#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/10/20/4102033.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_4102033
loop_
_publ_author_name
'Alexander J. M. Miller'
'Jay A. Labinger'
'John E. Bercaw'
_publ_section_title
;
 Homogeneous CO Hydrogenation: Dihydrogen Activation Involves a Frustrated
 Lewis Pair Instead of a Platinum Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3301
_journal_page_last               3303
_journal_paper_doi               10.1021/ja100574n
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C56 H72 B2 O6 P2 Re, B F4'
_chemical_formula_sum            'C56 H72 B3 F4 O6 P2 Re'
_chemical_formula_weight         1197.71
_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                92.554(2)
_cell_angle_beta                 104.359(2)
_cell_angle_gamma                105.481(2)
_cell_formula_units_Z            1
_cell_length_a                   9.7744(4)
_cell_length_b                   10.3565(4)
_cell_length_c                   14.9063(6)
_cell_measurement_reflns_used    9538
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      46.10
_cell_measurement_theta_min      2.25
_cell_volume                     1398.82(10)
_computing_cell_refinement       'Bruker SAINT-Plus v7.66A'
_computing_data_collection       'Bruker APEX2 v2009.7-0'
_computing_data_reduction        'Bruker SAINT-Plus v7.66A'
_computing_molecular_graphics    'Bruker XP v5.1'
_computing_publication_material  'Bruker XCIF 2008'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       'ω scans; 23 settings'
_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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            108791
_diffrn_reflns_theta_full        49.35
_diffrn_reflns_theta_max         49.35
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    2.290
_exptl_absorpt_correction_T_max  0.7497
_exptl_absorpt_correction_T_min  0.6272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1, Bruker-AXS, Madison, WI'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_refine_diff_density_max         4.186
_refine_diff_density_min         -2.302
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.373
_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     349
_refine_ls_number_reflns         28016
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.373
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/s²(Fo²)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0591
_refine_ls_wR_factor_ref         0.0592
_reflns_number_gt                27766
_reflns_number_total             28016
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja100574n_si_002.cif
_cod_data_source_block           ajmm49
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct methods' was changed to
'direct'.

'_atom_sites_solution_secondary' value 'Difference Fourier map' was
changed to 'difmap'.

'_atom_sites_solution_hydrogens' value 'Geometric positions' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4102033
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
Re1 Re 0.5000 0.5000 0.5000 0.01336(1) Uani 1 2 d S . .
P1 P 0.52336(3) 0.59646(2) 0.356801(15) 0.01603(3) Uani 1 1 d . . .
O1 O 0.6268(3) 0.2696(2) 0.45001(13) 0.1043(10) Uani 1 1 d . . .
O2 O 0.19773(17) 0.29359(18) 0.39635(10) 0.0800(6) Uani 1 1 d . . .
O3 O 0.58247(13) 0.25938(8) 0.13995(6) 0.0329(2) Uani 1 1 d . . .
B1 B 0.41523(19) 0.27724(11) 0.13664(8) 0.0297(3) Uani 1 1 d . . .
C1 C 0.5863(2) 0.35666(17) 0.46883(10) 0.0452(4) Uani 1 1 d . . .
C2 C 0.30493(15) 0.37188(15) 0.43440(9) 0.0390(3) Uani 1 1 d . . .
C3 C 0.67130(12) 0.75359(10) 0.37232(8) 0.02410(17) Uani 1 1 d . . .
C4 C 0.80391(17) 0.7563(2) 0.35395(14) 0.0488(4) Uani 1 1 d . . .
H4 H 0.8201 0.6748 0.3335 0.059 Uiso 1 1 calc R . .
C5 C 0.9140(2) 0.8784(3) 0.36538(18) 0.0699(7) Uani 1 1 d . . .
H5 H 1.0045 0.8795 0.3521 0.084 Uiso 1 1 calc R . .
C6 C 0.8929(2) 0.9963(2) 0.39551(15) 0.0615(6) Uani 1 1 d . . .
