#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:25:15 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179789 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/85/7008555.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_7008555
loop_
_publ_author_name
'Hawkeswood, Sarah'
'Stephan, Douglas W.'
_publ_section_title
;
 Syntheses and reactions of the bis-boryloxide O(Bpin)2(pin = O2C2Me4).
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2182
_journal_page_last               2187
_journal_paper_doi               10.1039/b504246a
_journal_year                    2005
_chemical_formula_sum            'C30 H65 B3 N O8 P'
_chemical_formula_weight         631.23
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.422(6)
_cell_angle_beta                 104.550(6)
_cell_angle_gamma                106.244(6)
_cell_formula_units_Z            2
_cell_length_a                   10.752(3)
_cell_length_b                   13.737(4)
_cell_length_c                   14.181(4)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     1921.8(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.1040
_diffrn_reflns_av_sigmaI/netI    0.3611
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8994
_diffrn_reflns_theta_full        23.32
_diffrn_reflns_theta_max         23.32
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.178
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.843
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5469
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.843
_refine_ls_R_factor_all          0.2470
_refine_ls_R_factor_gt           0.0854
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0585P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1554
_refine_ls_wR_factor_ref         0.1984
_reflns_number_gt                1562
_reflns_number_total             5469
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b504246a.txt
_cod_data_source_block           '[tBu3PNH2][(BpinO)2Bpin]'
_cod_original_cell_volume        1921.9(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7008555
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.2990(2) 0.31408(16) 0.22742(15) 0.0558(6) Uani 1 1 d . . .
N1 N 0.1706(6) 0.3559(5) 0.1808(4) 0.0588(19) Uani 1 1 d . . .
H1A H 0.133(6) 0.387(5) 0.228(5) 0.071 Uiso 1 1 d . . .
H1B H 0.075(6) 0.298(5) 0.158(4) 0.071 Uiso 1 1 d . . .
C1 C 0.2933(8) 0.2787(7) 0.3516(7) 0.073(3) Uani 1 1 d . . .
C2 C 0.1511(8) 0.2213(6) 0.3516(6) 0.094(3) Uani 1 1 d . . .
H2A H 0.1518 0.2033 0.4157 0.140 Uiso 1 1 calc R . .
H2B H 0.1168 0.1600 0.3034 0.140 Uiso 1 1 calc R . .
H2C H 0.0944 0.2641 0.3355 0.140 Uiso 1 1 calc R . .
C3 C 0.3889(8) 0.2142(6) 0.3904(5) 0.092(3) Uani 1 1 d . . .
H3A H 0.3810 0.1977 0.4536 0.138 Uiso 1 1 calc R . .
H3B H 0.4807 0.2534 0.3966 0.138 Uiso 1 1 calc R . .
H3C H 0.3639 0.1520 0.3447 0.138 Uiso 1 1 calc R . .
C4 C 0.3362(8) 0.3782(6) 0.4291(5) 0.092(3) Uani 1 1 d . . .
H4A H 0.3335 0.3596 0.4926 0.138 Uiso 1 1 calc R . .
H4B H 0.2751 0.4171 0.4094 0.138 Uiso 1 1 calc R . .
H4C H 0.4263 0.4189 0.4328 0.138 Uiso 1 1 calc R . .
C5 C 0.2799(8) 0.2036(7) 0.1366(7) 0.077(3) Uani 1 1 d . . .
C6 C 0.4065(8) 0.1714(6) 0.1504(6) 0.103(3) Uani 1 1 d . . .
H6A H 0.3899 0.1136 0.1013 0.154 Uiso 1 1 calc R . .
H6B H 0.4308 0.1529 0.2149 0.154 Uiso 1 1 calc R . .
H6C H 0.4791 0.2275 0.1439 0.154 Uiso 1 1 calc R . .
C7 C 0.2384(8) 0.2275(7) 0.0313(6) 0.115(4) Uani 1 1 d . . .
H7A H 0.2287 0.1694 -0.0152 0.173 Uiso 1 1 calc R . .
H7B H 0.3065 0.2862 0.0236 0.173 Uiso 1 1 calc R . .
H7C H 0.1539 0.2418 0.0198 0.173 Uiso 1 1 calc R . .
