#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:20:08 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179372 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/69/4326954.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_4326954
loop_
_publ_author_name
'Michael T. Mock'
'Robert G. Potter'
'Molly J. O'Hagan'
'Donald M. Camaioni'
'William G. Dougherty'
'W. Scott Kassel'
'Daniel L. DuBois'
_publ_section_title
;
 Synthesis and Hydride Transfer Reactions of Cobalt and Nickel Hydride
 Complexes to BX3 Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11914
_journal_page_last               11928
_journal_paper_doi               10.1021/ic200857x
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C20 H44 B2 Co F8 N4 P4'
_chemical_formula_weight         697.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.137(4)
_cell_angle_beta                 92.512(4)
_cell_angle_gamma                97.786(4)
_cell_formula_units_Z            2
_cell_length_a                   8.4911(5)
_cell_length_b                   12.9468(8)
_cell_length_c                   15.0180(9)
_cell_measurement_reflns_used    3301
_cell_measurement_temperature    117(2)
_cell_measurement_theta_max      67.51
_cell_measurement_theta_min      5.27
_cell_volume                     1633.62(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      117(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1526
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9633
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         68.10
_diffrn_reflns_theta_min         4.48
_exptl_absorpt_coefficient_mu    6.551
_exptl_absorpt_correction_T_max  0.5810
_exptl_absorpt_correction_T_min  0.3035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_description       block
_exptl_crystal_F_000             722
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         9633
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.0537
_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)+(0.0878P)²+3.1212P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1656
_reflns_number_gt                8151
_reflns_number_total             9633
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200857x_si_001_01.cif
_cod_data_source_block           pnl001_Codmpe2CH3CN2_BF42
_cod_database_code               4326954
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Co1 Co 0.5000 0.5000 1.0000 0.01712(19) Uani 1 2 d S . .
Co2 Co 0.5000 0.0000 0.5000 0.01845(19) Uani 1 2 d S . .
B1 B 0.9758(6) 0.6410(4) 0.6763(3) 0.0338(10) Uani 1 1 d . . .
B2 B 0.9514(5) 0.1316(3) 0.8307(3) 0.0284(9) Uani 1 1 d . . .
F1 F 1.0697(3) 0.7007(2) 0.74163(17) 0.0496(7) Uani 1 1 d . . .
F2 F 0.9929(3) 0.53687(19) 0.68719(18) 0.0480(7) Uani 1 1 d . . .
F3 F 0.8197(3) 0.6558(3) 0.6843(2) 0.0616(8) Uani 1 1 d . . .
F4 F 1.0267(4) 0.6726(2) 0.59327(17) 0.0518(7) Uani 1 1 d . . .
F5 F 0.8147(3) 0.1653(2) 0.7951(2) 0.0585(8) Uani 1 1 d . . .
F6 F 1.0590(4) 0.1364(3) 0.7659(2) 0.0704(9) Uani 1 1 d . . .
F7 F 0.9158(4) 0.0304(2) 0.8572(2) 0.0725(10) Uani 1 1 d . . .
F8 F 1.0118(4) 0.1937(2) 0.90216(19) 0.0642(9) Uani 1 1 d . . .
N1 N 0.3142(4) 0.3744(2) 1.0469(2) 0.0261(7) Uani 1 1 d . . .
N2 N 0.3088(4) -0.1284(2) 0.4465(2) 0.0267(7) Uani 1 1 d . . .
N3 N 0.4894(6) 0.4073(3) 0.6143(3) 0.0533(11) Uani 1 1 d . . .
N4 N 0.4724(6) 0.8884(4) 0.8815(3) 0.0615(12) Uani 1 1 d . . .
P1 P 0.33818(10) 0.51061(7) 0.87949(6) 0.0200(2) Uani 1 1 d . . .
P2 P 0.37027(11) 0.62119(7) 1.06160(6) 0.0217(2) Uani 1 1 d . . .
P3 P 0.34245(11) 0.03185(8) 0.61035(6) 0.0233(2) Uani 1 1 d . . .
P4 P 0.38257(10) 0.11847(7) 0.42363(6) 0.0222(2) Uani 1 1 d . . .
C1 C 0.2541(5) 0.3978(3) 0.8107(3) 0.0318(9) Uani 1 1 d . . .
H1A H 0.1707 0.4173 0.7697 0.048 Uiso 1 1 calc R . .
H1B H 0.2083 0.3422 0.8490 0.048 Uiso 1 1 calc R . .
