#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:24:52 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180077 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/23/7052384.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_7052384
loop_
_publ_author_name
'Sumby, Christopher J.'
'Carr, Michael J.'
'Franken, Andreas'
'Kennedy, John D.'
'Kilner, Colin A.'
'Hardie, Michaele J.'
_publ_section_title
;
 Crystal-packing motifs of [Ag4L4]4+ star-burst tetrahedra
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1390
_journal_paper_doi               10.1039/b609356f
_journal_volume                  30
_journal_year                    2006
_chemical_formula_sum            'C15 H33 B9 I N'
_chemical_formula_weight         451.61
_chemical_name_systematic
;
tetraethyleneammonium 1-phenyl-1-monocarba-6-iodo-undecaborane
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 104.5760(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1510(2)
_cell_length_b                   14.8907(3)
_cell_length_c                   17.1566(4)
_cell_measurement_temperature    150(2)
_cell_volume                     2262.60(9)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection
'DENZO-SMN and COLLECT (Otwinowski & Minor, 1996)'
_computing_data_reduction
'DENZO-SMN and COLLECT (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'X-Seed (Barbour)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
'Nonius KappaCCD area-detector diffractometer'
_diffrn_radiation_detector       'CCD plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Fine-focus Sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18685
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    1.415
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.5814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
?
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.139
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.07
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0382P)²+2.1210P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0839
_reflns_number_gt                4017
_reflns_number_total             4419
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B609356F.txt
_cod_data_source_block           Complex_(NEt4)_2
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7052384
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-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
I6 I 0.142748(19) 0.470768(12) 0.199482(11) 0.04143(9) Uani 1 1 d . . .
N20 N 0.1626(2) 0.24244(13) 0.44810(11) 0.0267(4) Uani 1 1 d . . .
C16 C 0.6715(3) 0.23317(17) 0.42951(15) 0.0302(5) Uani 1 1 d . . .
H16 H 0.6535 0.2045 0.3785 0.036 Uiso 1 1 calc . . .
B2 B 0.4714(3) 0.35684(18) 0.28046(16) 0.0268(5) Uani 1 1 d . . .
H2 H 0.4015 0.2945 0.277 0.032 Uiso 1 1 calc . . .
C1 C 0.6045(3) 0.38069(15) 0.35924(14) 0.0274(5) Uani 1 1 d . . .
C27 C 0.0396(3) 0.20920(17) 0.37713(15) 0.0326(5) Uani 1 1 d . . .
H27A H -0.0513 0.2468 0.3727 0.039 Uiso 1 1 calc . . .
H27B H 0.0129 0.147 0.3886 0.039 Uiso 1 1 calc . . .
C28 C 0.0793(4) 0.2099(2) 0.29622(16) 0.0433(7) Uani 1 1 d . . .
H28A H -0.0068 0.1876 0.2544 0.052 Uiso 1 1 calc . . .
H28B H 0.167 0.1712 0.299 0.052 Uiso 1 1 calc . . .
H28C H 0.1031 0.2714 0.2831 0.052 Uiso 1 1 calc . . .
C23 C 0.3041(3) 0.18520(18) 0.46006(17) 0.0350(6) Uani 1 1 d . . .
H23A H 0.3437 0.191 0.4117 0.042 Uiso 1 1 calc . . .
H23B H 0.3816 0.2095 0.5063 0.042 Uiso 1 1 calc . . .
B5 B 0.6703(3) 0.37248(19) 0.28056(16) 0.0288(6) Uani 1 1 d . . .
H5 H 0.7593 0.3221 0.2772 0.035 Uiso 1 1 calc . . .
C14 C 0.7431(3) 0.2234(2) 0.57430(17) 0.0449(7) Uani 1 1 d . . .
H14 H 0.7754 0.1889 0.6221 0.054 Uiso 1 1 calc . . .
C22 C 0.0835(3) 0.40639(18) 0.42186(18) 0.0419(7) Uani 1 1 d . . .
