#------------------------------------------------------------------------------
#$Date: 2017-09-13 05:08:25 +0300 (Wed, 13 Sep 2017) $
#$Revision: 200809 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/71/1547139.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_1547139
loop_
_publ_author_name
'Su, Yuanting'
'Li, Yongxin'
'Ganguly, Rakesh'
'Kinjo, Rei'
_publ_section_title
;
 Crystalline Boron-linked Tetraaminoethylene Radical Cations
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC03528D
_journal_year                    2017
_chemical_formula_sum            'C50 H54 B2 N4'
_chemical_formula_weight         732.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2017-05-08 deposited with the CCDC.
2017-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.914(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.662(3)
_cell_length_b                   17.724(3)
_cell_length_c                   16.037(3)
_cell_measurement_reflns_used    2187
_cell_measurement_temperature    103.(2)
_cell_measurement_theta_max      25.0391
_cell_measurement_theta_min      2.6659
_cell_volume                     4185.6(13)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX3 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2015)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XT, VERSION 2014/4'
_diffrn_ambient_temperature      103.(2)
_diffrn_detector_area_resol_mean 8.3333
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1729
_diffrn_reflns_av_unetI/netI     0.1719
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17039
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.80
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker KappaCCD'
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.268
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1922
_refine_ls_R_factor_gt           0.0782
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0616P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1728
_reflns_number_gt                1746
_reflns_number_total             3677
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7sc03528d2.cif
_cod_data_source_block           I_CCDC1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/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 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        4185.6(12)
_cod_database_code               1547139
loop_
_space_group_symop_operation_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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
B B1 0.1481(3) 0.9139(3) 0.8050(3) 0.0158(11) Uani d . . . 1
C C1 0.2534(3) 0.9141(2) 0.8419(2) 0.0144(9) Uani d . . . 1
C C2 0.3041(3) 0.8505(2) 0.8360(3) 0.0216(10) Uani d . . . 1
H H2 0.2728 0.8054 0.8115 0.026 Uiso calc U . R 1
C C3 0.3977(3) 0.8508(2) 0.8643(3) 0.0245(11) Uani d . . . 1
H H3 0.4295 0.8063 0.8593 0.029 Uiso calc U . R 1
C C4 0.4453(3) 0.9148(2) 0.8996(3) 0.0219(10) Uani d . . . 1
H H4 0.5097 0.9152 0.9182 0.026 Uiso calc U . R 1
C C5 0.3987(3) 0.9790(2) 0.9081(3) 0.0233(10) Uani d . . . 1
H H5 0.4312 1.0234 0.9334 0.028 Uiso calc U . R 1
C C6 0.3047(3) 0.9785(2) 0.8795(2) 0.0194(10) Uani d . . . 1
H H6 0.2737 1.0231 0.8856 0.023 Uiso calc U . R 1
C C7 0.1083(3) 0.7690(2) 0.8008(2) 0.0130(9) Uani d . . . 1
C C8 0.1203(3) 0.7423(2) 0.8863(2) 0.0149(10) Uani d . . . 1
C C9 0.1238(3) 0.7951(2) 0.9609(2) 0.0239(11) Uani d . . . 1
H H9A 0.1818 0.8221 0.9802 0.036 Uiso calc U . R 1
H H9B 0.1179 0.7661 1.0107 0.036 Uiso calc U . R 1
H H9C 0.0738 0.8315 0.9404 0.036 Uiso calc U . R 1
C C10 0.1315(3) 0.6647(2) 0.9022(3) 0.0187(10) Uani d . . . 1
H H10 0.1393 0.646 0.9599 0.022 Uiso calc U . R 1
C C11 0.1314(3) 0.6141(2) 0.8361(3) 0.0176(10) Uani d . . . 1
C C12 0.1381(3) 0.5297(2) 0.8518(3) 0.0301(12) Uani d . . . 1
H H12A 0.1697 0.5196 0.9149 0.045 Uiso calc U . R 1
