#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:21:30 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179373 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/70/4327091.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_4327091
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            'C41 H56 B Cl4 I N6 S3 Zn'
_chemical_formula_weight         1073.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :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            12
_cell_length_a                   15.1780(6)
_cell_length_b                   15.1780(6)
_cell_length_c                   69.100(3)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      31.73
_cell_measurement_theta_min      2.68
_cell_volume                     13786.0(10)
_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 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0806
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       102
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            66759
_diffrn_reflns_theta_full        31.88
_diffrn_reflns_theta_max         31.88
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    1.613
_exptl_absorpt_correction_T_max  0.8554
_exptl_absorpt_correction_T_min  0.7711
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       block
_exptl_crystal_F_000             6576
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_platon_squeeze_details
; The unit cell contains 24 methylene chloride molecules which have been
treated as a diffuse contribution to the overall scattering without
specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.288
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         5154
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0381
_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)+(0.0550P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1161
_reflns_number_gt                3356
_reflns_number_total             5154
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201504d_si_002_03.cif
_cod_data_source_block           novap
_cod_original_cell_volume        13785.9(10)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4327091
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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
I I 0.6667 0.3333 -0.076831(4) 0.03014(10) Uani 1 3 d S
Zn Zn 0.6667 0.3333 -0.039738(6) 0.01584(11) Uani 1 3 d S
S S 0.69389(5) 0.48668(5) -0.025775(8) 0.01665(12) Uani 1 1 d .
B B 0.6667 0.3333 0.01353(6) 0.0160(8) Uani 1 3 d SD
H1 H 0.6667 0.3333 0.0293(3) 0.019 Uiso 1 3 d SD
N11 N 0.76015(15) 0.43650(15) 0.00731(3) 0.0155(4) Uani 1 1 d .
C11 C 0.78063(19) 0.49813(18) -0.00836(3) 0.0151(4) Uani 1 1 d .
C12 C 0.84905(18) 0.47244(19) 0.01781(3) 0.0172(5) Uani 1 1 d .
H12A H 0.8562 0.4440 0.0295 0.021 Uiso 1 1 calc R
N12 N 0.88099(16) 0.57093(15) -0.00759(3) 0.0154(4) Uani 1 1 d .
C13 C 0.92364(19) 0.55393(19) 0.00877(3) 0.0177(5) Uani 1 1 d .
H13A H 0.9926 0.5927 0.0128 0.021 Uiso 1 1 calc R
C14 C 0.94199(18) 0.64880(18) -0.02290(3) 0.0158(4) Uani 1 1 d .
C15 C 0.9434(2) 0.59309(19) -0.04126(3) 0.0191(5) Uani 1 1 d .
H15A H 0.8730 0.5493 -0.0460 0.023 Uiso 1 1 calc R
H15B H 0.9727 0.5492 -0.0384 0.023 Uiso 1 1 calc R
C16 C 1.0075(2) 0.6714(2) -0.05691(4) 0.0247(6) Uani 1 1 d .
H16A H 1.0075 0.6351 -0.0690 0.030 Uiso 1 1 calc R
C17 C 0.9610(2) 0.7386(2) -0.06113(4) 0.0261(6) Uani 1 1 d .
H17A H 0.8901 0.6959 -0.0657 0.031 Uiso 1 1 calc R
H17B H 1.0003 0.7879 -0.0715 0.031 Uiso 1 1 calc R
C18 C 0.9621(2) 0.7958(2) -0.04277(4) 0.0235(5) Uani 1 1 d .
H18A H 0.9328 0.8404 -0.0458 0.028 Uiso 1 1 calc R
C19 C 0.8980(2) 0.71965(19) -0.02695(4) 0.0201(5) Uani 1 1 d .
H19A H 0.8264 0.6790 -0.0313 0.024 Uiso 1 1 calc R
H19B H 0.8998 0.7565 -0.0150 0.024 Uiso 1 1 calc R
C20 C 1.1163(2) 0.7374(2) -0.04976(4) 0.0276(6) Uani 1 1 d .
H20A H 1.1576 0.7876 -0.0598 0.033 Uiso 1 1 calc R
H20B H 1.1470 0.6943 -0.0471 0.033 Uiso 1 1 calc R
C21 C 1.05195(19) 0.71444(19) -0.01563(4) 0.0211(5) Uani 1 1 d .
