#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:21:30 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179373 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/70/4327095.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_4327095
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            'C42 H58 B Cl6 Ga I2 N6 S3'
_chemical_formula_weight         1290.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           198
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_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                   17.372(3)
_cell_length_b                   17.372(3)
_cell_length_c                   17.372(3)
_cell_measurement_reflns_used    9707
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.29
_cell_measurement_theta_min      2.34
_cell_volume                     5242.6(16)
_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      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            84700
_diffrn_reflns_theta_full        30.46
_diffrn_reflns_theta_max         30.46
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    2.164
_exptl_absorpt_correction_T_max  0.6714
_exptl_absorpt_correction_T_min  0.5629
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_description       block
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.146
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.002(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         5351
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0401
_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)+(0.0647P)²+6.9014P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1153
_reflns_number_gt                4762
_reflns_number_total             5351
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201504d_si_002_07.cif
_cod_data_source_block           198s10
_cod_original_cell_volume        5242.4(13)
_cod_database_code               4327095
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+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
Ga Ga 0.45823(2) 0.95823(2) 0.54177(2) 0.02442(14) Uani 1 3 d S . .
S S 0.57601(6) 0.90349(5) 0.52024(5) 0.02757(17) Uani 1 1 d . . .
I1 I 0.375363(16) 0.875363(16) 0.624637(16) 0.04653(15) Uani 1 3 d S . .
I2 I 0.575177(15) 0.924823(15) 0.075177(15) 0.03572(11) Uani 1 3 d S . .
B B 0.5767(2) 1.0767(2) 0.4233(2) 0.0287(12) Uani 1 3 d SD . .
H1 H 0.6132(7) 1.1132(7) 0.3868(7) 0.034 Uiso 1 3 d SD . .
C1 C 0.3791(3) 0.89111(19) 0.2151(18) 0.1054(13) Uani 0.693(4) 1 d PDU A 1
H1A H 0.4045 0.9095 0.2628 0.126 Uiso 0.693(4) 1 calc PR A 1
H1B H 0.4095 0.9101 0.1708 0.126 Uiso 0.693(4) 1 calc PR A 1
Cl1 Cl 0.37922(17) 0.78972(18) 0.21450(16) 0.0774(8) Uani 0.693(4) 1 d PD A 1
Cl2 Cl 0.2856(2) 0.92985(17) 0.21029(17) 0.0843(10) Uani 0.693(4) 1 d PD A 1
C2 C 0.2894(6) 0.8554(15) 0.2624(14) 0.100 Uiso 0.307(4) 1 d PD A 2
H2A H 0.2780 0.7997 0.2584 0.120 Uiso 0.307(4) 1 calc PR A 2
H2B H 0.2933 0.8684 0.3178 0.120 Uiso 0.307(4) 1 calc PR A 2
Cl3 Cl 0.2131(4) 0.9079(6) 0.2214(5) 0.102(3) Uani 0.307(4) 1 d PD A 2
Cl4 Cl 0.3783(4) 0.8743(6) 0.2177(9) 0.1036(7) Uani 0.307(4) 1 d PDU A 2
C11 C 0.5806(2) 0.9229(2) 0.42165(19) 0.0242(6) Uani 1 1 d . . .
N11 N 0.58129(19) 0.86929(18) 0.36472(17) 0.0258(6) Uani 1 1 d . . .
C12 C 0.5836(2) 0.9844(2) 0.3108(2) 0.0300(7) Uani 1 1 d . . .
H12A H 0.5845 1.0248 0.2739 0.036 Uiso 1 1 calc R . .
N12 N 0.58232(19) 0.99387(19) 0.38972(18) 0.0278(6) Uani 1 1 d . . .
C13 C 0.5836(2) 0.9083(2) 0.2946(2) 0.0304(8) Uani 1 1 d . . .
H13A H 0.5848 0.8857 0.2449 0.036 Uiso 1 1 calc R . .
C14 C 0.5783(2) 0.7827(2) 0.3714(2) 0.0255(6) Uani 1 1 d . . .
C15 C 0.6457(2) 0.7545(2) 0.4209(2) 0.0285(7) Uani 1 1 d . . .
H15A H 0.6428 0.7780 0.4727 0.034 Uiso 1 1 calc R . .
H15B H 0.6951 0.7700 0.3969 0.034 Uiso 1 1 calc R . .
C16 C 0.6419(2) 0.6655(2) 0.4276(3) 0.0352(8) Uani 1 1 d . . .
H16A H 0.6854 0.6465 0.4602 0.042 Uiso 1 1 calc R . .
C17 C 0.5655(3) 0.6424(3) 0.4637(3) 0.0400(9) Uani 1 1 d . . .
H17A H 0.5616 0.6648 0.5160 0.048 Uiso 1 1 calc R . .
H17B H 0.5630 0.5857 0.4685 0.048 Uiso 1 1 calc R . .
C18 C 0.4986(3) 0.6708(3) 0.4146(3) 0.0371(9) Uani 1 1 d . . .
