#------------------------------------------------------------------------------
#$Date: 2016-03-25 22:21:48 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180009 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/03/7030322.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_7030322
loop_
_publ_author_name
'Jami, Ananda Kumar'
'Baskar, Viswanathan'
_publ_section_title
;
 Tetranuclear stiboxanes (RSb)4O6, exhibiting an adamantane-type
 structure.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12524
_journal_page_last               12529
_journal_paper_doi               10.1039/c2dt30587a
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C88 H72 Br4 N4 O10 Sb4'
_chemical_formula_sum            'C88 H72 Br4 N4 O10 Sb4'
_chemical_formula_weight         2152.14
_chemical_name_systematic
;
?
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                   19.226(9)
_cell_length_b                   19.226(9)
_cell_length_c                   21.370(19)
_cell_measurement_reflns_used    5782
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.13
_cell_measurement_theta_min      3.71
_cell_volume                     7899(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26544
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    3.440
_exptl_absorpt_correction_T_max  0.7248
_exptl_absorpt_correction_T_min  0.5182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   brukarsadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4208
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.237
_refine_diff_density_min         -1.289
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         3472
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0506
_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)+(0.0762P)²+108.0603P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1443
_reflns_number_gt                2956
_reflns_number_total             3472
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30587a.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'I4(1)/a '
_cod_database_code               7030322
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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
Br1 Br 0.20685(7) 0.49978(6) -0.12930(5) 0.0746(4) Uani 1 1 d .
C1 C 0.2317(4) 0.1876(4) 0.0667(3) 0.0324(15) Uani 1 1 d .
C2 C 0.1959(4) 0.1586(3) 0.0149(3) 0.0313(15) Uani 1 1 d .
C3 C 0.2321(4) 0.1165(4) -0.0235(4) 0.048(2) Uani 1 1 d .
H3 H 0.2110 0.0993 -0.0595 0.058 Uiso 1 1 calc R
C4 C 0.3006(5) 0.0983(5) -0.0101(6) 0.071(3) Uani 1 1 d .
H4 H 0.3239 0.0682 -0.0369 0.085 Uiso 1 1 calc R
C5 C 0.3344(5) 0.1230(6) 0.0408(6) 0.071(3) Uani 1 1 d .
H5 H 0.3800 0.1097 0.0487 0.085 Uiso 1 1 calc R
C6 C 0.3006(4) 0.1687(4) 0.0816(5) 0.050(2) Uani 1 1 d .
C7 C 0.3298(4) 0.1975(4) 0.1351(4) 0.046(2) Uani 1 1 d .
H7 H 0.3745 0.1853 0.1474 0.055 Uiso 1 1 calc R
C8 C 0.2923(4) 0.2436(4) 0.1693(4) 0.0386(17) Uani 1 1 d .
H8 H 0.3117 0.2635 0.2050 0.046 Uiso 1 1 calc R
C9 C 0.2250(4) 0.2613(4) 0.1513(3) 0.0306(15) Uani 1 1 d .
H9 H 0.2002 0.2935 0.1748 0.037 Uiso 1 1 calc R
C10 C 0.1289(4) 0.3273(4) 0.0036(3) 0.0302(15) Uani 1 1 d .
C11 C 0.1335(4) 0.3950(4) 0.0228(3) 0.0367(17) Uani 1 1 d .
H11 H 0.1204 0.4061 0.0634 0.044 Uiso 1 1 calc R
C12 C 0.1567(4) 0.4472(4) -0.0159(4) 0.0407(18) Uani 1 1 d .
H12 H 0.1595 0.4929 -0.0021 0.049 Uiso 1 1 calc R
C13 C 0.1753(4) 0.4297(4) -0.0750(4) 0.044(2) Uani 1 1 d .
C14 C 0.1684(5) 0.3635(5) -0.0979(4) 0.059(3) Uani 1 1 d .
H14 H 0.1798 0.3534 -0.1393 0.071 Uiso 1 1 calc R
C15 C 0.1441(5) 0.3118(5) -0.0580(4) 0.051(2) Uani 1 1 d .
