#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/05/4310518.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_4310518
loop_
_publ_author_name
'Cory A. Jaska'
'Alan J. Lough'
'Ian Manners'
_publ_section_title
;
 Linear Hybrid Aminoborane/Phosphinoborane Chains: Synthesis,
 Proton-Hydride Interactions, and Thermolysis Behavior
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1090
_journal_page_last               1099
_journal_paper_doi               10.1021/ic034938f
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C15 H24 B2 N P'
_chemical_formula_weight         270.94
_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                   11.9203(2)
_cell_length_b                   9.6239(3)
_cell_length_c                   28.7897(7)
_cell_measurement_reflns_used    4109
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     3302.75(14)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2002)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL V6.12 (Sheldrick, 2001)'
_computing_publication_material  'SHELXTL V6.12 (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL V6.12 (Sheldrick, 2001)'
_computing_structure_solution    'SHELXTL V6.12 (Sheldrick, 2001)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scan and ω scans with κ offsets'
_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  0.042
_diffrn_reflns_av_sigmaI/netI    0.046
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            20296
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.81
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.153
_exptl_absorpt_correction_T_max  0.9556
_exptl_absorpt_correction_T_min  0.9415
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.0021(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3776
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0405
_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)+(0.0396P)²+1.2846P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.1038
_reflns_number_gt                2776
_reflns_number_total             3776
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic034938fsi20030806_112146.cif
_cod_data_source_block           k0229a
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'C15 H6 H18 B2 N P'
_cod_database_code               4310518
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
P1 P 0.41790(3) 0.25784(4) 0.368104(13) 0.02476(13) Uani 1 1 d . . .
N1 N 0.42360(11) 0.31361(14) 0.24611(5) 0.0303(3) Uani 1 1 d . . .
H1N H 0.4565(13) 0.3715(16) 0.2636(6) 0.030(5) Uiso 1 1 d . . .
C1 C 0.34379(13) 0.17596(16) 0.32097(5) 0.0305(4) Uani 1 1 d . . .
H1A H 0.3221 0.0810 0.3307 0.037 Uiso 1 1 calc R . .
H1B H 0.2739 0.2286 0.3150 0.037 Uiso 1 1 calc R . .
C2 C 0.31386(15) 0.3773(2) 0.23494(7) 0.0489(5) Uani 1 1 d . . .
H2A H 0.3257 0.4613 0.2164 0.073 Uiso 1 1 calc R . .
H2B H 0.2750 0.4017 0.2638 0.073 Uiso 1 1 calc R . .
H2C H 0.2683 0.3110 0.2173 0.073 Uiso 1 1 calc R . .
C3 C 0.49181(17) 0.29877(18) 0.20324(6) 0.0442(5) Uani 1 1 d . . .
H3A H 0.4985 0.3893 0.1879 0.066 Uiso 1 1 calc R . .
H3B H 0.4553 0.2329 0.1822 0.066 Uiso 1 1 calc R . .
H3C H 0.5667 0.2643 0.2113 0.066 Uiso 1 1 calc R . .
C4 C 0.52597(13) 0.13542(15) 0.38519(5) 0.0275(3) Uani 1 1 d . . .
C5 C 0.50213(15) 0.02165(17) 0.41329(6) 0.0413(4) Uani 1 1 d . . .
H5A H 0.4281 0.0081 0.4246 0.050 Uiso 1 1 calc R . .
C6 C 0.58591(17) -0.07195(19) 0.42483(7) 0.0518(5) Uani 1 1 d . . .
H6A H 0.5692 -0.1491 0.4442 0.062 Uiso 1 1 calc R . .
C7 C 0.69356(16) -0.05345(19) 0.40827(7) 0.0467(5) Uani 1 1 d . . .
H7A H 0.7506 -0.1182 0.4161 0.056 Uiso 1 1 calc R . .
C8 C 0.71830(15) 0.05854(19) 0.38046(6) 0.0412(4) Uani 1 1 d . . .
H8A H 0.7924 0.0711 0.3691 0.049 Uiso 1 1 calc R . .
C9 C 0.63506(13) 0.15307(18) 0.36901(6) 0.0331(4) Uani 1 1 d . . .
H9A H 0.6526 0.2306 0.3499 0.040 Uiso 1 1 calc R . .
C10 C 0.32623(13) 0.26693(15) 0.41834(5) 0.0282(3) Uani 1 1 d . . .
C11 C 0.36305(15) 0.33999(18) 0.45729(6) 0.0394(4) Uani 1 1 d . . .
H11A H 0.4350 0.3825 0.4570 0.047 Uiso 1 1 calc R . .
C12 C 0.29597(17) 0.3512(2) 0.49634(6) 0.0484(5) Uani 1 1 d . . .
H12A H 0.3220 0.4010 0.5227 0.058 Uiso 1 1 calc R . .