H22A H 0.1228 0.4656 0.4127 0.05 Uiso 1 1 calc . . .
H22B H 0.0447 0.4084 0.4701 0.05 Uiso 1 1 calc . . .
H22C H 0.0018 0.3896 0.3752 0.05 Uiso 1 1 calc . . .
C12 C 0.6759(3) 0.3655(2) 0.50937(16) 0.0410(6) Uani 1 1 d . . .
H12 H 0.6616 0.4283 0.5133 0.049 Uiso 1 1 calc . . .
C21 C 0.2087(3) 0.33780(17) 0.43350(17) 0.0347(6) Uani 1 1 d . . .
H21A H 0.2915 0.3565 0.4798 0.042 Uiso 1 1 calc . . .
H21B H 0.2491 0.338 0.3851 0.042 Uiso 1 1 calc . . .
C25 C 0.0966(3) 0.23792(18) 0.52084(15) 0.0329(5) Uani 1 1 d . . .
H25A H 0.0016 0.2729 0.5088 0.039 Uiso 1 1 calc . . .
H25B H 0.0704 0.1746 0.5288 0.039 Uiso 1 1 calc . . .
B7 B 0.5350(4) 0.5450(2) 0.2793(2) 0.0375(7) Uani 1 1 d . . .
H7 H 0.5266 0.618 0.2933 0.045 Uiso 1 1 calc . . .
C11 C 0.6514(3) 0.32544(17) 0.43372(14) 0.0293(5) Uani 1 1 d . . .
C15 C 0.7179(3) 0.1825(2) 0.49952(17) 0.0392(6) Uani 1 1 d . . .
H15 H 0.7324 0.1196 0.4961 0.047 Uiso 1 1 calc . . .
C26 C 0.1977(4) 0.2723(2) 0.59881(16) 0.0429(7) Uani 1 1 d . . .
H26A H 0.1453 0.2671 0.6419 0.051 Uiso 1 1 calc . . .
H26B H 0.2227 0.3354 0.5923 0.051 Uiso 1 1 calc . . .
H26C H 0.2908 0.2367 0.6127 0.051 Uiso 1 1 calc . . .
C24 C 0.2824(4) 0.08624(19) 0.47495(18) 0.0428(7) Uani 1 1 d . . .
H24A H 0.379 0.0548 0.4822 0.051 Uiso 1 1 calc . . .
H24B H 0.2086 0.0607 0.4287 0.051 Uiso 1 1 calc . . .
H24C H 0.2457 0.0793 0.5236 0.051 Uiso 1 1 calc . . .
B9 B 0.5229(3) 0.3996(2) 0.19227(17) 0.0317(6) Uani 1 1 d . . .
H9 H 0.505 0.357 0.1369 0.038 Uiso 1 1 calc . . .
B4 B 0.6793(4) 0.47480(19) 0.34230(19) 0.0336(6) Uani 1 1 d . . .
H4 H 0.7753 0.5058 0.3881 0.04 Uiso 1 1 calc . . .
B3 B 0.4805(4) 0.45972(19) 0.34258(19) 0.0331(6) Uani 1 1 d . . .
H3 H 0.4176 0.4787 0.3883 0.04 Uiso 1 1 calc . . .
C13 C 0.7209(4) 0.3144(2) 0.57885(17) 0.0487(8) Uani 1 1 d . . .
H13 H 0.7366 0.3425 0.63 0.058 Uiso 1 1 calc . . .
B6 B 0.3912(3) 0.46140(18) 0.23599(19) 0.0316(6) Uani 1 1 d . . .
B8 B 0.6706(4) 0.4828(2) 0.2359(2) 0.0374(7) Uani 1 1 d . . .
H8 H 0.7712 0.5066 0.2156 0.045 Uiso 1 1 calc . . .
B10 B 0.4956(4) 0.5119(2) 0.1807(2) 0.0408(7) Uani 1 1 d . . .