H H12B 0.172 0.5068 0.8169 0.045 Uiso calc U . R 1
H H12C 0.077 0.5079 0.8337 0.045 Uiso calc U . R 1
C C13 0.1240(3) 0.6429(2) 0.7532(3) 0.0188(10) Uani d . . . 1
H H13 0.1266 0.6092 0.7081 0.023 Uiso calc U . R 1
C C14 0.1127(3) 0.7199(2) 0.7344(3) 0.0169(10) Uani d . . . 1
C C15 0.1083(3) 0.7484(2) 0.6437(3) 0.0248(11) Uani d . . . 1
H H15A 0.0593 0.7224 0.5977 0.037 Uiso calc U . R 1
H H15B 0.1663 0.7384 0.635 0.037 Uiso calc U . R 1
H H15C 0.0965 0.8028 0.6399 0.037 Uiso calc U . R 1
C C16 0 0.8757(3) 0.75 0.0178(14) Uani d T P S 1
C C17 0 0.9503(3) 0.75 0.0229(15) Uani d T P S 1
C C18 0.1069(3) 1.0566(2) 0.8106(2) 0.0129(9) Uani d . . . 1
C C19 0.1077(3) 1.0770(2) 0.8955(3) 0.0161(10) Uani d . . . 1
C C20 0.0970(3) 1.0180(2) 0.9591(3) 0.0259(11) Uani d . . . 1
H H20A 0.0436 0.9868 0.9292 0.039 Uiso calc U . R 1
H H20B 0.089 1.0429 1.0105 0.039 Uiso calc U . R 1
H H20C 0.1513 0.9861 0.9788 0.039 Uiso calc U . R 1
C C21 0.1217(3) 1.1526(2) 0.9209(3) 0.0206(10) Uani d . . . 1
H H21 0.1206 1.1672 0.9775 0.025 Uiso calc U . R 1
C C22 0.1371(3) 1.2067(2) 0.8656(3) 0.0212(10) Uani d . . . 1
C C23 0.1512(3) 1.2894(2) 0.8937(3) 0.0339(12) Uani d . . . 1
H H23A 0.0995 1.3192 0.8566 0.051 Uiso calc U . R 1
H H23B 0.2072 1.308 0.8864 0.051 Uiso calc U . R 1
H H23C 0.1559 1.294 0.956 0.051 Uiso calc U . R 1
C C24 0.1415(3) 1.1838(2) 0.7843(3) 0.0179(10) Uani d . . . 1
H H24 0.1556 1.2202 0.7474 0.021 Uiso calc U . R 1
C C25 0.1261(3) 1.1096(2) 0.7550(2) 0.0134(10) Uani d . . . 1
C C26 0.1312(3) 1.0880(2) 0.6656(3) 0.0249(11) Uani d . . . 1
H H26A 0.0709 1.0925 0.6203 0.037 Uiso calc U . R 1
H H26B 0.1525 1.0358 0.6677 0.037 Uiso calc U . R 1
H H26C 0.1736 1.1217 0.6508 0.037 Uiso calc U . R 1
N N1 0.0887(2) 0.84798(17) 0.78227(19) 0.0143(8) Uani d . . . 1
N N2 0.0881(2) 0.97940(17) 0.78314(19) 0.0159(8) Uani d . . . 1
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 B1 N2 . . 105.8(4)
N1 B1 C1 . . 127.1(4)
N2 B1 C1 . . 127.1(4)
C2 C1 C6 . . 115.4(4)
C2 C1 B1 . . 121.7(4)
C6 C1 B1 . . 122.9(4)
C3 C2 C1 . . 122.5(4)
C4 C3 C2 . . 120.4(4)
C3 C4 C5 . . 119.5(4)
C4 C5 C6 . . 120.0(4)
C5 C6 C1 . . 122.2(4)
C14 C7 C8 . . 120.8(3)
C14 C7 N1 . . 120.7(3)
C8 C7 N1 . . 118.5(3)
C10 C8 C7 . . 118.5(4)
C10 C8 C9 . . 119.9(3)
C7 C8 C9 . . 121.6(3)
C11 C10 C8 . . 121.9(4)
C10 C11 C13 . . 118.1(3)
C10 C11 C12 . . 121.9(4)
C13 C11 C12 . . 120.0(4)
C11 C13 C14 . . 121.9(4)
C7 C14 C13 . . 118.7(4)
C7 C14 C15 . . 121.7(3)
C13 C14 C15 . . 119.6(3)
C17 C16 N1 . . 110.6(2)
C17 C16 N1 . 2_556 110.6(2)
N1 C16 N1 . 2_556 138.8(5)
C16 C17 N2 . 2_556 111.6(3)
C16 C17 N2 . . 111.6(3)
N2 C17 N2 2_556 . 136.7(5)
C25 C18 C19 . . 120.9(3)
C25 C18 N2 . . 120.7(3)
C19 C18 N2 . . 118.4(3)
C21 C19 C18 . . 118.5(3)
C21 C19 C20 . . 120.7(3)
C18 C19 C20 . . 120.7(3)
C22 C21 C19 . . 121.6(3)
C21 C22 C24 . . 118.3(4)
C21 C22 C23 . . 121.1(4)
C24 C22 C23 . . 120.5(4)
C25 C24 C22 . . 122.3(4)
C24 C25 C18 . . 118.1(3)
C24 C25 C26 . . 120.1(3)
C18 C25 C26 . . 121.8(3)
C16 N1 C7 . . 122.2(3)
C16 N1 B1 . . 106.3(3)
C7 N1 B1 . . 130.7(3)
C17 N2 C18 . . 122.7(3)
C17 N2 B1 . . 105.7(3)
C18 N2 B1 . . 129.5(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
B1 N1 . 1.460(5)
B1 N2 . 1.460(5)
B1 C1 . 1.551(6)
C1 C2 . 1.401(5)
C1 C6 . 1.407(5)
C2 C3 . 1.379(5)
C3 C4 . 1.370(5)
C4 C5 . 1.381(5)
C5 C6 . 1.386(5)
C7 C14 . 1.395(5)
C7 C8 . 1.401(5)
C7 N1 . 1.443(5)
C8 C10 . 1.399(5)
C8 C9 . 1.506(5)
C10 C11 . 1.387(5)
C11 C13 . 1.390(5)
C11 C12 . 1.516(5)
C13 C14 . 1.396(5)
C14 C15 . 1.519(5)
C16 C17 . 1.323(7)
C16 N1 . 1.396(3)
C16 N1 2_556 1.396(3)
C17 N2 2_556 1.397(4)
C17 N2 . 1.397(4)
C18 C25 . 1.397(5)
C18 C19 . 1.405(5)
C18 N2 . 1.437(5)
C19 C21 . 1.396(5)
C19 C20 . 1.508(5)
C21 C22 . 1.382(5)
C22 C24 . 1.391(5)
C22 C23 . 1.527(5)
C24 C25 . 1.389(5)
C25 C26 . 1.512(5)