H1C H 0.3379 0.3732 0.7765 0.048 Uiso 1 1 calc R . .
C2 C 0.4104(4) 0.6050(3) 0.7979(2) 0.0251(8) Uani 1 1 d . . .
H2A H 0.3263 0.6096 0.7519 0.038 Uiso 1 1 calc R . .
H2B H 0.5033 0.5829 0.7703 0.038 Uiso 1 1 calc R . .
H2C H 0.4406 0.6734 0.8275 0.038 Uiso 1 1 calc R . .
C3 C 0.1583(4) 0.5563(3) 0.9194(2) 0.0271(8) Uani 1 1 d . . .
H3A H 0.0931 0.5776 0.8684 0.032 Uiso 1 1 calc R . .
H3B H 0.0938 0.4996 0.9502 0.032 Uiso 1 1 calc R . .
C4 C 0.2081(5) 0.6488(3) 0.9835(3) 0.0292(8) Uani 1 1 d . . .
H4A H 0.1157 0.6632 1.0174 0.035 Uiso 1 1 calc R . .
H4B H 0.2444 0.7115 0.9493 0.035 Uiso 1 1 calc R . .
C5 C 0.4757(5) 0.7508(3) 1.0860(3) 0.0304(8) Uani 1 1 d . . .
H5A H 0.4015 0.7959 1.1084 0.046 Uiso 1 1 calc R . .
H5B H 0.5213 0.7798 1.0315 0.046 Uiso 1 1 calc R . .
H5C H 0.5611 0.7468 1.1313 0.046 Uiso 1 1 calc R . .
C6 C 0.2717(5) 0.5862(3) 1.1633(3) 0.0321(9) Uani 1 1 d . . .
H6A H 0.2061 0.6398 1.1793 0.048 Uiso 1 1 calc R . .
H6B H 0.3517 0.5809 1.2115 0.048 Uiso 1 1 calc R . .
H6C H 0.2040 0.5189 1.1542 0.048 Uiso 1 1 calc R . .
C7 C 0.2378(4) 0.3023(3) 1.0720(2) 0.0223(7) Uani 1 1 d . . .
C8 C 0.1457(5) 0.2085(3) 1.1037(3) 0.0340(9) Uani 1 1 d . . .
H8A H 0.0773 0.1740 1.0545 0.051 Uiso 1 1 calc R . .
H8B H 0.0796 0.2271 1.1518 0.051 Uiso 1 1 calc R . .
H8C H 0.2181 0.1611 1.1261 0.051 Uiso 1 1 calc R . .
C9 C 0.2181(7) -0.0735(4) 0.6600(4) 0.0693(19) Uani 1 1 d . A .
H9A H 0.1403 -0.0451 0.6964 0.104 Uiso 1 1 calc R . .
H9B H 0.2843 -0.1131 0.6977 0.104 Uiso 1 1 calc R . .
H9C H 0.1621 -0.1197 0.6129 0.104 Uiso 1 1 calc R . .
C10 C 0.4284(6) 0.1068(5) 0.7058(3) 0.0576(15) Uani 1 1 d . A .
H10A H 0.3436 0.1247 0.7431 0.086 Uiso 1 1 calc R . .
H10B H 0.4911 0.1709 0.6864 0.086 Uiso 1 1 calc R . .
H10C H 0.4976 0.0660 0.7402 0.086 Uiso 1 1 calc R . .
C11 C 0.2442(14) 0.1492(11) 0.5793(8) 0.0364(15) Uani 0.374(8) 1 d P A 1
H11A H 0.1440 0.1494 0.6106 0.044 Uiso 0.374(8) 1 calc PR A 1
H11B H 0.3157 0.2144 0.5954 0.044 Uiso 0.374(8) 1 calc PR A 1
C12 C 0.211(2) 0.1403(13) 0.4815(14) 0.034(2) Uani 0.374(8) 1 d P A 1
H12A H 0.1739 0.2052 0.4605 0.041 Uiso 0.374(8) 1 calc PR A 1
H12B H 0.1250 0.0819 0.4678 0.041 Uiso 0.374(8) 1 calc PR A 1
C11' C 0.1764(8) 0.0902(7) 0.5589(5) 0.0364(15) Uani 0.626(8) 1 d P A 2
H11C H 0.1045 0.0370 0.5230 0.044 Uiso 0.626(8) 1 calc PR A 2
H11D H 0.1145 0.1192 0.6055 0.044 Uiso 0.626(8) 1 calc PR A 2
C12' C 0.2487(14) 0.1767(7) 0.4997(7) 0.034(2) Uani 0.626(8) 1 d P A 2
H12C H 0.3098 0.2340 0.5365 0.041 Uiso 0.626(8) 1 calc PR A 2
H12D H 0.1637 0.2053 0.4647 0.041 Uiso 0.626(8) 1 calc PR A 2
C13 C 0.4985(6) 0.2408(4) 0.3972(5) 0.075(2) Uani 1 1 d . A .