C8 C 0.1625(9) 0.1104(6) 0.1432(6) 0.109(3) Uani 1 1 d . . .
H8A H 0.1526 0.0527 0.0961 0.164 Uiso 1 1 calc R . .
H8B H 0.0800 0.1279 0.1292 0.164 Uiso 1 1 calc R . .
H8C H 0.1822 0.0931 0.2085 0.164 Uiso 1 1 calc R . .
C9 C 0.4493(7) 0.4253(6) 0.2355(6) 0.062(2) Uani 1 1 d . . .
C10 C 0.4287(7) 0.5257(5) 0.2735(6) 0.088(3) Uani 1 1 d . . .
H10A H 0.5068 0.5824 0.2769 0.131 Uiso 1 1 calc R . .
H10B H 0.4161 0.5228 0.3380 0.131 Uiso 1 1 calc R . .
H10C H 0.3504 0.5346 0.2293 0.131 Uiso 1 1 calc R . .
C11 C 0.5809(7) 0.4125(6) 0.3043(6) 0.083(3) Uani 1 1 d . . .
H11A H 0.6568 0.4706 0.3067 0.124 Uiso 1 1 calc R . .
H11B H 0.5949 0.3509 0.2787 0.124 Uiso 1 1 calc R . .
H11C H 0.5715 0.4082 0.3695 0.124 Uiso 1 1 calc R . .
C12 C 0.4710(8) 0.4373(6) 0.1337(6) 0.088(3) Uani 1 1 d . . .
H12A H 0.5492 0.4951 0.1402 0.132 Uiso 1 1 calc R . .
H12B H 0.3931 0.4482 0.0909 0.132 Uiso 1 1 calc R . .
H12C H 0.4844 0.3762 0.1063 0.132 Uiso 1 1 calc R . .
B1 B -0.1731(8) 0.2937(7) 0.1910(6) 0.046(2) Uani 1 1 d . . .
B2 B -0.0197(9) 0.4724(7) 0.2894(6) 0.044(2) Uani 1 1 d . . .
B3 B -0.2508(9) 0.1462(8) 0.2804(7) 0.052(2) Uani 1 1 d . . .
O1 O -0.1211(4) 0.2347(3) 0.1256(3) 0.0465(13) Uani 1 1 d . . .
O2 O -0.2691(4) 0.3314(3) 0.1242(4) 0.0494(13) Uani 1 1 d . . .
O3 O -0.0545(4) 0.3745(4) 0.2548(3) 0.0617(15) Uani 1 1 d . . .
O4 O 0.1117(5) 0.5331(4) 0.3103(4) 0.0640(15) Uani 1 1 d . . .
O5 O -0.0994(5) 0.5275(4) 0.3126(4) 0.0738(17) Uani 1 1 d . . .
O6 O -0.2415(5) 0.2353(4) 0.2546(3) 0.0621(15) Uani 1 1 d . . .
O7 O -0.1771(6) 0.0830(4) 0.2738(4) 0.098(2) Uani 1 1 d . . .
O8 O -0.3486(7) 0.0987(5) 0.3257(5) 0.121(3) Uani 1 1 d . . .
C13 C -0.2087(7) 0.2161(6) 0.0294(5) 0.054(2) Uani 1 1 d . . .
C14 C -0.3243(7) 0.1173(5) 0.0174(5) 0.069(2) Uani 1 1 d . . .
H14A H -0.3727 0.1248 0.0645 0.103 Uiso 1 1 calc R . .
H14B H -0.2883 0.0612 0.0283 0.103 Uiso 1 1 calc R . .
H14C H -0.3845 0.1036 -0.0482 0.103 Uiso 1 1 calc R . .
C15 C -0.1336(7) 0.2035(6) -0.0473(5) 0.077(3) Uani 1 1 d . . .
H15A H -0.0613 0.2656 -0.0408 0.116 Uiso 1 1 calc R . .
H15B H -0.1952 0.1894 -0.1124 0.116 Uiso 1 1 calc R . .
H15C H -0.0972 0.1476 -0.0366 0.116 Uiso 1 1 calc R . .
C16 C -0.2564(7) 0.3140(5) 0.0278(5) 0.051(2) Uani 1 1 d . . .
C17 C -0.3917(6) 0.2999(5) -0.0470(5) 0.067(2) Uani 1 1 d . . .
