#------------------------------------------------------------------------------
#$Date: 2015-07-05 12:16:25 +0300 (Sun, 05 Jul 2015) $
#$Revision: 140152 $
#$URL: svn://www.crystallography.net/cod/cif/4/03/10/4031078.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_4031078
loop_
_publ_author_name
'Kaleta, Jiří'
'Dron, Paul I.'
'Zhao, Ke'
'Shen, Yongqiang'
'Císařová, Ivana'
'Rogers, Charles T.'
'Michl, Josef'
_publ_section_title
;
 Arrays of Molecular Rotors with Triptycene Stoppers: Surface Inclusion in
 Hexagonal Tris(o-phenylenedioxy)cyclotriphosphazene.
;
_journal_issue                   12
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              6173
_journal_page_last               6192
_journal_paper_doi               10.1021/acs.joc.5b00661
_journal_volume                  80
_journal_year                    2015
_chemical_compound_source        'synthesized by Dr. Kaleta'
_chemical_formula_moiety         'C28 H14 Br4'
_chemical_formula_sum            'C28 H14 Br4'
_chemical_formula_weight         670.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.9662(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.7286(7)
_cell_length_b                   7.9945(2)
_cell_length_c                   13.6141(4)
_cell_measurement_reflns_used    3210
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.3655
_cell_measurement_theta_min      2.9929
_cell_volume                     2364.56(12)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2013.12.0.0'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8476
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.87
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.823
_exptl_absorpt_correction_T_max  0.5947
_exptl_absorpt_correction_T_min  0.1863
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.882
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0326
_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)+(0.0404P)²+3.9473P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0835
_reflns_number_gt                2113
_reflns_number_total             2709
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            jo5b00661_si_003.cif
_cod_data_source_block           JK513
_cod_depositor_comments
'Adding full bibliography for 4031076--4031079.cif.'
_cod_database_code               4031078
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Br1 Br 0.296019(17) 0.10278(5) 0.74352(2) 0.04608(14) Uani 1 1 d .
Br2 Br 0.2713(2) -0.0269(6) 0.5279(3) 0.0507(7) Uani 0.70(3) 1 d P
Br2B Br 0.2651(6) 0.009(4) 0.5194(10) 0.067(3) Uani 0.30(3) 1 d P
C1 C 0.32306(15) 0.0906(4) 0.6137(2) 0.0280(6) Uani 1 1 d .
C2 C 0.37659(13) 0.1532(4) 0.58894(19) 0.0234(6) Uani 1 1 d .
H2 H 0.4006 0.2042 0.6396 0.028 Uiso 1 1 calc R
C3 C 0.40191(13) 0.1516(4) 0.49277(19) 0.0224(6) Uani 1 1 d .
C4 C 0.42777(13) 0.1570(3) 0.41652(18) 0.0205(6) Uani 1 1 d .
C5 C 0.46486(12) 0.1590(3) 0.32791(17) 0.0170(5) Uani 1 1 d .
C6 C 0.52711(12) 0.2480(3) 0.34367(17) 0.0158(5) Uani 1 1 d .
C7 C 0.54593(13) 0.3295(3) 0.42875(18) 0.0202(6) Uani 1 1 d .
H7 H 0.5203 0.3311 0.4846 0.024 Uiso 1 1 calc R
C8 C 0.60302(14) 0.4092(4) 0.4315(2) 0.0263(6) Uani 1 1 d .
H8 H 0.6164 0.4651 0.4896 0.032 Uiso 1 1 calc R
C9 C 0.64007(14) 0.4075(4) 0.3507(2) 0.0269(6) Uani 1 1 d .
H9 H 0.6788 0.4623 0.3534 0.032 Uiso 1 1 calc R
C10 C 0.62113(13) 0.3255(4) 0.26426(19) 0.0227(6) Uani 1 1 d .
H10 H 0.6468 0.3236 0.2085 0.027 Uiso 1 1 calc R
C11 C 0.56470(12) 0.2478(3) 0.26188(17) 0.0158(5) Uani 1 1 d .
C12 C 0.48128(13) -0.0178(3) 0.29065(18) 0.0182(5) Uani 1 1 d .
C13 C 0.46074(14) -0.1661(4) 0.33092(19) 0.0238(6) Uani 1 1 d .
H13 H 0.4338 -0.1657 0.3852 0.029 Uiso 1 1 calc R
C14 C 0.48067(15) -0.3172(3) 0.2895(2) 0.0280(7) Uani 1 1 d .
H14 H 0.4673 -0.4205 0.3164 0.034 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'
Br Br -0.2901 2.4595 '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
C2 C1 Br2 124.0(3) . .
C2 C1 Br1 121.0(2) . .
Br2 C1 Br1 114.9(2) . .
C2 C1 Br2B 122.5(4) . .
Br2 C1 Br2B 10.2(9) . .
Br1 C1 Br2B 116.1(4) . .
C1 C2 C3 126.0(3) . .
C1 C2 H2 117.0 . .
C3 C2 H2 117.0 . .
C4 C3 C2 173.9(3) . .
C3 C4 C5 174.6(3) . .
C4 C5 C6 112.6(2) . .
C4 C5 C11 115.5(2) . 2_655
C6 C5 C11 104.50(19) . 2_655
C4 C5 C12 113.2(2) . .
C6 C5 C12 105.1(2) . .
C11 C5 C12 104.82(19) 2_655 .
C7 C6 C11 120.0(3) . .
C7 C6 C5 125.5(2) . .
C11 C6 C5 114.4(2) . .
C6 C7 C8 119.2(2) . .
C6 C7 H7 120.4 . .
C8 C7 H7 120.4 . .
C9 C8 C7 120.5(3) . .
C9 C8 H8 119.8 . .
C7 C8 H8 119.8 . .
C8 C9 C10 120.6(3) . .
C8 C9 H9 119.7 . .
C10 C9 H9 119.7 . .
C11 C10 C9 118.7(2) . .
C11 C10 H10 120.7 . .
C9 C10 H10 120.7 . .
C10 C11 C6 121.1(2) . .
C10 C11 C5 125.8(2) . 2_655
C6 C11 C5 113.1(2) . 2_655
C13 C12 C12 120.98(16) . 2_655
C13 C12 C5 125.2(2) . .
C12 C12 C5 113.85(13) 2_655 .
C12 C13 C14 118.3(3) . .
C12 C13 H13 120.8 . .
C14 C13 H13 120.8 . .
C14 C14 C13 120.66(17) 2_655 .
C14 C14 H14 119.7 2_655 .
C13 C14 H14 119.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 C1 1.874(3) .
Br2 C1 1.863(5) .
Br2B C1 1.899(11) .
C1 C2 1.315(4) .
C2 C3 1.429(4) .
C2 H2 0.9500 .
C3 C4 1.189(4) .
C4 C5 1.462(3) .
C5 C6 1.540(4) .
C5 C11 1.544(3) 2_655
C5 C12 1.545(4) .
C6 C7 1.385(3) .
C6 C11 1.392(3) .
C7 C8 1.395(4) .
C7 H7 0.9500 .
C8 C9 1.374(4) .
C8 H8 0.9500 .
C9 C10 1.403(4) .
C9 H9 0.9500 .
C10 C11 1.374(4) .
C10 H10 0.9500 .
C11 C5 1.544(3) 2_655
C12 C13 1.383(4) .
C12 C12 1.385(5) 2_655
C13 C14 1.405(4) .
C13 H13 0.9500 .
C14 C14 1.377(6) 2_655
C14 H14 0.9500 .
