 Ni P2 180.0 . 5_666
P2 Ni P1 95.222(14) . 5_666
P2 Ni P1 84.778(14) 5_666 5_666
P2 Ni P1 84.778(14) . .
P2 Ni P1 95.222(14) 5_666 .
P1 Ni P1 180.0 5_666 .
C1 P1 C3 106.42(8) . .
C1 P1 C5 104.35(8) . .
C3 P1 C5 103.50(7) . .
C1 P1 Ni 111.12(5) . .
C3 P1 Ni 119.78(5) . .
C5 P1 Ni 110.37(5) . .
C7 P2 C6 103.18(7) . .
C7 P2 C9 105.26(7) . .
C6 P2 C9 105.72(8) . .
C7 P2 Ni 125.18(6) . .
C6 P2 Ni 107.62(6) . .
C9 P2 Ni 108.39(6) . .
C2 C1 P1 112.45(12) . .
C4 C3 P1 114.05(12) . .
C6 C5 P1 110.01(11) . .
C5 C6 P2 108.00(11) . .
C8 C7 P2 112.57(11) . .
C10 C9 P2 115.87(13) . .
F1 B F4 109.61(15) . .
F1 B F3 109.70(15) . .
F4 B F3 110.38(17) . .
F1 B F2 110.27(18) . .
F4 B F2 109.10(15) . .
F3 B F2 107.75(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni P2 2.2290(4) .
Ni P2 2.2290(4) 5_666
Ni P1 2.2358(3) 5_666
Ni P1 2.2358(3) .
P1 C1 1.8295(16) .
P1 C3 1.8294(15) .
P1 C5 1.8490(18) .
P2 C7 1.8267(15) .
P2 C6 1.8329(16) .
P2 C9 1.8387(16) .
C1 C2 1.531(2) .
C3 C4 1.532(2) .
C5 C6 1.529(2) .
C7 C8 1.537(2) .
C9 C10 1.527(3) .
B F1 1.379(2) .
B F4 1.382(2) .
B F3 1.396(2) .
B F2 1.399(2) .
