#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:36:17 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179508 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/05/4340591.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_4340591
loop_
_publ_author_name
'Swarnakar, Anindya K.'
'McDonald, Sean M.'
'Deutsch, Kelsey C.'
'Choi, Paul'
'Ferguson, Michael J.'
'McDonald, Robert'
'Rivard, Eric'
_publ_section_title
;
 Application of the Donor-Acceptor Concept to Intercept Low Oxidation
 State Group 14 Element Hydrides using a Wittig Reagent as a Lewis Base.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8662
_journal_page_last               8671
_journal_paper_doi               10.1021/ic501265k
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C21 H24 B P'
_chemical_formula_sum            'C21 H24 B P'
_chemical_formula_weight         318.18
_chemical_name_common            7
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                99.4355(4)
_cell_angle_beta                 92.3567(5)
_cell_angle_gamma                113.1114(4)
_cell_formula_units_Z            2
_cell_length_a                   9.7208(4)
_cell_length_b                   9.9807(4)
_cell_length_c                   10.0913(4)
_cell_measurement_reflns_used    7908
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.94
_cell_measurement_theta_min      2.26
_cell_volume                     882.28(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT-2013 (Sheldrick 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0128
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8248
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.937
_diffrn_reflns_theta_min         2.060
_exptl_absorpt_coefficient_mu    0.153
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9358
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       block
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         4297
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0348
_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)+(0.0455P)²+0.3291P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.0928
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3890
_reflns_number_total             4297
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic501265k_si_002.cif
_cod_data_source_block           riv13d0
_cod_depositor_comments
'Adding full bibliography for 4340585--4340595.cif.'
_cod_database_code               4340591
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.958
_shelx_estimated_absorpt_t_max   0.985
_shelxl_version_number           2013-3
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
P P 0.37294(3) 0.14267(3) 0.26766(3) 0.01516(9) Uani 1 1 d . .
C1 C 0.31964(13) 0.21922(13) 0.13226(11) 0.0187(2) Uani 1 1 d . .
C2 C 0.43696(14) 0.37888(14) 0.13779(14) 0.0253(3) Uani 1 1 d . .
H2A H 0.4012 0.4245 0.0729 0.030 Uiso 1 1 calc R U
H2B H 0.5329 0.3760 0.1148 0.030 Uiso 1 1 calc R U
H2C H 0.4513 0.4375 0.2292 0.030 Uiso 1 1 calc R U
C3 C 0.31424(15) 0.12205(15) -0.00565(12) 0.0259(3) Uani 1 1 d . .
H3A H 0.3063 0.1735 -0.0785 0.031 Uiso 1 1 calc R U
H3B H 0.2266 0.0269 -0.0176 0.031 Uiso 1 1 calc R U
H3C H 0.4064 0.1042 -0.0082 0.031 Uiso 1 1 calc R U
C11 C 0.29626(12) 0.17706(13) 0.42354(11) 0.0180(2) Uani 1 1 d . .
C12 C 0.23040(14) 0.06263(14) 0.49372(13) 0.0245(3) Uani 1 1 d . .
H12 H 0.2216 -0.0348 0.4573 0.029 Uiso 1 1 calc R U
C13 C 0.17749(16) 0.09031(16) 0.61670(14) 0.0310(3) Uani 1 1 d . .
H13 H 0.1327 0.0119 0.6641 0.037 Uiso 1 1 calc R U
C14 C 0.19001(16) 0.23200(16) 0.67009(13) 0.0300(3) Uani 1 1 d . .
H14 H 0.1541 0.2508 0.7542 0.036 Uiso 1 1 calc R U
C15 C 0.25492(15) 0.34649(15) 0.60102(13) 0.0282(3) Uani 1 1 d . .
H15 H 0.2628 0.4435 0.6378 0.034 Uiso 1 1 calc R U
C16 C 0.30853(14) 0.31999(14) 0.47835(13) 0.0238(2) Uani 1 1 d . .