H6 H 0.9683 1.0790 0.4030 0.074 Uiso 1 1 calc R . .
C7 C 0.7643(2) 0.99455(15) 0.41456(17) 0.0586(5) Uani 1 1 d . . .
H7 H 0.7501 1.0764 0.4362 0.070 Uiso 1 1 calc R . .
C8 C 0.65186(17) 0.87348(13) 0.40268(14) 0.0429(3) Uani 1 1 d . . .
H8 H 0.5616 0.8739 0.4156 0.051 Uiso 1 1 calc R . .
C9 C 0.36807(13) 0.64782(11) 0.29010(8) 0.02666(18) Uani 1 1 d . . .
C10 C 0.3824(2) 0.71529(14) 0.21245(9) 0.0426(3) Uani 1 1 d . . .
H10 H 0.4714 0.7313 0.1942 0.051 Uiso 1 1 calc R . .
C11 C 0.2671(3) 0.75901(18) 0.16182(13) 0.0633(6) Uani 1 1 d . . .
H11 H 0.2770 0.8026 0.1081 0.076 Uiso 1 1 calc R . .
C12 C 0.1402(3) 0.7403(2) 0.1881(2) 0.0792(9) Uani 1 1 d . . .
H12 H 0.0628 0.7727 0.1541 0.095 Uiso 1 1 calc R . .
C13 C 0.1255(2) 0.6749(3) 0.2632(3) 0.0839(10) Uani 1 1 d . . .
H13 H 0.0364 0.6610 0.2811 0.101 Uiso 1 1 calc R . .
C14 C 0.23812(16) 0.62735(19) 0.31512(15) 0.0503(4) Uani 1 1 d . . .
H14 H 0.2250 0.5811 0.3674 0.060 Uiso 1 1 calc R . .
C15 C 0.55600(14) 0.48677(10) 0.26987(7) 0.02453(18) Uani 1 1 d . . .
H15A H 0.5672 0.5356 0.2153 0.029 Uiso 1 1 calc R . .
H15B H 0.6493 0.4650 0.2967 0.029 Uiso 1 1 calc R . .
C16 C 0.42999(16) 0.35460(10) 0.23728(7) 0.0303(2) Uani 1 1 d . . .
H16A H 0.3358 0.3748 0.2350 0.036 Uiso 1 1 calc R . .
H16B H 0.4435 0.2920 0.2848 0.036 Uiso 1 1 calc R . .
C17 C 0.30420(18) 0.12597(10) 0.11560(8) 0.0339(3) Uani 1 1 d . . .
H17 H 0.3363 0.0747 0.1682 0.041 Uiso 1 1 calc R . .
C18 C 0.14967(19) 0.13782(12) 0.11462(9) 0.0380(3) Uani 1 1 d . . .
H18A H 0.0785 0.0466 0.0985 0.046 Uiso 1 1 calc R . .
H18B H 0.1519 0.1717 0.1783 0.046 Uiso 1 1 calc R . .
C19 C 0.0934(2) 0.23138(13) 0.04595(10) 0.0397(3) Uani 1 1 d . . .
H19A H 0.0094 0.2530 0.0625 0.048 Uiso 1 1 calc R . .
H19B H 0.0560 0.1817 -0.0176 0.048 Uiso 1 1 calc R . .
C20 C 0.20978(19) 0.36508(12) 0.04392(9) 0.0360(3) Uani 1 1 d . . .
H20A H 0.1735 0.4041 -0.0136 0.043 Uiso 1 1 calc R . .
H20B H 0.2181 0.4292 0.0976 0.043 Uiso 1 1 calc R . .
C21 C 0.36546(17) 0.35367(10) 0.04729(8) 0.0306(2) Uani 1 1 d . . .
H21 H 0.4349 0.4467 0.0570 0.037 Uiso 1 1 calc R . .
C22 C 0.36985(19) 0.27936(11) -0.04367(8) 0.0363(3) Uani 1 1 d . . .