H10 H 0.4607 0.5528 0.1242 0.049 Uiso 1 1 calc . . .
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 0 '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'
I I -0.4742 1.8119 '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'
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
C27 N20 C25 106.04(18) . . ?
C27 N20 C21 110.67(18) . . ?
C25 N20 C21 111.17(19) . . ?
C27 N20 C23 111.09(19) . . ?
C25 N20 C23 111.46(19) . . ?
C21 N20 C23 106.49(19) . . ?
C11 C16 C15 120.4(3) . . ?
C1 B2 B6 107.74(19) . . ?
C1 B2 B9 108.8(2) . . ?
B6 B2 B9 60.47(16) . . ?
C1 B2 B5 55.42(15) . . ?
B6 B2 B5 100.88(19) . . ?
B9 B2 B5 59.28(15) . . ?
C1 B2 B3 54.71(15) . . ?
B6 B2 B3 59.06(16) . . ?
B9 B2 B3 101.88(19) . . ?
B5 B2 B3 89.63(18) . . ?
C11 C1 B3 126.5(2) . . ?
C11 C1 B2 126.2(2) . . ?
B3 C1 B2 70.30(17) . . ?
C11 C1 B5 126.0(2) . . ?
B3 C1 B5 107.5(2) . . ?
B2 C1 B5 69.20(17) . . ?
C11 C1 B4 126.1(2) . . ?
B3 C1 B4 69.27(19) . . ?
B2 C1 B4 107.7(2) . . ?
B5 C1 B4 69.62(18) . . ?
N20 C27 C28 115.5(2) . . ?
C24 C23 N20 115.1(2) . . ?
C1 B5 B9 109.1(2) . . ?
C1 B5 B8 109.0(2) . . ?
B9 B5 B8 61.44(17) . . ?
C1 B5 B2 55.38(15) . . ?
B9 B5 B2 59.70(15) . . ?
B8 B5 B2 102.82(19) . . ?
C1 B5 B4 55.26(15) . . ?
B9 B5 B4 102.30(19) . . ?
B8 B5 B4 59.33(17) . . ?
B2 B5 B4 90.37(18) . . ?
C13 C14 C15 119.5(3) . . ?
C13 C12 C11 120.6(3) . . ?
C22 C21 N20 114.9(2) . . ?
C26 C25 N20 115.5(2) . . ?
B10 B7 B4 111.3(2) . . ?
B10 B7 B3 111.6(2) . . ?
B4 B7 B3 60.64(17) . . ?
B10 B7 B6 56.69(18) . . ?
B4 B7 B6 101.01(19) . . ?
B3 B7 B6 59.33(17) . . ?
B10 B7 B8 56.85(19) . . ?
B4 B7 B8 59.27(17) . . ?
B3 B7 B8 101.7(2) . . ?
B6 B7 B8 89.0(2) . . ?
C16 C11 C12 118.6(2) . . ?
C16 C11 C1 121.0(2) . . ?
C12 C11 C1 120.4(2) . . ?
C14 C15 C16 120.3(3) . . ?
B10 B9 B5 112.2(2) . . ?
B10 B9 B2 112.6(2) . . ?
B5 B9 B2 61.02(15) . . ?
B10 B9 B6 57.10(18) . . ?
B5 B9 B6 101.53(19) . . ?
B2 B9 B6 59.67(16) . . ?
B10 B9 B8 57.14(18) . . ?
B5 B9 B8 59.58(16) . . ?
B2 B9 B8 102.43(19) . . ?
B6 B9 B8 89.27(19) . . ?
C1 B4 B8 109.0(2) . . ?
C1 B4 B7 109.2(2) . . ?
B8 B4 B7 61.35(18) . . ?
C1 B4 B3 55.15(15) . . ?
B8 B4 B3 102.6(2) . . ?
B7 B4 B3 59.87(17) . . ?
C1 B4 B5 55.13(15) . . ?