H18A H 0.4488 0.6551 0.4389 0.045 Uiso 1 1 calc R . .
C19 C 0.5014(2) 0.7583(2) 0.4070(2) 0.0303(8) Uani 1 1 d . . .
H19A H 0.4956 0.7823 0.4584 0.036 Uiso 1 1 calc R . .
H19B H 0.4584 0.7761 0.3741 0.036 Uiso 1 1 calc R . .
C20 C 0.5848(2) 0.7473(3) 0.2906(2) 0.0332(8) Uani 1 1 d . . .
H20A H 0.6340 0.7631 0.2666 0.040 Uiso 1 1 calc R . .
H20B H 0.5421 0.7660 0.2579 0.040 Uiso 1 1 calc R . .
C21 C 0.6477(3) 0.6298(3) 0.3462(3) 0.0397(9) Uani 1 1 d . . .
H21A H 0.6973 0.6444 0.3222 0.048 Uiso 1 1 calc R . .
H21B H 0.6457 0.5730 0.3498 0.048 Uiso 1 1 calc R . .
C22 C 0.5049(3) 0.6352(3) 0.3333(3) 0.0421(10) Uani 1 1 d . . .
H22A H 0.5018 0.5784 0.3368 0.051 Uiso 1 1 calc R . .
H22B H 0.4617 0.6534 0.3008 0.051 Uiso 1 1 calc R . .
C23 C 0.5815(3) 0.6587(3) 0.2970(3) 0.0377(9) Uani 1 1 d . . .
H23A H 0.5855 0.6357 0.2444 0.045 Uiso 1 1 calc R . .
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
S Ga S 107.08(3) . 8_656
S Ga S 107.08(3) . 11_466
S Ga S 107.08(3) 8_656 11_466
S Ga I1 111.77(3) . .
S Ga I1 111.77(3) 8_656 .
S Ga I1 111.77(3) 11_466 .
C11 S Ga 96.96(12) . .
H1 B N12 106.4(3) . 11_466
H1 B N12 106.4(3) . 8_656
N12 B N12 112.4(2) 11_466 8_656
H1 B N12 106.4(3) . .
N12 B N12 112.4(2) 11_466 .
N12 B N12 112.4(2) 8_656 .
Cl2 C1 Cl1 112.5(2) . .
Cl3 C2 Cl4 112.7(3) . .
N12 C11 N11 109.0(3) . .
N12 C11 S 125.4(3) . .
N11 C11 S 125.6(3) . .
C11 N11 C13 107.6(3) . .
C11 N11 C14 128.8(3) . .
C13 N11 C14 123.5(3) . .
C13 C12 N12 108.8(3) . .
C11 N12 C12 107.4(3) . .
C11 N12 B 133.5(3) . .
C12 N12 B 118.9(3) . .
C12 C13 N11 107.1(3) . .
N11 C14 C19 109.7(3) . .
N11 C14 C15 109.6(3) . .
C19 C14 C15 110.5(3) . .
N11 C14 C20 109.0(3) . .
C19 C14 C20 108.9(3) . .
C15 C14 C20 109.1(3) . .
C14 C15 C16 109.1(3) . .
C17 C16 C21 109.2(4) . .
C17 C16 C15 109.3(3) . .
C21 C16 C15 109.1(4) . .
C16 C17 C18 110.4(4) . .
C17 C18 C19 110.3(4) . .
C17 C18 C22 109.2(4) . .
C19 C18 C22 108.5(4) . .
C18 C19 C14 109.8(3) . .
C14 C20 C23 109.3(3) . .
C23 C21 C16 109.4(4) . .
C23 C22 C18 109.3(4) . .
C21 C23 C22 109.9(4) . .
C21 C23 C20 110.0(4) . .
C22 C23 C20 109.2(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ga S 2.2870(10) .
Ga S 2.2870(10) 8_656
Ga S 2.2870(10) 11_466
Ga I1 2.4934(9) .
S C11 1.747(3) .
B H1 1.10(2) .
B N12 1.556(4) 11_466
B N12 1.556(4) 8_656
B N12 1.556(4) .
C1 Cl2 1.7608(11) .
C1 Cl1 1.7615(11) .
C2 Cl3 1.7601(11) .
C2 Cl4 1.7602(11) .
C11 N12 1.352(5) .
C11 N11 1.359(4) .
N11 C13 1.394(5) .
N11 C14 1.509(5) .
C12 C13 1.351(6) .
C12 N12 1.381(5) .
C14 C19 1.532(5) .
C14 C15 1.534(5) .
C14 C20 1.535(5) .
C15 C16 1.553(6) .
C16 C17 1.522(6) .
C16 C21 1.547(6) .
C17 C18 1.523(7) .
C18 C19 1.526(6) .
C18 C22 1.546(7) .
C20 C23 1.544(6) .
C21 C23 1.517(7) .
C22 C23 1.529(7) .