H22A H 0.3287 0.3243 -0.0968 0.044 Uiso 1 1 calc R . .
H22B H 0.4741 0.2891 -0.0418 0.044 Uiso 1 1 calc R . .
C23 C 0.2852(2) 0.12830(11) -0.06200(9) 0.0406(4) Uani 1 1 d . . .
H23A H 0.3162 0.0853 -0.1112 0.049 Uiso 1 1 calc R . .
H23B H 0.1786 0.1187 -0.0860 0.049 Uiso 1 1 calc R . .
C24 C 0.3088(2) 0.05228(11) 0.02448(9) 0.0387(3) Uani 1 1 d . . .
H24A H 0.4056 0.0340 0.0349 0.046 Uiso 1 1 calc R . .
H24B H 0.2321 -0.0359 0.0110 0.046 Uiso 1 1 calc R . .
C25 C 0.7013(2) 0.36082(13) 0.11655(10) 0.0381(3) Uani 1 1 d . . .
H25A H 0.6832 0.4504 0.1182 0.046 Uiso 1 1 calc R . .
H25B H 0.7088 0.3352 0.0535 0.046 Uiso 1 1 calc R . .
C26 C 0.8428(2) 0.36382(17) 0.19090(14) 0.0489(4) Uani 1 1 d . . .
H26A H 0.9300 0.3884 0.1659 0.059 Uiso 1 1 calc R . .
H26B H 0.8593 0.4278 0.2465 0.059 Uiso 1 1 calc R . .
C27 C 0.8097(2) 0.21892(17) 0.21338(13) 0.0474(4) Uani 1 1 d . . .
H27A H 0.8708 0.2125 0.2759 0.057 Uiso 1 1 calc R . .
H27B H 0.8275 0.1595 0.1663 0.057 Uiso 1 1 calc R . .
C28 C 0.6472(2) 0.18190(14) 0.21055(11) 0.0412(3) Uani 1 1 d . . .
H28A H 0.6004 0.0838 0.1925 0.049 Uiso 1 1 calc R . .
H28B H 0.6345 0.2071 0.2722 0.049 Uiso 1 1 calc R . .
B2 B 0.9772(3) 0.4397(4) 0.4887(3) 0.0365(6) Uani 0.50 1 d P . .
F1 F 0.8569(3) 0.4842(3) 0.4623(3) 0.0797(10) Uani 0.50 1 d P . .
F2 F 0.9290(4) 0.3035(3) 0.4893(4) 0.1209(18) Uani 0.50 1 d P . .
F3 F 1.0636(4) 0.4693(6) 0.4351(4) 0.145(2) Uani 0.50 1 d P . .
F4 F 1.0567(5) 0.4993(3) 0.5779(2) 0.0928(13) Uani 0.50 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'
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'
Re Re -1.0185 7.2310 '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 Re1 C1 179.999(1) . 2_666 yes
C1 Re1 C2 93.65(9) . 2_666 yes
C1 Re1 C2 86.35(9) 2_666 2_666 yes
C1 Re1 C2 86.35(9) . . yes
C1 Re1 C2 93.65(9) 2_666 . yes
C2 Re1 C2 180.00(8) 2_666 . yes
C1 Re1 P1 89.04(3) . 2_666 yes
C1 Re1 P1 90.96(3) 2_666 2_666 yes
C2 Re1 P1 91.43(3) 2_666 2_666 yes
C2 Re1 P1 88.57(3) . 2_666 yes
C1 Re1 P1 90.96(3) . . yes
C1 Re1 P1 89.04(3) 2_666 . yes
C2 Re1 P1 88.57(3) 2_666 . yes
C2 Re1 P1 91.43(3) . . yes
P1 Re1 P1 180.0 2_666 . yes
C9 P1 C3 100.32(5) . . ?
C9 P1 C15 102.77(6) . . ?
C3 P1 C15 104.49(5) . . ?