H15 H 0.1380 0.2667 -0.0728 0.061 Uiso 1 1 calc R
C16 C 0.3314(14) 0.8291(15) -0.0068(13) 0.279(8) Uani 1 1 d DU
H16A H 0.2940 0.8615 -0.0129 0.418 Uiso 1 1 calc R
H16B H 0.3156 0.7909 0.0184 0.418 Uiso 1 1 calc R
H16C H 0.3468 0.8120 -0.0467 0.418 Uiso 1 1 calc R
C17 C 0.3889(11) 0.8640(13) 0.0246(9) 0.279(8) Uani 1 1 d DU
C18 C 0.3848(13) 0.9277(13) 0.0531(11) 0.279(8) Uani 1 1 d DU
H18 H 0.3434 0.9526 0.0535 0.334 Uiso 1 1 calc R
C19 C 0.4445(16) 0.9542(12) 0.0814(11) 0.279(8) Uani 1 1 d DU
H19 H 0.4434 0.9975 0.1009 0.334 Uiso 1 1 calc R
C20 C 0.5053(12) 0.9158(16) 0.0804(11) 0.279(8) Uani 1 1 d DU
H20 H 0.5451 0.9331 0.0995 0.334 Uiso 1 1 calc R
C21 C 0.5071(13) 0.8512(15) 0.0509(13) 0.279(8) Uani 1 1 d DU
H21 H 0.5483 0.8260 0.0504 0.334 Uiso 1 1 calc R
C22 C 0.4483(14) 0.8238(12) 0.0221(11) 0.279(8) Uani 1 1 d DU
H22 H 0.4490 0.7808 0.0022 0.334 Uiso 1 1 calc R
N1 N 0.1961(3) 0.2337(3) 0.1021(2) 0.0264(12) Uani 1 1 d .
O1 O 0.1294(2) 0.1760(2) 0.0063(2) 0.0283(10) Uani 1 1 d .
O2 O 0.0669(2) 0.1724(2) 0.11800(19) 0.0235(9) Uani 1 1 d .
O3 O 0.0000 0.2500 0.0236(3) 0.0262(13) Uani 1 2 d S
Sb1 Sb 0.08956(2) 0.25034(2) 0.064691(18) 0.02252(18) 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 0.0033 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'
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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
N1 C1 C6 121.2(7) . .
N1 C1 C2 116.7(6) . .
C6 C1 C2 122.1(7) . .
O1 C2 C3 124.2(7) . .
O1 C2 C1 118.3(6) . .
C3 C2 C1 117.4(7) . .
C2 C3 C4 121.0(8) . .
C2 C3 H3 119.5 . .
C4 C3 H3 119.5 . .
C5 C4 C3 122.1(8) . .
C5 C4 H4 119.0 . .
C3 C4 H4 119.0 . .
C4 C5 C6 119.9(8) . .
C4 C5 H5 120.0 . .
C6 C5 H5 120.0 . .
C7 C6 C5 125.2(8) . .
C7 C6 C1 117.6(8) . .
C5 C6 C1 117.2(8) . .
C8 C7 C6 119.3(7) . .
C8 C7 H7 120.3 . .
C6 C7 H7 120.3 . .
C7 C8 C9 120.3(7) . .
C7 C8 H8 119.9 . .
C9 C8 H8 119.9 . .
N1 C9 C8 121.4(7) . .
N1 C9 H9 119.3 . .
C8 C9 H9 119.3 . .
C11 C10 C15 118.6(7) . .
C11 C10 Sb1 120.3(5) . .
C15 C10 Sb1 120.8(6) . .
C10 C11 C12 122.3(7) . .
C10 C11 H11 118.8 . .
C12 C11 H11 118.8 . .
C13 C12 C11 117.7(8) . .
C13 C12 H12 121.1 . .
C11 C12 H12 121.1 . .
C12 C13 C14 122.5(7) . .
C12 C13 Br1 118.9(7) . .