B8 B4 B5 59.46(16) . . ?
B7 B4 B5 102.3(2) . . ?
B3 B4 B5 89.96(18) . . ?
C1 B3 B6 108.0(2) . . ?
C1 B3 B7 109.3(2) . . ?
B6 B3 B7 60.57(17) . . ?
C1 B3 B4 55.59(16) . . ?
B6 B3 B4 101.1(2) . . ?
B7 B3 B4 59.49(17) . . ?
C1 B3 B2 54.98(14) . . ?
B6 B3 B2 59.10(15) . . ?
B7 B3 B2 102.3(2) . . ?
B4 B3 B2 90.04(19) . . ?
C14 C13 C12 120.5(3) . . ?
B10 B6 B3 113.6(2) . . ?
B10 B6 B2 113.3(2) . . ?
B3 B6 B2 61.84(15) . . ?
B10 B6 B9 57.69(18) . . ?
B3 B6 B9 103.43(19) . . ?
B2 B6 B9 59.86(15) . . ?
B10 B6 B7 58.17(19) . . ?
B3 B6 B7 60.10(17) . . ?
B2 B6 B7 103.94(19) . . ?
B9 B6 B7 91.6(2) . . ?
B10 B6 I6 120.13(19) . . ?
B3 B6 I6 117.39(19) . . ?
B2 B6 I6 117.06(17) . . ?
B9 B6 I6 131.06(18) . . ?
B7 B6 I6 131.10(18) . . ?
B10 B8 B4 112.0(2) . . ?
B10 B8 B5 111.4(2) . . ?
B4 B8 B5 61.22(16) . . ?
B10 B8 B9 56.92(17) . . ?
B4 B8 B9 101.9(2) . . ?
B5 B8 B9 58.98(16) . . ?
B10 B8 B7 57.51(19) . . ?
B4 B8 B7 59.37(18) . . ?
B5 B8 B7 102.2(2) . . ?
B9 B8 B7 90.1(2) . . ?
B6 B10 B9 65.21(19) . . ?
B6 B10 B8 99.2(2) . . ?
B9 B10 B8 65.94(18) . . ?
B6 B10 B7 65.1(2) . . ?
B9 B10 B7 100.3(2) . . ?
B8 B10 B7 65.6(2) . . ?
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
I6 B6 2.205(3) . ?
N20 C27 1.518(3) . ?
N20 C25 1.519(3) . ?
N20 C21 1.520(3) . ?
N20 C23 1.520(3) . ?
C16 C11 1.390(4) . ?
C16 C15 1.391(4) . ?
B2 C1 1.615(3) . ?
B2 B6 1.806(4) . ?
B2 B9 1.810(4) . ?
B2 B5 1.834(4) . ?
B2 B3 1.856(4) . ?
C1 C11 1.489(3) . ?
C1 B3 1.609(4) . ?
C1 B5 1.615(4) . ?
C1 B4 1.618(4) . ?
C27 C28 1.520(4) . ?
C23 C24 1.517(4) . ?
B5 B9 1.802(4) . ?
B5 B8 1.814(4) . ?
B5 B4 1.846(4) . ?
C14 C13 1.375(5) . ?
C14 C15 1.386(4) . ?
C22 C21 1.510(4) . ?
C12 C13 1.386(4) . ?
C12 C11 1.394(4) . ?
C25 C26 1.512(4) . ?
B7 B10 1.712(5) . ?
B7 B4 1.813(4) . ?
B7 B3 1.820(5) . ?
B7 B6 1.829(4) . ?
B7 B8 1.849(5) . ?
B9 B10 1.695(4) . ?
B9 B6 1.821(4) . ?
B9 B8 1.847(4) . ?
B4 B8 1.811(5) . ?
B4 B3 1.834(5) . ?
B3 B6 1.806(4) . ?
B6 B10 1.684(5) . ?
B8 B10 1.699(5) . ?
