#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:21:30 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179373 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/70/4327090.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_4327090
loop_
_publ_author_name
'Kevin Yurkerwich'
'Michael Yurkerwich'
'Gerard Parkin'
_publ_section_title
;
 Synthesis and Structural Characterization of
 Tris(2-mercapto-1-adamantylimidazolyl)hydroborato Complexes: A Sterically
 Demanding Tripodal [S3] Donor Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12284
_journal_page_last               12295
_journal_paper_doi               10.1021/ic201504d
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C24 H34 B N6 O3 Re S3'
_chemical_formula_weight         747.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   15.9998(8)
_cell_length_b                   15.9998(8)
_cell_length_c                   19.3190(10)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      32.36
_cell_measurement_theta_min      2.55
_cell_volume                     4283.0(4)
_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      125(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14958
_diffrn_reflns_theta_full        29.11
_diffrn_reflns_theta_max         29.11
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    4.513
_exptl_absorpt_correction_T_max  0.4655
_exptl_absorpt_correction_T_min  0.3011
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_description       block
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.022
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         2415
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0226
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0100P)²+10.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0480
_refine_ls_wR_factor_ref         0.0517
_reflns_number_gt                2139
_reflns_number_total             2415
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201504d_si_002_02.cif
_cod_data_source_block           ky312s10
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4327090
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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_group
Re1 Re 0.0000 0.0000 0.164786(12) 0.01845(10) Uani 0.5065(5) 3 d SP 1
S1 S 0.14443(7) 0.03882(7) 0.24011(5) 0.0213(2) Uani 0.5065(5) 1 d P 1
C1 C 0.0701(3) 0.1067(4) 0.1039(2) 0.0287(9) Uani 0.5065(5) 1 d P 1
O1 O 0.1094(3) 0.1668(3) 0.06336(19) 0.0431(9) Uani 0.5065(5) 1 d P 1
B1 B 0.0000 0.0000 0.3811(6) 0.020 Uiso 0.5065(5) 3 d SPD 1
H1 H 0.0000 0.0000 0.4372(12) 0.024 Uiso 0.5065(5) 3 d SPD 1
N11 N 0.0930(2) 0.0939(2) 0.35978(17) 0.0218(7) Uani 0.5065(5) 1 d PD 1
N12 N 0.2218(3) 0.2127(3) 0.31105(17) 0.0233(7) Uani 0.5065(5) 1 d P 1
C11 C 0.1529(3) 0.1177(3) 0.30485(19) 0.0196(7) Uani 0.5065(5) 1 d P 1
C12 C 0.1253(3) 0.1753(3) 0.4012(2) 0.0270(9) Uani 0.5065(5) 1 d P 1
H12A H 0.0969 0.1788 0.4435 0.032 Uiso 0.5065(5) 1 calc PR 1
C13 C 0.2039(3) 0.2486(3) 0.3711(2) 0.0266(9) Uani 0.5065(5) 1 d P 1
H13A H 0.2403 0.3129 0.3880 0.032 Uiso 0.5065(5) 1 calc PR 1