C9 P1 Re1 117.29(4) . . ?
C3 P1 Re1 114.95(4) . . ?
C15 P1 Re1 115.03(3) . . ?
C25 O3 C28 109.26(13) . . ?
C25 O3 B1 124.75(9) . . ?
C28 O3 B1 118.78(9) . . ?
C17 B1 C21 106.61(11) . . ?
C17 B1 C16 113.80(8) . . ?
C21 B1 C16 115.66(9) . . ?
C17 B1 O3 105.54(10) . . ?
C21 B1 O3 108.07(8) . . ?
C16 B1 O3 106.59(11) . . ?
O1 C1 Re1 175.7(2) . . ?
O2 C2 Re1 176.1(2) . . ?
C8 C3 C4 118.41(12) . . ?
C8 C3 P1 119.93(9) . . ?
C4 C3 P1 121.66(11) . . ?
C3 C4 C5 120.21(19) . . ?
C6 C5 C4 120.61(19) . . ?
C7 C6 C5 119.65(14) . . ?
C6 C7 C8 120.69(18) . . ?
C3 C8 C7 120.43(16) . . ?
C14 C9 C10 118.36(13) . . ?
C14 C9 P1 122.58(10) . . ?
C10 C9 P1 119.02(12) . . ?
C11 C10 C9 120.24(19) . . ?
C12 C11 C10 120.90(18) . . ?
C13 C12 C11 119.19(18) . . ?
C12 C13 C14 121.6(2) . . ?
C9 C14 C13 119.65(19) . . ?
C16 C15 P1 112.43(7) . . ?
C15 C16 B1 116.16(8) . . ?
C18 C17 C24 113.54(13) . . ?
C18 C17 B1 107.13(10) . . ?
C24 C17 B1 111.21(9) . . ?
C19 C18 C17 114.65(10) . . ?
C18 C19 C20 114.90(14) . . ?
C21 C20 C19 115.60(12) . . ?
C22 C21 C20 112.34(12) . . ?
C22 C21 B1 111.60(10) . . ?
C20 C21 B1 107.16(9) . . ?
C23 C22 C21 115.11(8) . . ?
C22 C23 C24 114.20(11) . . ?
C23 C24 C17 115.48(10) . . ?
O3 C25 C26 105.54(12) . . ?
C27 C26 C25 101.93(14) . . ?
C26 C27 C28 103.45(15) . . ?
O3 C28 C27 105.02(11) . . ?
B2 B2 F4 69.2(4) 2_766 2_766 ?
B2 B2 F3 81.6(4) 2_766 . ?
F4 B2 F3 60.8(4) 2_766 . ?
B2 B2 F1 75.3(3) 2_766 . ?
F4 B2 F1 51.9(3) 2_766 . ?
F3 B2 F1 112.7(4) . . ?
B2 B2 F2 163.8(6) 2_766 . ?
F4 B2 F2 125.4(4) 2_766 . ?
F3 B2 F2 110.9(5) . . ?
F1 B2 F2 107.5(3) . . ?
B2 B2 F4 55.9(3) 2_766 . ?
F4 B2 F4 125.1(3) 2_766 . ?
F3 B2 F4 107.7(3) . . ?
F1 B2 F4 108.9(4) . . ?
F2 B2 F4 109.1(4) . . ?
B2 B2 F1 56.4(3) 2_766 2_766 ?
F4 B2 F1 104.9(3) 2_766 2_766 ?
F3 B2 F1 63.5(3) . 2_766 ?
F1 B2 F1 131.7(3) . 2_766 ?
F2 B2 F1 118.8(3) . 2_766 ?
F4 B2 F1 44.6(2) . 2_766 ?
B2 B2 F3 51.3(3) 2_766 2_766 ?
F4 B2 F3 97.0(4) 2_766 2_766 ?
F3 B2 F3 132.9(3) . 2_766 ?
F1 B2 F3 60.5(3) . 2_766 ?