H21A H 1.0525 0.7500 -0.0036 0.025 Uiso 1 1 calc R
H21B H 1.0813 0.6705 -0.0127 0.025 Uiso 1 1 calc R
C22 C 1.0719(2) 0.8619(2) -0.03586(4) 0.0276(6) Uani 1 1 d .
H22A H 1.0737 0.9005 -0.0242 0.033 Uiso 1 1 calc R
H22B H 1.1130 0.9113 -0.0461 0.033 Uiso 1 1 calc R
C23 C 1.1162(2) 0.7929(2) -0.03121(4) 0.0256(5) Uani 1 1 d .
H23A H 1.1876 0.8354 -0.0264 0.031 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'
Zn Zn 0.2839 1.4301 '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 Zn S 104.40(2) . 3_665
S Zn S 104.40(2) . 2_655
S Zn S 104.40(2) 3_665 2_655
S Zn I 114.160(17) . .
S Zn I 114.164(17) 3_665 .
S Zn I 114.164(17) 2_655 .
C11 S Zn 97.64(8) . .
H1 B N11 106.01(17) . .
H1 B N11 106.02(17) . 2_655
N11 B N11 112.70(15) . 2_655
H1 B N11 106.02(17) . 3_665
N11 B N11 112.69(15) . 3_665
N11 B N11 112.69(15) 2_655 3_665
C11 N11 C12 107.7(2) . .
C11 N11 B 133.6(2) . .
C12 N11 B 118.1(2) . .
N11 C11 N12 107.7(2) . .
N11 C11 S 125.76(19) . .
N12 C11 S 126.51(18) . .
C13 C12 N11 109.1(2) . .
C11 N12 C13 108.45(19) . .
C11 N12 C14 127.31(19) . .
C13 N12 C14 123.7(2) . .
C12 C13 N12 107.0(2) . .
N12 C14 C15 108.72(19) . .
N12 C14 C21 108.66(18) . .
C15 C14 C21 108.6(2) . .
N12 C14 C19 111.20(19) . .
C15 C14 C19 111.32(19) . .
C21 C14 C19 108.3(2) . .
C14 C15 C16 109.5(2) . .
C20 C16 C17 109.5(2) . .
C20 C16 C15 109.8(2) . .
C17 C16 C15 108.9(2) . .
C16 C17 C18 110.0(2) . .
C22 C18 C17 109.3(2) . .
C22 C18 C19 110.2(2) . .
C17 C18 C19 109.9(2) . .
C18 C19 C14 108.7(2) . .
C16 C20 C23 109.4(2) . .
C23 C21 C14 109.6(2) . .
C18 C22 C23 108.8(2) . .
C20 C23 C22 108.7(2) . .
C20 C23 C21 109.5(2) . .
C22 C23 C21 110.5(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I Zn 2.5631(5) .
Zn S 2.3574(6) .
Zn S 2.3575(6) 3_665
Zn S 2.3575(6) 2_655
S C11 1.727(2) .
B H1 1.091(19) .
B N11 1.558(2) .
B N11 1.558(2) 2_655
B N11 1.558(2) 3_665
N11 C11 1.361(3) .
N11 C12 1.381(3) .
C11 N12 1.364(3) .
C12 C13 1.342(3) .
N12 C13 1.389(3) .
N12 C14 1.510(3) .
C14 C15 1.531(3) .
C14 C21 1.539(3) .
C14 C19 1.549(3) .
C15 C16 1.540(3) .
C16 C20 1.524(4) .
C16 C17 1.530(4) .
C17 C18 1.532(4) .
C18 C22 1.530(4) .
C18 C19 1.534(3) .
C20 C23 1.534(4) .
C21 C23 1.538(3) .
C22 C23 1.535(4) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 24 2 ' '
2 -0.333 0.333 0.083 538 146 ' '
3 0.000 0.000 0.250 534 146 ' '
4 0.333 0.667 0.417 538 146 ' '
5 0.000 0.000 0.500 24 2 ' '
6 -0.333 0.333 0.583 538 146 ' '
7 0.000 1.000 0.750 534 146 ' '
8 0.333 0.667 0.917 538 146 ' '
9 0.333 0.667 0.167 24 2 ' '
10 0.333 0.667 0.667 24 2 ' '
11 0.667 0.333 0.333 24 2 ' '
12 0.667 0.333 0.833 24 2 ' '