H16 H 0.3535 0.3989 0.4316 0.029 Uiso 1 1 calc R U
C21 C 0.31318(13) -0.05641(12) 0.21946(11) 0.0179(2) Uani 1 1 d . .
C22 C 0.41438(14) -0.12135(13) 0.23908(12) 0.0212(2) Uani 1 1 d . .
H22 H 0.5149 -0.0610 0.2782 0.025 Uiso 1 1 calc R U
C23 C 0.36801(15) -0.27417(14) 0.20135(13) 0.0258(3) Uani 1 1 d . .
H23 H 0.4375 -0.3176 0.2139 0.031 Uiso 1 1 calc R U
C24 C 0.22144(16) -0.36354(14) 0.14565(13) 0.0278(3) Uani 1 1 d . .
H24 H 0.1901 -0.4681 0.1207 0.033 Uiso 1 1 calc R U
C25 C 0.12024(15) -0.29949(14) 0.12640(14) 0.0286(3) Uani 1 1 d . .
H25 H 0.0195 -0.3607 0.0882 0.034 Uiso 1 1 calc R U
C26 C 0.16528(14) -0.14675(14) 0.16255(13) 0.0243(3) Uani 1 1 d . .
H26 H 0.0957 -0.1037 0.1486 0.029 Uiso 1 1 calc R U
C31 C 0.57510(12) 0.21674(12) 0.31205(12) 0.0178(2) Uani 1 1 d . .
C32 C 0.66962(14) 0.21940(14) 0.21027(13) 0.0232(2) Uani 1 1 d . .
H32 H 0.6279 0.1877 0.1180 0.028 Uiso 1 1 calc R U
C33 C 0.82346(14) 0.26801(15) 0.24345(14) 0.0273(3) Uani 1 1 d . .
H33 H 0.8869 0.2688 0.1742 0.033 Uiso 1 1 calc R U
C34 C 0.88499(14) 0.31572(15) 0.37850(14) 0.0286(3) Uani 1 1 d . .
H34 H 0.9905 0.3489 0.4013 0.034 Uiso 1 1 calc R U
C35 C 0.79324(15) 0.31484(15) 0.47914(14) 0.0280(3) Uani 1 1 d . .
H35 H 0.8359 0.3482 0.5711 0.034 Uiso 1 1 calc R U
C36 C 0.63828(14) 0.26526(14) 0.44691(12) 0.0225(2) Uani 1 1 d . .
H36 H 0.5756 0.2645 0.5168 0.027 Uiso 1 1 calc R U
B B 0.15124(16) 0.22169(17) 0.14985(15) 0.0242(3) Uani 1 1 d . .
H1A H 0.1625(18) 0.3192(18) 0.2349(16) 0.033(4) Uiso 1 1 d . .
H1B H 0.1141(19) 0.2435(19) 0.0492(17) 0.040(5) Uiso 1 1 d . .