C14 C 0.3062(12) 0.2691(15) 0.2646(11) 0.019(3) Uani 0.5065(5) 1 d P 1
C15 C 0.2614(4) 0.2770(4) 0.1930(3) 0.0402(12) Uani 0.5065(5) 1 d P 1
H15A H 0.2209 0.3060 0.2008 0.060 Uiso 0.5065(5) 1 calc PR 1
H15B H 0.2222 0.2124 0.1731 0.060 Uiso 0.5065(5) 1 calc PR 1
H15C H 0.3137 0.3174 0.1609 0.060 Uiso 0.5065(5) 1 calc PR 1
C16 C 0.3622(4) 0.3751(4) 0.2917(3) 0.0388(11) Uani 0.5065(5) 1 d P 1
H16A H 0.3918 0.3767 0.3365 0.058 Uiso 0.5065(5) 1 calc PR 1
H16B H 0.3174 0.3995 0.2973 0.058 Uiso 0.5065(5) 1 calc PR 1
H16C H 0.4126 0.4155 0.2585 0.058 Uiso 0.5065(5) 1 calc PR 1
C17 C 0.3712(11) 0.2277(14) 0.2605(11) 0.040(4) Uani 0.5065(5) 1 d P 1
H17A H 0.3959 0.2269 0.3068 0.060 Uiso 0.5065(5) 1 calc PR 1
H17B H 0.4253 0.2672 0.2296 0.060 Uiso 0.5065(5) 1 calc PR 1
H17C H 0.3351 0.1616 0.2426 0.060 Uiso 0.5065(5) 1 calc PR 1
Re2 Re 0.0000 0.0000 0.362957(12) 0.01551(9) Uani 0.4935(5) 3 d SP 2
S2 S 0.14662(7) 0.04422(7) 0.28840(5) 0.0191(2) Uani 0.4935(5) 1 d P 2
C2 C 0.0720(3) 0.1087(3) 0.4224(2) 0.0219(8) Uani 0.4935(5) 1 d P 2
O2 O 0.1131(3) 0.1707(2) 0.46116(17) 0.0321(7) Uani 0.4935(5) 1 d P 2
B2 B 0.0000 0.0000 0.1472(6) 0.020 Uiso 0.4935(5) 3 d SPD 2
H2 H 0.0000 0.0000 0.0921(12) 0.024 Uiso 0.4935(5) 3 d SPD 2
N21 N 0.0904(2) 0.0962(2) 0.16963(16) 0.0197(6) Uani 0.4935(5) 1 d PD 2
N22 N 0.2203(2) 0.2171(3) 0.21624(18) 0.0204(7) Uani 0.4935(5) 1 d P 2
C21 C 0.1517(3) 0.1215(3) 0.22382(19) 0.0178(7) Uani 0.4935(5) 1 d P 2
C22 C 0.1197(3) 0.1765(3) 0.1283(2) 0.0240(8) Uani 0.4935(5) 1 d P 2
H22A H 0.0890 0.1789 0.0869 0.029 Uiso 0.4935(5) 1 calc PR 2
C23 C 0.1992(3) 0.2510(3) 0.1565(2) 0.0255(9) Uani 0.4935(5) 1 d P 2
H23A H 0.2342 0.3148 0.1387 0.031 Uiso 0.4935(5) 1 calc PR 2
C24 C 0.3045(13) 0.2812(17) 0.2586(11) 0.024(4) Uani 0.4935(5) 1 d P 2
C25 C 0.2733(4) 0.2798(4) 0.3347(3) 0.0374(11) Uani 0.4935(5) 1 d P 2
H25A H 0.2318 0.3085 0.3375 0.056 Uiso 0.4935(5) 1 calc PR 2
H25B H 0.3307 0.3170 0.3636 0.056 Uiso 0.4935(5) 1 calc PR 2
H25C H 0.2377 0.2130 0.3513 0.056 Uiso 0.4935(5) 1 calc PR 2
C26 C 0.3615(4) 0.3797(3) 0.2331(3) 0.0338(10) Uani 0.4935(5) 1 d P 2
H26A H 0.3803 0.3787 0.1850 0.051 Uiso 0.4935(5) 1 calc PR 2
H26B H 0.4195 0.4150 0.2617 0.051 Uiso 0.4935(5) 1 calc PR 2
H26C H 0.3230 0.4118 0.2356 0.051 Uiso 0.4935(5) 1 calc PR 2
C27 C 0.3714(11) 0.2354(13) 0.2542(11) 0.034(3) Uani 0.4935(5) 1 d P 2
H27A H 0.3900 0.2351 0.2059 0.051 Uiso 0.4935(5) 1 calc PR 2
H27B H 0.3364 0.1690 0.2717 0.051 Uiso 0.4935(5) 1 calc PR 2
H27C H 0.4293 0.2735 0.2823 0.051 Uiso 0.4935(5) 1 calc PR 2
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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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
C1 Re1 C1 86.0(2) . 2
C1 Re1 C1 86.0(2) . 3
C1 Re1 C1 86.0(2) 2 3
C1 Re1 S1 94.52(13) . .
C1 Re1 S1 175.21(13) 2 .
C1 Re1 S1 89.30(14) 3 .
C1 Re1 S1 89.30(14) . 2
C1 Re1 S1 94.52(13) 2 2
C1 Re1 S1 175.21(13) 3 2
S1 Re1 S1 90.25(3) . 2
C1 Re1 S1 175.21(13) . 3
C1 Re1 S1 89.30(14) 2 3
C1 Re1 S1 94.52(13) 3 3
S1 Re1 S1 90.25(3) . 3
S1 Re1 S1 90.25(3) 2 3
C11 S1 Re1 108.82(13) . .
O1 C1 Re1 175.3(4) . .