H13A H 0.4268 0.2916 0.3816 0.113 Uiso 1 1 calc R . .
H13B H 0.5641 0.2299 0.3467 0.113 Uiso 1 1 calc R . .
H13C H 0.5673 0.2672 0.4491 0.113 Uiso 1 1 calc R . .
C14 C 0.2717(9) 0.0781(5) 0.3221(4) 0.078(2) Uani 1 1 d . A .
H14A H 0.2102 0.1331 0.3029 0.118 Uiso 1 1 calc R . .
H14B H 0.1991 0.0141 0.3318 0.118 Uiso 1 1 calc R . .
H14C H 0.3450 0.0647 0.2760 0.118 Uiso 1 1 calc R . .
C15 C 0.2274(4) -0.2003(3) 0.4190(2) 0.0258(8) Uani 1 1 d . . .
C16 C 0.1257(5) -0.2934(3) 0.3856(3) 0.0337(9) Uani 1 1 d . . .
H16A H 0.1916 -0.3441 0.3636 0.051 Uiso 1 1 calc R . .
H16B H 0.0549 -0.2751 0.3369 0.051 Uiso 1 1 calc R . .
H16C H 0.0619 -0.3238 0.4338 0.051 Uiso 1 1 calc R . .
C17 C 0.2540(6) 0.4868(4) 0.5390(4) 0.0529(13) Uani 1 1 d . . .
H17A H 0.2961 0.5443 0.5016 0.079 Uiso 1 1 calc R . .
H17B H 0.1895 0.5130 0.5847 0.079 Uiso 1 1 calc R . .
H17C H 0.1880 0.4330 0.5020 0.079 Uiso 1 1 calc R . .
C18 C 0.3850(6) 0.4424(3) 0.5817(3) 0.0390(10) Uani 1 1 d . . .
C19 C 0.2514(6) 0.9827(4) 0.9434(4) 0.0618(15) Uani 1 1 d . . .
H19A H 0.2227 0.9539 1.0012 0.093 Uiso 1 1 calc R . .
H19B H 0.1578 0.9726 0.9020 0.093 Uiso 1 1 calc R . .
H19C H 0.2896 1.0574 0.9509 0.093 Uiso 1 1 calc R . .
C20 C 0.3757(6) 0.9299(4) 0.9079(3) 0.0409(10) Uani 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 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 '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
P1 Co1 P1 180.00(4) . 2_667
P1 Co1 P2 85.56(3) . .
P1 Co1 P2 94.44(3) 2_667 .
P1 Co1 P2 94.44(3) . 2_667
P1 Co1 P2 85.56(3) 2_667 2_667
P2 Co1 P2 180.0 . 2_667
P1 Co1 N1 92.88(8) . 2_667
P1 Co1 N1 87.12(8) 2_667 2_667
P2 Co1 N1 90.41(9) . 2_667
P2 Co1 N1 89.59(9) 2_667 2_667
P1 Co1 N1 87.12(8) . .
P1 Co1 N1 92.88(8) 2_667 .
P2 Co1 N1 89.59(9) . .
P2 Co1 N1 90.40(9) 2_667 .
N1 Co1 N1 180.0 2_667 .
P3 Co2 P3 180.0 . 2_656
P3 Co2 P4 94.14(3) . 2_656
P3 Co2 P4 85.86(3) 2_656 2_656
P3 Co2 P4 85.86(3) . .
P3 Co2 P4 94.14(3) 2_656 .
P4 Co2 P4 180.00(4) 2_656 .
P3 Co2 N2 89.15(8) . .
P3 Co2 N2 90.85(8) 2_656 .
P4 Co2 N2 89.69(8) 2_656 .
P4 Co2 N2 90.31(8) . .
