#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/24/7012440.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_7012440
loop_
_publ_author_name
'Monkowius, Uwe'
'Nogai, Stefan'
'Schmidbaur, Hubert'
_publ_section_title
;
 Trivinylphosphineborane (CH2CH)3PBH3 and related compounds
;
_journal_issue                   5
_journal_name_full               'Dalton Transactions'
_journal_page_first              987
_journal_paper_doi               10.1039/b210991c
_journal_year                    2003
_chemical_formula_sum            'C6 H9 B Br3 P'
_chemical_formula_weight         362.64
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.1093(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.95430(10)
_cell_length_b                   11.3363(2)
_cell_length_c                   14.5709(2)
_cell_measurement_reflns_used    45210
_cell_measurement_temperature    143(2)
_cell_volume                     1147.02(3)
_computing_cell_refinement       DENZO
_computing_data_collection       XPRESS
_computing_data_reduction        SCALEPACK
_computing_molecular_graphics    SHELXTL-PLUS
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius DIP 2020'
_diffrn_measurement_method       phi-rotation
_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  0.050
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45210
_diffrn_reflns_theta_full        31.90
_diffrn_reflns_theta_max         31.90
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    10.633
_exptl_absorpt_correction_T_max  0.703
_exptl_absorpt_correction_T_min  0.244
_exptl_absorpt_correction_type   delabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.100
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    isotropic
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         3930
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0304
_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)+(0.0000P)²+0.3640P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0680
_reflns_number_gt                3467
_reflns_number_total             3930
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b210991c.txt
_cod_data_source_block           uwe10
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7012440
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.75892(7) 0.74822(4) 0.52799(4) 0.02137(10) Uani 1 1 d . . .
B1 B 0.6980(3) 0.73636(19) 0.39598(16) 0.0241(4) Uani 1 1 d . . .
Br1 Br 0.78086(3) 0.575373(19) 0.357258(15) 0.03210(7) Uani 1 1 d . . .
Br2 Br 0.41227(3) 0.75894(2) 0.376100(16) 0.03273(7) Uani 1 1 d . . .
Br3 Br 0.84628(4) 0.86312(2) 0.334877(17) 0.03800(7) Uani 1 1 d . . .
C11 C 1.0121(3) 0.7311(2) 0.55300(17) 0.0319(4) Uani 1 1 d . . .
H11 H 1.079(5) 0.667(3) 0.517(2) 0.053(9) Uiso 1 1 d . . .
C12 C 1.1089(4) 0.7945(3) 0.6161(2) 0.0464(6) Uani 1 1 d . . .
H12B H 1.046(6) 0.856(3) 0.652(3) 0.074(12) Uiso 1 1 d . . .
H12A H 1.245(7) 0.793(4) 0.626(3) 0.080(13) Uiso 1 1 d . . .
C21 C 0.6360(3) 0.63412(18) 0.58654(15) 0.0269(4) Uani 1 1 d . . .
H21 H 0.502(6) 0.623(3) 0.563(3) 0.064(11) Uiso 1 1 d . . .
C22 C 0.7179(4) 0.5725(2) 0.65482(18) 0.0359(5) Uani 1 1 d . . .
H22B H 0.649(4) 0.511(3) 0.682(2) 0.033(7) Uiso 1 1 d . . .
H22A H 0.850(5) 0.586(3) 0.674(2) 0.036(7) Uiso 1 1 d . . .
C31 C 0.6849(3) 0.88828(19) 0.57147(17) 0.0300(4) Uani 1 1 d . . .
H31 H 0.708(5) 0.951(3) 0.529(2) 0.046(8) Uiso 1 1 d . . .
C32 C 0.6043(4) 0.9004(2) 0.65082(18) 0.0345(5) Uani 1 1 d . . .
H32B H 0.579(4) 0.835(3) 0.689(2) 0.041(8) Uiso 1 1 d . . .
H32A H 0.551(5) 0.979(3) 0.668(3) 0.064(11) 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'
P P 0.1023 0.0942 '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
_geom_angle_publ_flag
C11 P1 C21 108.33(11) . . ?
C11 P1 C31 108.76(11) . . ?
C21 P1 C31 108.48(11) . . ?
C11 P1 B1 110.61(11) . . ?
C21 P1 B1 109.63(10) . . ?
C31 P1 B1 110.96(10) . . ?
P1 B1 Br1 106.84(11) . . ?
P1 B1 Br3 107.39(11) . . ?
Br1 B1 Br3 111.40(11) . . ?
P1 B1 Br2 107.07(11) . . ?
Br1 B1 Br2 111.89(11) . . ?
Br3 B1 Br2 111.91(11) . . ?
C12 C11 P1 122.8(2) . . ?
C12 C11 H11 121(2) . . ?
P1 C11 H11 116(2) . . ?
C11 C12 H12B 122(2) . . ?
C11 C12 H12A 124(3) . . ?
H12B C12 H12A 113(4) . . ?
C22 C21 P1 122.93(19) . . ?
C22 C21 H21 124(2) . . ?
P1 C21 H21 113(2) . . ?
C21 C22 H22B 120.0(17) . . ?
C21 C22 H22A 120.3(18) . . ?
H22B C22 H22A 120(2) . . ?
C32 C31 P1 123.03(19) . . ?
C32 C31 H31 125.4(19) . . ?
P1 C31 H31 111.6(19) . . ?
C31 C32 H32B 122.3(19) . . ?
C31 C32 H32A 119(2) . . ?
H32B C32 H32A 118(3) . . ?
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 C11 1.789(2) . ?
P1 C21 1.792(2) . ?
P1 C31 1.795(2) . ?
P1 B1 1.952(2) . ?
B1 Br1 2.004(2) . ?
B1 Br3 2.005(2) . ?
B1 Br2 2.009(2) . ?
C11 C12 1.322(4) . ?
C11 H11 1.02(4) . ?
C12 H12B 0.99(4) . ?
C12 H12A 0.95(5) . ?
C21 C22 1.319(3) . ?
C21 H21 0.98(4) . ?
C22 H22B 0.95(3) . ?
C22 H22A 0.96(3) . ?
C31 C32 1.319(3) . ?
C31 H31 0.96(3) . ?
C32 H32B 0.96(3) . ?
C32 H32A 1.00(4) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 P1 B1 Br1 60.73(14) . . . . ?
C21 P1 B1 Br1 -58.67(13) . . . . ?
C31 P1 B1 Br1 -178.48(10) . . . . ?
C11 P1 B1 Br3 -58.90(14) . . . . ?
C21 P1 B1 Br3 -178.30(10) . . . . ?
C31 P1 B1 Br3 61.90(13) . . . . ?
C11 P1 B1 Br2 -179.25(10) . . . . ?
C21 P1 B1 Br2 61.35(13) . . . . ?
C31 P1 B1 Br2 -58.45(13) . . . . ?
C21 P1 C11 C12 -99.3(3) . . . . ?
C31 P1 C11 C12 18.4(3) . . . . ?
B1 P1 C11 C12 140.5(2) . . . . ?
C11 P1 C21 C22 17.1(2) . . . . ?
C31 P1 C21 C22 -100.9(2) . . . . ?
B1 P1 C21 C22 137.8(2) . . . . ?
C11 P1 C31 C32 -98.5(2) . . . . ?
C21 P1 C31 C32 19.1(3) . . . . ?
B1 P1 C31 C32 139.6(2) . . . . ?