H17A H -0.4587 0.2418 -0.0372 0.101 Uiso 1 1 calc R . .
H17B H -0.3835 0.2886 -0.1125 0.101 Uiso 1 1 calc R . .
H17C H -0.4181 0.3605 -0.0385 0.101 Uiso 1 1 calc R . .
C18 C -0.1525(7) 0.4077(5) 0.0117(5) 0.076(2) Uani 1 1 d . . .
H18A H -0.0663 0.4176 0.0581 0.114 Uiso 1 1 calc R . .
H18B H -0.1806 0.4674 0.0210 0.114 Uiso 1 1 calc R . .
H18C H -0.1454 0.3973 -0.0542 0.114 Uiso 1 1 calc R . .
C19 C 0.1280(10) 0.6319(7) 0.3641(8) 0.086(3) Uani 1 1 d . . .
C20 C 0.2265(9) 0.7156(6) 0.3341(7) 0.125(4) Uani 1 1 d . . .
H20A H 0.1932 0.7170 0.2649 0.187 Uiso 1 1 calc R . .
H20B H 0.3122 0.7030 0.3472 0.187 Uiso 1 1 calc R . .
H20C H 0.2372 0.7805 0.3710 0.187 Uiso 1 1 calc R . .
C21 C 0.1775(10) 0.6243(7) 0.4730(7) 0.131(4) Uani 1 1 d . . .
H21A H 0.2689 0.6224 0.4882 0.196 Uiso 1 1 calc R . .
H21B H 0.1209 0.5628 0.4868 0.196 Uiso 1 1 calc R . .
H21C H 0.1740 0.6829 0.5124 0.196 Uiso 1 1 calc R . .
C22 C -0.0207(10) 0.6333(6) 0.3360(7) 0.077(3) Uani 1 1 d . . .
C23 C -0.0597(9) 0.6781(7) 0.2413(7) 0.129(4) Uani 1 1 d . . .
H23A H -0.0321 0.6468 0.1905 0.194 Uiso 1 1 calc R . .
H23B H -0.0154 0.7509 0.2536 0.194 Uiso 1 1 calc R . .
H23C H -0.1558 0.6647 0.2203 0.194 Uiso 1 1 calc R . .
C24 C -0.0629(9) 0.6844(7) 0.4133(7) 0.133(4) Uani 1 1 d . . .
H24A H -0.1553 0.6822 0.3875 0.200 Uiso 1 1 calc R . .
H24B H -0.0064 0.7546 0.4327 0.200 Uiso 1 1 calc R . .
H24C H -0.0541 0.6495 0.4695 0.200 Uiso 1 1 calc R . .
C25 C -0.2319(10) -0.0140(7) 0.3029(7) 0.080(3) Uani 1 1 d . . .
C26 C -0.2934(11) -0.0919(7) 0.2131(7) 0.154(5) Uani 1 1 d . . .
H26A H -0.3698 -0.0775 0.1722 0.231 Uiso 1 1 calc R . .
H26B H -0.3222 -0.1587 0.2313 0.231 Uiso 1 1 calc R . .
H26C H -0.2280 -0.0903 0.1775 0.231 Uiso 1 1 calc R . .
C27 C -0.1159(11) -0.0410(8) 0.3657(8) 0.177(6) Uani 1 1 d . . .
H27A H -0.1493 -0.1050 0.3879 0.266 Uiso 1 1 calc R . .
H27B H -0.0688 0.0120 0.4218 0.266 Uiso 1 1 calc R . .
H27C H -0.0553 -0.0475 0.3279 0.266 Uiso 1 1 calc R . .
C28 C -0.3329(11) 0.0053(7) 0.3542(7) 0.083(3) Uani 1 1 d . . .
C29 C -0.4681(12) -0.0754(9) 0.3239(10) 0.193(6) Uani 1 1 d . . .
H29A H -0.4986 -0.0928 0.2533 0.289 Uiso 1 1 calc R . .
H29B H -0.5317 -0.0497 0.3465 0.289 Uiso 1 1 calc R . .
H29C H -0.4608 -0.1354 0.3524 0.289 Uiso 1 1 calc R . .