H1 B1 N11 105.4(4) . 3
H1 B1 N11 105.4(4) . 2
N11 B1 N11 113.2(4) 3 2
H1 B1 N11 105.4(4) . .
N11 B1 N11 113.2(4) 3 .
N11 B1 N11 113.2(4) 2 .
C11 N11 C12 108.1(3) . .
C11 N11 B1 133.1(5) . .
C12 N11 B1 118.8(4) . .
C11 N12 C13 108.4(3) . .
C11 N12 C14 127.1(7) . .
C13 N12 C14 124.4(7) . .
N11 C11 N12 108.0(3) . .
N11 C11 S1 125.2(3) . .
N12 C11 S1 126.8(3) . .
C13 C12 N11 108.3(4) . .
C12 C13 N12 107.2(4) . .
N12 C14 C17 112.7(18) . .
N12 C14 C16 108.0(11) . .
C17 C14 C16 110.6(12) . .
N12 C14 C15 105.3(10) . .
C17 C14 C15 115.6(14) . .
C16 C14 C15 104.1(15) . .
C2 Re2 C2 87.78(17) . 3
C2 Re2 C2 87.78(17) . 2
C2 Re2 C2 87.78(17) 3 2
C2 Re2 S2 91.99(13) . .
C2 Re2 S2 89.36(13) 3 .
C2 Re2 S2 177.13(13) 2 .
C2 Re2 S2 177.13(12) . 3
C2 Re2 S2 91.99(13) 3 3
C2 Re2 S2 89.36(13) 2 3
S2 Re2 S2 90.87(3) . 3
C2 Re2 S2 89.36(13) . 2
C2 Re2 S2 177.13(13) 3 2
C2 Re2 S2 91.99(13) 2 2
S2 Re2 S2 90.87(3) . 2
S2 Re2 S2 90.87(3) 3 2
C21 S2 Re2 108.43(13) . .
O2 C2 Re2 176.2(4) . .
H2 B2 N21 106.2(5) . .
H2 B2 N21 106.2(5) . 2
N21 B2 N21 112.5(4) . 2
H2 B2 N21 106.2(5) . 3
N21 B2 N21 112.5(4) . 3
N21 B2 N21 112.5(4) 2 3
C21 N21 C22 108.2(3) . .
C21 N21 B2 133.5(5) . .
C22 N21 B2 118.3(5) . .
C21 N22 C23 108.0(3) . .
C21 N22 C24 131.4(11) . .
C23 N22 C24 120.6(11) . .
N21 C21 N22 107.9(3) . .
N21 C21 S2 125.3(3) . .
N22 C21 S2 126.8(3) . .
C23 C22 N21 108.7(4) . .
C22 C23 N22 107.3(4) . .
C26 C24 N22 115.3(17) . .
C26 C24 C27 106.4(13) . .
N22 C24 C27 104.2(13) . .
C26 C24 C25 111.0(13) . .
N22 C24 C25 110.0(12) . .
C27 C24 C25 109.5(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 C1 1.909(5) .
Re1 C1 1.909(5) 2
Re1 C1 1.909(5) 3
Re1 S1 2.5315(10) .
Re1 S1 2.5315(10) 2
Re1 S1 2.5315(10) 3
S1 C11 1.733(4) .
C1 O1 1.152(6) .
B1 H1 1.09(2) .
B1 N11 1.551(4) 3
B1 N11 1.551(4) 2
B1 N11 1.551(4) .
N11 C11 1.350(5) .
N11 C12 1.390(5) .
N12 C11 1.366(5) .
N12 C13 1.386(5) .
N12 C14 1.49(2) .
C12 C13 1.349(6) .
C14 C17 1.49(3) .
C14 C16 1.560(18) .
C14 C15 1.59(2) .
Re2 C2 1.914(4) .
Re2 C2 1.914(4) 3
Re2 C2 1.914(4) 2
Re2 S2 2.5334(10) .
Re2 S2 2.5335(10) 3
Re2 S2 2.5335(10) 2
S2 C21 1.729(4) .
C2 O2 1.151(5) .
B2 H2 1.06(2) .
B2 N21 1.557(5) .
B2 N21 1.557(5) 2
B2 N21 1.557(5) 3
N21 C21 1.351(5) .
N21 C22 1.380(5) .
N22 C21 1.373(5) .
N22 C23 1.387(5) .
N22 C24 1.468(19) .
C22 C23 1.348(6) .
C24 C26 1.46(2) .
C24 C27 1.57(3) .
C24 C25 1.55(2) .