C14 C13 Br1 118.5(6) . .
C13 C14 C15 118.5(8) . .
C13 C14 H14 120.7 . .
C15 C14 H14 120.7 . .
C10 C15 C14 120.0(8) . .
C10 C15 H15 120.0 . .
C14 C15 H15 120.0 . .
C17 C16 H16A 109.5 . .
C17 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C17 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C18 C17 C22 124.5(15) . .
C18 C17 C16 124.9(18) . .
C22 C17 C16 111(2) . .
C17 C18 C19 118.2(12) . .
C17 C18 H18 120.9 . .
C19 C18 H18 120.9 . .
C20 C19 C18 119.6(13) . .
C20 C19 H19 120.2 . .
C18 C19 H19 120.2 . .
C19 C20 C21 120.3(12) . .
C19 C20 H20 119.9 . .
C21 C20 H20 119.9 . .
C22 C21 C20 121.2(15) . .
C22 C21 H21 119.4 . .
C20 C21 H21 119.4 . .
C17 C22 C21 116.3(16) . .
C17 C22 H22 121.9 . .
C21 C22 H22 121.9 . .
C9 N1 C1 120.2(6) . .
C9 N1 Sb1 128.7(5) . .
C1 N1 Sb1 111.1(4) . .
C2 O1 Sb1 116.7(4) . .
Sb1 O2 Sb1 132.7(2) . 15
Sb1 O3 Sb1 126.0(3) 6_454 .
O2 Sb1 O3 93.67(17) . .
O2 Sb1 O2 92.73(16) . 12_666
O3 Sb1 O2 103.53(17) . 12_666
O2 Sb1 O1 84.41(18) . .
O3 Sb1 O1 93.09(17) . .
O2 Sb1 O1 163.29(18) 12_666 .
O2 Sb1 C10 171.1(2) . .
O3 Sb1 C10 92.3(2) . .
O2 Sb1 C10 92.2(2) 12_666 .
O1 Sb1 C10 88.7(2) . .
O2 Sb1 N1 83.37(19) . .
O3 Sb1 N1 169.79(16) . .
O2 Sb1 N1 86.40(19) 12_666 .
O1 Sb1 N1 76.92(19) . .
C10 Sb1 N1 89.6(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 C13 1.878(7) .
C1 N1 1.351(9) .
C1 C6 1.409(11) .
C1 C2 1.417(10) .
C2 O1 1.334(9) .
C2 C3 1.347(10) .
C3 C4 1.393(13) .
C3 H3 0.9300 .
C4 C5 1.353(14) .
C4 H4 0.9300 .
C5 C6 1.398(13) .
C5 H5 0.9300 .
C6 C7 1.389(12) .
C7 C8 1.355(12) .
C7 H7 0.9300 .
C8 C9 1.392(10) .
C8 H8 0.9300 .
C9 N1 1.302(9) .
C9 H9 0.9300 .
C10 C11 1.367(11) .
C10 C15 1.381(10) .
C10 Sb1 2.114(7) .
C11 C12 1.375(10) .
C11 H11 0.9300 .
C12 C13 1.355(11) .
C12 H12 0.9300 .
C13 C14 1.369(13) .
C14 C15 1.391(12) .
C14 H14 0.9300 .
C15 H15 0.9300 .
C16 C17 1.458(10) .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
C17 C18 1.370(9) .
C17 C22 1.380(10) .
C18 C19 1.393(9) .
C18 H18 0.9300 .
C19 C20 1.383(9) .
C19 H19 0.9300 .
C20 C21 1.393(9) .
C20 H20 0.9300 .
C21 C22 1.389(10) .
C21 H21 0.9300 .
C22 H22 0.9300 .
N1 Sb1 2.222(6) .
O1 Sb1 2.046(5) .
O2 Sb1 1.933(4) .
O2 Sb1 1.938(4) 15
O3 Sb1 1.933(3) 6_454
O3 Sb1 1.933(3) .
Sb1 O2 1.938(4) 12_666