H1C H 0.0663(19) 0.1137(19) 0.1712(17) 0.037(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'
P P 0.1023 0.0942 '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
C11 P C21 106.97(5)
C11 P C31 105.65(5)
C21 P C31 105.41(5)
C11 P C1 113.95(5)
C21 P C1 111.54(5)
C31 P C1 112.72(5)
C2 C1 C3 109.03(10)
C2 C1 B 109.48(10)
C3 C1 B 109.70(10)
C2 C1 P 109.71(8)
C3 C1 P 109.30(8)
B C1 P 109.60(8)
C12 C11 C16 119.24(11)
C12 C11 P 120.23(9)
C16 C11 P 120.46(9)
C13 C12 C11 120.35(12)
C14 C13 C12 120.01(12)
C13 C14 C15 120.13(12)
C14 C15 C16 120.27(12)
C15 C16 C11 120.01(12)
C22 C21 C26 119.36(11)
C22 C21 P 120.31(9)
C26 C21 P 120.33(9)
C23 C22 C21 120.04(11)
C24 C23 C22 120.55(11)
C23 C24 C25 119.61(11)
C26 C25 C24 120.50(12)
C25 C26 C21 119.93(11)
C36 C31 C32 119.11(11)
C36 C31 P 120.96(9)
C32 C31 P 119.87(9)
C33 C32 C31 120.39(11)
C32 C33 C34 119.91(12)
C35 C34 C33 120.13(12)
C34 C35 C36 120.42(12)
C35 C36 C31 120.04(11)
C1 B H1A 109.7(8)
C1 B H1B 104.9(9)
H1A B H1B 108.6(12)
C1 B H1C 112.8(9)
H1A B H1C 110.0(12)
H1B B H1C 110.6(12)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
P C11 1.8078(11)
P C21 1.8099(11)
P C31 1.8132(11)
P C1 1.8205(11)
C1 C2 1.5433(17)
C1 C3 1.5465(16)
C1 B 1.6631(18)
C11 C12 1.3943(16)
C11 C16 1.3992(16)
C12 C13 1.3901(18)
C13 C14 1.384(2)
C14 C15 1.386(2)
C15 C16 1.3884(17)
C21 C22 1.3977(15)
C21 C26 1.3981(17)
C22 C23 1.3893(17)
C23 C24 1.3834(19)
C24 C25 1.3903(19)
C25 C26 1.3890(17)
C31 C36 1.3948(16)
C31 C32 1.4026(16)
C32 C33 1.3857(17)
C33 C34 1.3922(19)
C34 C35 1.3778(19)
C35 C36 1.3934(17)
B H1A 1.153(16)
B H1B 1.146(17)
B H1C 1.132(17)
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
C11 P C1 C2 90.16(9)
C21 P C1 C2 -148.60(8)
C31 P C1 C2 -30.23(10)
C11 P C1 C3 -150.34(8)
C21 P C1 C3 -29.09(10)
C31 P C1 C3 89.27(9)
C11 P C1 B -30.08(10)
C21 P C1 B 91.17(9)
C31 P C1 B -150.47(8)
C21 P C11 C12 10.38(11)
C31 P C11 C12 -101.59(10)
C1 P C11 C12 134.12(10)
C21 P C11 C16 -172.61(10)
C31 P C11 C16 75.42(11)
C1 P C11 C16 -48.86(11)
C16 C11 C12 C13 0.03(19)
P C11 C12 C13 177.08(10)
C11 C12 C13 C14 0.0(2)
C12 C13 C14 C15 0.2(2)
C13 C14 C15 C16 -0.4(2)
C14 C15 C16 C11 0.4(2)
C12 C11 C16 C15 -0.24(18)
P C11 C16 C15 -177.28(10)
C11 P C21 C22 -103.75(10)
C31 P C21 C22 8.38(11)
C1 P C21 C22 131.03(9)
C11 P C21 C26 76.10(11)
C31 P C21 C26 -171.77(10)
C1 P C21 C26 -49.12(11)
C26 C21 C22 C23 0.42(18)
P C21 C22 C23 -179.73(9)
C21 C22 C23 C24 -0.75(19)
C22 C23 C24 C25 0.5(2)
C23 C24 C25 C26 0.0(2)
C24 C25 C26 C21 -0.4(2)
C22 C21 C26 C25 0.13(18)
P C21 C26 C25 -179.72(10)
C11 P C31 C36 8.64(11)
C21 P C31 C36 -104.42(10)
C1 P C31 C36 133.69(10)
C11 P C31 C32 -174.31(9)
C21 P C31 C32 72.64(10)
C1 P C31 C32 -49.25(11)
C36 C31 C32 C33 0.73(18)
P C31 C32 C33 -176.38(10)
C31 C32 C33 C34 -0.5(2)
C32 C33 C34 C35 -0.1(2)
C33 C34 C35 C36 0.5(2)
C34 C35 C36 C31 -0.30(19)
C32 C31 C36 C35 -0.31(18)
P C31 C36 C35 176.77(9)
