#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:07:13 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178491 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/02/4060254.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_4060254
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/om034268l
_journal_year                    2004
_chemical_formula_sum            'C17 H32 B10 N P'
_chemical_formula_weight         389.51
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 98.978(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2153(11)
_cell_length_b                   19.240(2)
_cell_length_c                   11.8583(12)
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_cell_volume                     2302.1(4)
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0606
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12303
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.40
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1069P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1570
_refine_ls_wR_factor_ref         0.1808
_reflns_number_gt                2557
_reflns_number_total             4039
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4060254
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 0.86123(7) 0.07896(4) 0.33042(6) 0.0385(3) Uani 1 1 d . . .
N1 N 0.7036(2) 0.08241(12) 0.3527(2) 0.0434(6) Uani 1 1 d . . .
C1 C 0.9229(3) 0.17170(14) 0.3233(2) 0.0359(7) Uani 1 1 d . . .
C3 C 0.8492(3) 0.05045(15) 0.1822(2) 0.0409(7) Uani 1 1 d . . .
C4 C 0.8870(3) -0.02110(15) 0.1593(2) 0.0395(7) Uani 1 1 d . . .
C5 C 0.9484(3) -0.07257(17) 0.2326(3) 0.0486(8) Uani 1 1 d . . .
H5A H 0.968(3) -0.0557(16) 0.308(3) 0.055(9) Uiso 1 1 d . . .
C6 C 0.9726(4) -0.13637(19) 0.1876(3) 0.0607(10) Uani 1 1 d . . .
H6A H 1.021(3) -0.1728(18) 0.240(3) 0.062(10) Uiso 1 1 d . . .
C7 C 0.9347(4) -0.14993(19) 0.0719(3) 0.0607(10) Uani 1 1 d . . .
H7A H 0.952(3) -0.1966(17) 0.044(2) 0.049(9) Uiso 1 1 d . . .
C8 C 0.8754(4) -0.09950(18) 0.0001(3) 0.0523(9) Uani 1 1 d . . .
H8A H 0.855(3) -0.1021(19) -0.079(3) 0.074(11) Uiso 1 1 d . . .
C9 C 0.8515(3) -0.03504(16) 0.0426(2) 0.0429(7) Uani 1 1 d . . .
C10 C 0.7923(3) 0.02868(15) -0.0138(2) 0.0433(7) Uani 1 1 d . . .
H10A H 0.8437 0.0452 -0.0706 0.052 Uiso 1 1 calc R . .
H10B H 0.7019 0.0204 -0.0503 0.052 Uiso 1 1 calc R . .
C11 C 0.7964(3) 0.07879(17) 0.0806(2) 0.0434(7) Uani 1 1 d . . .
H11A H 0.768(3) 0.1276(16) 0.066(2) 0.047(8) Uiso 1 1 d . . .
C30 C 0.6723(3) 0.04568(19) 0.4554(3) 0.0594(9) Uani 1 1 d . . .
H30A H 0.5756 0.0464 0.4498 0.071 Uiso 1 1 calc R . .
C31 C 0.7127(5) -0.0300(2) 0.4598(4) 0.0945(15) Uani 1 1 d . . .
H31A H 0.6744 -0.0525 0.3902 0.142 Uiso 1 1 calc R . .
H31B H 0.6817 -0.0521 0.5232 0.142 Uiso 1 1 calc R . .
H31C H 0.8075 -0.0333 0.4687 0.142 Uiso 1 1 calc R . .
C32 C 0.7264(5) 0.0841(3) 0.5640(3) 0.0938(15) Uani 1 1 d . . .
H32A H 0.6977 0.1316 0.5578 0.141 Uiso 1 1 calc R . .
H32B H 0.8215 0.0824 0.5758 0.141 Uiso 1 1 calc R . .
H32C H 0.6943 0.0626 0.6275 0.141 Uiso 1 1 calc R . .
C40 C 0.5901(3) 0.10602(17) 0.2679(3) 0.0511(8) Uani 1 1 d . . .
H40A H 0.6274 0.1294 0.2068 0.061 Uiso 1 1 calc R . .
C41 C 0.5074(4) 0.0459(2) 0.2133(4) 0.0820(13) Uani 1 1 d . . .
H41A H 0.5634 0.0138 0.1812 0.123 Uiso 1 1 calc R . .
H41B H 0.4406 0.0632 0.1540 0.123 Uiso 1 1 calc R . .
H41C H 0.4659 0.0227 0.2700 0.123 Uiso 1 1 calc R . .
C42 C 0.5063(3) 0.1596(2) 0.3184(3) 0.0703(11) Uani 1 1 d . . .
H42A H 0.5618 0.1971 0.3508 0.106 Uiso 1 1 calc R . .
H42B H 0.4647 0.1383 0.3769 0.106 Uiso 1 1 calc R . .
H42C H 0.4395 0.1773 0.2595 0.106 Uiso 1 1 calc R . .
C2 C 0.9780(3) 0.20438(16) 0.2107(2) 0.0403(7) Uani 1 1 d . . .
B3 B 1.0918(3) 0.1719(2) 0.3194(3) 0.0464(9) Uani 1 1 d . . .
B4 B 1.0286(4) 0.1965(2) 0.4437(3) 0.0484(9) Uani 1 1 d . . .
H4 H 1.040(3) 0.1575(16) 0.511(3) 0.061(9) Uiso 1 1 d . . .
B5 B 0.8738(4) 0.23812(19) 0.4019(3) 0.0459(9) Uani 1 1 d . . .
H5 H 0.798(3) 0.2264(17) 0.450(3) 0.064(10) Uiso 1 1 d . . .
B6 B 0.8422(4) 0.24135(18) 0.2514(3) 0.0423(8) Uani 1 1 d . . .
H6 H 0.743(3) 0.2346(16) 0.199(2) 0.054(9) Uiso 1 1 d . . .
B7 B 1.1218(4) 0.2492(2) 0.2450(3) 0.0512(10) Uani 1 1 d . . .
H7 H 1.188(3) 0.2468(15) 0.187(2) 0.047(8) Uiso 1 1 d . . .
B8 B 1.1540(4) 0.2468(2) 0.3959(3) 0.0562(11) Uani 1 1 d . . .
H8 H 1.257(3) 0.2463(16) 0.441(3) 0.069(10) Uiso 1 1 d . . .
B9 B 1.0194(4) 0.2873(2) 0.4467(3) 0.0565(11) Uani 1 1 d . . .
H9 H 1.032(4) 0.315(2) 0.523(3) 0.097(13) Uiso 1 1 d . . .
B10 B 0.9038(4) 0.3153(2) 0.3285(3) 0.0525(10) Uani 1 1 d . . .
H10 H 0.835(3) 0.3602(18) 0.327(3) 0.068(10) Uiso 1 1 d . . .
B11 B 0.9669(4) 0.29174(19) 0.2036(3) 0.0488(9) Uani 1 1 d . . .
H11 H 0.942(3) 0.3159(15) 0.122(2) 0.051(8) Uiso 1 1 d . . .
B12 B 1.0773(4) 0.3204(2) 0.3247(3) 0.0548(10) Uani 1 1 d . . .
H12 H 1.122(3) 0.3688(16) 0.318(2) 0.050(8) Uiso 1 1 d . . .
H3 H 1.136(3) 0.1180(14) 0.311(2) 0.037(7) Uiso 1 1 d . . .
H2A H 0.966(3) 0.1705(15) 0.146(2) 0.049(8) Uiso 1 1 d . . .