F2 B2 F3 115.5(4) . 2_766 ?
F4 B2 F3 49.1(3) . 2_766 ?
F1 B2 F3 86.7(3) 2_766 2_766 ?
F4 F1 B2 58.3(3) 2_766 . ?
F4 F1 F3 107.8(3) 2_766 2_766 ?
B2 F1 F3 69.0(3) . 2_766 ?
F4 F1 B2 59.0(2) 2_766 2_766 ?
B2 F1 B2 48.3(3) . 2_766 ?
F3 F1 B2 49.3(2) 2_766 2_766 ?
F4 F3 B2 57.1(2) 2_766 . ?
F4 F3 F1 105.1(3) 2_766 2_766 ?
B2 F3 F1 67.2(3) . 2_766 ?
F4 F3 B2 55.1(2) 2_766 2_766 ?
B2 F3 B2 47.1(3) . 2_766 ?
F1 F3 B2 50.5(2) 2_766 2_766 ?
F1 F4 B2 69.8(3) 2_766 2_766 ?
F1 F4 F3 131.9(4) 2_766 2_766 ?
B2 F4 F3 62.1(4) 2_766 2_766 ?
F1 F4 B2 76.4(3) 2_766 . ?
B2 F4 B2 54.9(3) 2_766 . ?
F3 F4 B2 75.8(3) 2_766 . ?
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
Re1 C1 1.9832(13) . yes
Re1 C1 1.9832(13) 2_666 yes
Re1 C2 1.9902(11) 2_666 yes
Re1 C2 1.9903(11) . yes
Re1 P1 2.4324(2) 2_666 yes
Re1 P1 2.4324(2) . yes
P1 C9 1.8180(12) . ?
P1 C3 1.8267(10) . ?
P1 C15 1.8272(9) . ?
O1 C1 1.1270(18) . ?
O2 C2 1.1348(16) . ?
O3 C25 1.4689(15) . ?
O3 C28 1.4725(18) . ?
O3 B1 1.683(2) . ?
B1 C17 1.6156(16) . ?
B1 C21 1.6171(17) . ?
B1 C16 1.6240(15) . ?
C3 C8 1.3788(19) . ?
C3 C4 1.3832(19) . ?
C4 C5 1.397(2) . ?
C5 C6 1.366(4) . ?
C6 C7 1.352(3) . ?
C7 C8 1.400(2) . ?
C9 C14 1.377(2) . ?
C9 C10 1.3956(17) . ?
C10 C11 1.387(3) . ?
C11 C12 1.360(4) . ?
C12 C13 1.351(4) . ?
C13 C14 1.398(2) . ?
C15 C16 1.5397(16) . ?
C17 C18 1.544(2) . ?
C17 C24 1.5445(15) . ?
C18 C19 1.544(2) . ?
C19 C20 1.5467(17) . ?
C20 C21 1.546(2) . ?
C21 C22 1.5447(15) . ?
C22 C23 1.5379(16) . ?
C23 C24 1.5410(18) . ?
C25 C26 1.534(3) . ?
C26 C27 1.519(2) . ?
C27 C28 1.520(3) . ?
B2 B2 1.210(7) 2_766 ?
B2 F4 1.225(5) 2_766 ?
B2 F3 1.289(4) . ?
B2 F1 1.352(4) . ?
B2 F2 1.364(5) . ?
B2 F4 1.383(5) . ?
B2 F1 1.569(4) 2_766 ?
B2 F3 1.634(5) 2_766 ?
F1 F4 1.134(5) 2_766 ?
F1 F3 1.523(6) 2_766 ?
F1 B2 1.569(4) 2_766 ?
F3 F4 1.273(7) 2_766 ?
F3 F1 1.523(6) 2_766 ?
F3 B2 1.634(5) 2_766 ?
F4 F1 1.134(5) 2_766 ?
F4 B2 1.225(5) 2_766 ?
F4 F3 1.273(7) 2_766 ?
