#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/13/4001396.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_4001396
loop_
_publ_author_name
'Chizmeshya, A. V. G.'
'Ritter, C. J.'
'Groy, T. L.'
'Tice, J. B.'
'Kouvetakis, J.'
_publ_section_title
;
 Synthesis of Molecular Adducts of Beryllium, Boron, and Gallium Cyanides:
 Theoretical and Experimental Correlations between Solid-State and
 Molecular Analogues
;
_journal_issue                   24
_journal_name_full               'Chemistry of Materials'
_journal_page_first              5890
_journal_paper_doi               10.1021/cm071275h
_journal_volume                  19
_journal_year                    2007
_chemical_formula_moiety         'C4 B N4, C5 H6 N'
_chemical_formula_sum            'C9 H6 B N5'
_chemical_formula_weight         195.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   13.2610(9)
_cell_length_b                   7.6398(5)
_cell_length_c                   21.3062(14)
_cell_measurement_reflns_used    2535
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.101
_cell_measurement_theta_min      3.072
_cell_volume                     2158.6(2)
_computing_cell_refinement       'SAINT V6.28A'
_computing_data_collection       'SMART V5.625'
_computing_data_reduction        'SAINT V6.28A'
_computing_molecular_graphics    'Bruker SHELXTL Ver. 6.12 (2001)'
_computing_publication_material  'Bruker SHELXTL Ver. 6.12 (2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       'ω scan'
_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  0.0654
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16174
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0.00
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.990
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.128
_refine_diff_density_min         -0.117
_refine_diff_density_rms         0.026
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.810
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         1906
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.810
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0595P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1175
_reflns_number_gt                1056
_reflns_number_total             1906
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm071275h-file001.cif
_cod_data_source_block           pbca
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4001396
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
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
B B 0.61906(16) 0.0255(3) 0.41920(10) 0.0507(6) Uani 1 1 d . . .
C1 C 0.65167(16) -0.1279(4) 0.46463(13) 0.0680(12) Uani 0.95(3) 1 d P A 1
N1 N 0.67345(17) -0.2363(4) 0.49855(13) 0.1079(12) Uani 0.95(3) 1 d P A 1
N1' N 0.65167(16) -0.1279(4) 0.46463(13) 0.0680(12) Uani 0.05(3) 1 d P A 2
C1' C 0.67345(17) -0.2363(4) 0.49855(13) 0.1079(12) Uani 0.05(3) 1 d P A 2
C2 C 0.5193(2) -0.0300(3) 0.38218(11) 0.0611(10) Uani 0.94(3) 1 d P A 3
N2 N 0.4489(2) -0.0698(3) 0.35576(11) 0.0832(9) Uani 0.94(3) 1 d P A 3
N2' N 0.5193(2) -0.0300(3) 0.38218(11) 0.0611(10) Uani 0.06(3) 1 d P A 4
C2' C 0.4489(2) -0.0698(3) 0.35576(11) 0.0832(9) Uani 0.06(3) 1 d P A 4
C3 C 0.7065(2) 0.0658(3) 0.36994(12) 0.0611(10) Uani 0.93(3) 1 d P A 5
N3 N 0.76808(19) 0.0960(3) 0.33454(11) 0.0854(9) Uani 0.93(3) 1 d P A 5
N3' N 0.7065(2) 0.0658(3) 0.36994(12) 0.0611(10) Uani 0.07(3) 1 d P A 6
C3' C 0.76808(19) 0.0960(3) 0.33454(11) 0.0854(9) Uani 0.07(3) 1 d P A 6
C4 C 0.59685(15) 0.1934(4) 0.46021(12) 0.0587(10) Uani 0.99(3) 1 d P A 7
N4 N 0.58040(15) 0.3119(4) 0.49083(11) 0.0817(10) Uani 0.99(3) 1 d P A 7
N4' N 0.59685(15) 0.1934(4) 0.46021(12) 0.0587(10) Uani 0.01(3) 1 d P A 8
C4' C 0.58040(15) 0.3119(4) 0.49083(11) 0.0817(10) Uani 0.01(3) 1 d P A 8
N5 N 0.60261(18) 0.5056(2) 0.60549(9) 0.0773(6) Uani 1 1 d . . .
H5A H 0.6000 0.4659 0.5678 0.093 Uiso 1 1 calc R . .
C5 C 0.6905(2) 0.5576(4) 0.62803(13) 0.0859(8) Uani 1 1 d . . .
H5B H 0.7483 0.5501 0.6034 0.103 Uiso 1 1 calc R . .
C6 C 0.6959(2) 0.6214(3) 0.68658(13) 0.0850(8) Uani 1 1 d . . .
H6 H 0.7573 0.6576 0.7031 0.102 Uiso 1 1 calc R . .
C7 C 0.6110(2) 0.6322(3) 0.72111(11) 0.0855(8) Uani 1 1 d . . .
H7 H 0.6136 0.6785 0.7615 0.103 Uiso 1 1 calc R . .
C8 C 0.5218(2) 0.5760(3) 0.69736(12) 0.0845(8) Uani 1 1 d . . .
H8 H 0.4634 0.5815 0.7214 0.101 Uiso 1 1 calc R . .
C9 C 0.5188(2) 0.5123(3) 0.63862(14) 0.0775(7) Uani 1 1 d . . .
H9 H 0.4583 0.4732 0.6215 0.093 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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C4 B C1 108.33(17)
C4 B C3 110.06(17)
C1 B C3 110.32(16)
C4 B C2 109.54(16)
C1 B C2 109.40(17)
C3 B C2 109.18(16)
N1 C1 B 178.1(2)
N2 C2 B 179.7(3)
N3 C3 B 179.2(2)
N4 C4 B 178.5(2)
C9 N5 C5 122.5(2)
C9 N5 H5A 118.7
C5 N5 H5A 118.7
N5 C5 C6 119.6(2)
N5 C5 H5B 120.2
C6 C5 H5B 120.2
C5 C6 C7 119.1(2)
C5 C6 H6 120.4
C7 C6 H6 120.4
C6 C7 C8 120.4(2)
C6 C7 H7 119.8
C8 C7 H7 119.8
C9 C8 C7 119.2(2)
C9 C8 H8 120.4
C7 C8 H8 120.4
N5 C9 C8 119.3(2)
N5 C9 H9 120.4
C8 C9 H9 120.4
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
B C4 1.580(4)
B C1 1.580(4)
B C3 1.594(4)
B C2 1.597(4)
C1 N1 1.137(2)
C2 N2 1.133(2)
C3 N3 1.135(2)
C4 N4 1.137(2)
N5 C9 1.317(3)
N5 C5 1.322(3)
N5 H5A 0.8600
C5 C6 1.341(3)
C5 H5B 0.9300
C6 C7 1.347(3)
C6 H6 0.9300
C7 C8 1.357(3)
C7 H7 0.9300
C8 C9 1.343(3)
C8 H8 0.9300
C9 H9 0.9300