C13 C 0.19113(17) 0.29002(18) 0.49703(6) 0.0455(5) Uani 1 1 d . . .
H13A H 0.1443 0.2992 0.5236 0.055 Uiso 1 1 calc R . .
C14 C 0.15498(15) 0.21593(18) 0.45912(7) 0.0434(5) Uani 1 1 d . . .
H14A H 0.0837 0.1717 0.4599 0.052 Uiso 1 1 calc R . .
C15 C 0.22112(14) 0.20469(17) 0.41959(6) 0.0366(4) Uani 1 1 d . . .
H15A H 0.1945 0.1545 0.3934 0.044 Uiso 1 1 calc R . .
B1 B 0.41468(17) 0.16546(19) 0.27252(6) 0.0319(4) Uani 1 1 d . . .
H1 H 0.3709(13) 0.0943(17) 0.2475(6) 0.038(4) Uiso 1 1 d . . .
H2 H 0.5044(14) 0.1334(16) 0.2782(5) 0.035(4) Uiso 1 1 d . . .
B2 B 0.47588(16) 0.43900(19) 0.35260(7) 0.0317(4) Uani 1 1 d . . .
H3 H 0.5085(15) 0.4873(19) 0.3859(7) 0.052(5) Uiso 1 1 d . . .
H4 H 0.3991(14) 0.4955(17) 0.3369(6) 0.043(5) Uiso 1 1 d . . .
H5 H 0.5433(13) 0.4241(16) 0.3259(6) 0.034(4) Uiso 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'
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'
P P 0.1023 0.0942 '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'
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
C1 P1 C4 105.58(7) . . ?
C1 P1 C10 109.04(7) . . ?
C4 P1 C10 104.05(7) . . ?
C1 P1 B2 113.40(8) . . ?
C4 P1 B2 113.30(8) . . ?
C10 P1 B2 110.90(8) . . ?
H1N N1 C2 105.4(11) . . ?
H1N N1 C3 107.7(11) . . ?
C2 N1 C3 110.08(14) . . ?
H1N N1 B1 109.3(11) . . ?
C2 N1 B1 114.11(14) . . ?
C3 N1 B1 109.97(13) . . ?
N1 H1N H5 151.8(15) . . ?
B1 C1 P1 114.62(11) . . ?
C5 C4 C9 118.80(15) . . ?
C5 C4 P1 121.61(12) . . ?
C9 C4 P1 119.58(12) . . ?
C6 C5 C4 120.27(17) . . ?
C7 C6 C5 120.23(18) . . ?
C8 C7 C6 120.11(17) . . ?
C7 C8 C9 119.98(17) . . ?
C8 C9 C4 120.61(16) . . ?
C15 C10 C11 118.71(15) . . ?
C15 C10 P1 122.88(12) . . ?
C11 C10 P1 118.40(12) . . ?
C12 C11 C10 120.71(17) . . ?
C13 C12 C11 120.08(18) . . ?
C14 C13 C12 119.58(16) . . ?
C13 C14 C15 120.91(17) . . ?
C14 C15 C10 119.99(16) . . ?
H1 B1 H2 111.6(11) . . ?
H1 B1 N1 105.4(8) . . ?
H2 B1 N1 104.3(8) . . ?
H1 B1 C1 110.2(9) . . ?
H2 B1 C1 112.7(8) . . ?
N1 B1 C1 112.36(13) . . ?
H5 B2 H3 112.8(12) . . ?
H5 B2 H4 111.1(12) . . ?
H3 B2 H4 114.1(13) . . ?
H5 B2 P1 107.5(8) . . ?
H3 B2 P1 107.3(9) . . ?
H4 B2 P1 103.4(8) . . ?
B2 H5 H1N 105.0(11) . . ?
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
P1 C1 1.8007(15) . ?
P1 C4 1.8137(16) . ?
P1 C10 1.8148(15) . ?
P1 B2 1.9278(18) . ?
N1 H1N 0.848(16) . ?
N1 C2 1.480(2) . ?
N1 C3 1.485(2) . ?
N1 B1 1.619(2) . ?
H1N H5 2.13(2) . ?
C1 B1 1.634(2) . ?
C4 C5 1.391(2) . ?
C4 C9 1.392(2) . ?
C5 C6 1.385(2) . ?
C6 C7 1.380(3) . ?
C7 C8 1.374(3) . ?
C8 C9 1.386(2) . ?
C10 C15 1.389(2) . ?
C10 C11 1.394(2) . ?
C11 C12 1.384(2) . ?
C12 C13 1.382(3) . ?
C13 C14 1.373(3) . ?
C14 C15 1.389(2) . ?
B1 H1 1.123(17) . ?
B1 H2 1.125(16) . ?
B2 H5 1.121(16) . ?
B2 H3 1.134(19) . ?
B2 H4 1.156(17) . ?