P3 Co2 N2 90.85(8) . 2_656
P3 Co2 N2 89.15(8) 2_656 2_656
P4 Co2 N2 90.31(8) 2_656 2_656
P4 Co2 N2 89.69(8) . 2_656
N2 Co2 N2 180.000(1) . 2_656
F3 B1 F1 109.1(4) . .
F3 B1 F2 110.4(4) . .
F1 B1 F2 108.9(4) . .
F3 B1 F4 109.9(4) . .
F1 B1 F4 108.7(4) . .
F2 B1 F4 109.7(4) . .
F6 B2 F8 110.0(4) . .
F6 B2 F7 109.9(4) . .
F8 B2 F7 109.7(4) . .
F6 B2 F5 107.8(4) . .
F8 B2 F5 110.3(4) . .
F7 B2 F5 109.2(4) . .
C7 N1 Co1 170.1(3) . .
C15 N2 Co2 171.6(3) . .
C2 P1 C1 102.94(18) . .
C2 P1 C3 104.68(17) . .
C1 P1 C3 101.39(19) . .
C2 P1 Co1 115.97(12) . .
C1 P1 Co1 123.07(13) . .
C3 P1 Co1 106.55(12) . .
C6 P2 C5 104.07(19) . .
C6 P2 C4 104.18(19) . .
C5 P2 C4 101.85(18) . .
C6 P2 Co1 116.36(14) . .
C5 P2 Co1 119.21(14) . .
C4 P2 Co1 109.28(13) . .
C10 P3 C9 102.3(3) . .
C10 P3 C11' 111.2(3) . .
C9 P3 C11' 95.1(3) . .
C10 P3 C11 86.8(5) . .
C9 P3 C11 116.3(4) . .
C11' P3 C11 28.9(4) . .
C10 P3 Co2 118.69(15) . .
C9 P3 Co2 120.59(16) . .
C11' P3 Co2 106.6(2) . .
C11 P3 Co2 107.6(3) . .
C12 P4 C14 93.9(7) . .
C12 P4 C13 110.8(6) . .
C14 P4 C13 104.1(3) . .
C12 P4 C12' 18.3(5) . .
C14 P4 C12' 108.3(4) . .
C13 P4 C12' 95.7(4) . .
C12 P4 Co2 107.1(7) . .
C14 P4 Co2 118.74(18) . .
C13 P4 Co2 119.37(16) . .
C12' P4 Co2 108.0(3) . .
C4 C3 P1 108.4(2) . .
C3 C4 P2 110.4(3) . .
N1 C7 C8 177.8(4) . .
C12 C11 P3 106.0(10) . .
C11 C12 P4 112.0(13) . .
C12' C11' P3 106.9(6) . .
C11' C12' P4 107.3(6) . .
N2 C15 C16 178.5(4) . .
N3 C18 C17 179.1(5) . .
N4 C20 C19 179.1(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 P1 2.2417(9) .
Co1 P1 2.2418(9) 2_667
Co1 P2 2.2429(9) .
Co1 P2 2.2430(9) 2_667
Co1 N1 2.253(3) 2_667
Co1 N1 2.253(3) .
Co2 P3 2.2411(9) .
Co2 P3 2.2412(9) 2_656
Co2 P4 2.2464(9) 2_656
Co2 P4 2.2465(9) .
Co2 N2 2.269(3) .
Co2 N2 2.269(3) 2_656
B1 F3 1.375(6) .
B1 F1 1.388(6) .
B1 F2 1.388(5) .
B1 F4 1.389(5) .
B2 F6 1.360(5) .
B2 F8 1.367(5) .
B2 F7 1.374(5) .
B2 F5 1.384(5) .
N1 C7 1.143(5) .
N2 C15 1.140(5) .
N3 C18 1.145(6) .
N4 C20 1.123(6) .
P1 C2 1.814(4) .
P1 C1 1.817(4) .
P1 C3 1.831(4) .
P2 C6 1.810(4) .
P2 C5 1.814(4) .
P2 C4 1.846(4) .
P3 C10 1.786(4) .
P3 C9 1.803(5) .
P3 C11' 1.836(6) .
P3 C11 1.887(12) .
P4 C12 1.78(2) .
P4 C14 1.787(5) .
P4 C13 1.809(5) .
P4 C12' 1.865(11) .
C3 C4 1.524(6) .
C7 C8 1.453(5) .
C11 C12 1.48(2) .
C11' C12' 1.525(13) .
C15 C16 1.451(5) .
C17 C18 1.450(7) .
C19 C20 1.447(8) .