C30 C -0.2780(13) 0.0293(8) 0.4641(8) 0.192(6) Uani 1 1 d . . .
H30A H -0.1892 0.0784 0.4818 0.288 Uiso 1 1 calc R . .
H30B H -0.2731 -0.0324 0.4901 0.288 Uiso 1 1 calc R . .
H30C H -0.3364 0.0574 0.4910 0.288 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'
O O 0.0106 0.0060 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 C5 105.1(4) . . ?
N1 P1 C9 103.5(3) . . ?
C5 P1 C9 112.8(4) . . ?
N1 P1 C1 109.7(3) . . ?
C5 P1 C1 112.9(4) . . ?
C9 P1 C1 112.1(4) . . ?
C2 C1 C3 109.3(8) . . ?
C2 C1 C4 104.9(7) . . ?
C3 C1 C4 107.6(7) . . ?
C2 C1 P1 111.5(6) . . ?
C3 C1 P1 113.2(6) . . ?
C4 C1 P1 109.8(6) . . ?
C6 C5 C7 108.8(7) . . ?
C6 C5 C8 108.6(7) . . ?
C7 C5 C8 105.9(7) . . ?
C6 C5 P1 113.6(6) . . ?
C7 C5 P1 110.3(6) . . ?
C8 C5 P1 109.4(6) . . ?
C12 C9 C10 106.0(7) . . ?
C12 C9 C11 107.8(6) . . ?
C10 C9 C11 109.9(6) . . ?
C12 C9 P1 111.4(6) . . ?
C10 C9 P1 110.4(5) . . ?
C11 C9 P1 111.2(5) . . ?
O6 B1 O2 108.5(6) . . ?
O6 B1 O3 107.6(7) . . ?
O2 B1 O3 114.3(6) . . ?
O6 B1 O1 115.6(6) . . ?
O2 B1 O1 105.0(6) . . ?
O3 B1 O1 106.0(6) . . ?
O3 B2 O4 120.7(7) . . ?
O3 B2 O5 128.3(8) . . ?
O4 B2 O5 111.0(7) . . ?
O6 B3 O7 131.1(9) . . ?
O6 B3 O8 121.8(8) . . ?
O7 B3 O8 107.1(8) . . ?
C13 O1 B1 107.8(5) . . ?
C16 O2 B1 108.5(5) . . ?
B2 O3 B1 138.7(6) . . ?
B2 O4 C19 109.6(6) . . ?
B2 O5 C22 107.8(7) . . ?
B3 O6 B1 134.3(6) . . ?
B3 O7 C25 112.1(8) . . ?
B3 O8 C28 111.8(7) . . ?
O1 C13 C14 108.7(6) . . ?
O1 C13 C15 110.6(6) . . ?
C14 C13 C15 108.9(6) . . ?
O1 C13 C16 101.7(5) . . ?
C14 C13 C16 112.8(6) . . ?
C15 C13 C16 113.9(7) . . ?
O2 C16 C17 109.1(6) . . ?
O2 C16 C18 109.0(6) . . ?
C17 C16 C18 108.3(6) . . ?
O2 C16 C13 102.6(5) . . ?
C17 C16 C13 114.6(6) . . ?
C18 C16 C13 113.0(6) . . ?
O4 C19 C20 110.4(8) . . ?
O4 C19 C21 106.0(8) . . ?
C20 C19 C21 111.8(8) . . ?
O4 C19 C22 100.6(7) . . ?
C20 C19 C22 116.0(9) . . ?
C21 C19 C22 111.1(8) . . ?
O5 C22 C24 108.8(8) . . ?
O5 C22 C23 105.2(8) . . ?
C24 C22 C23 108.0(8) . . ?
O5 C22 C19 104.3(7) . . ?
C24 C22 C19 116.6(9) . . ?
C23 C22 C19 113.1(8) . . ?
O7 C25 C26 107.9(8) . . ?
O7 C25 C27 107.3(8) . . ?
C26 C25 C27 107.7(8) . . ?
O7 C25 C28 103.6(7) . . ?
C26 C25 C28 113.9(9) . . ?
C27 C25 C28 115.9(9) . . ?
O8 C28 C29 109.1(9) . . ?
O8 C28 C30 104.2(9) . . ?
C29 C28 C30 110.9(9) . . ?
O8 C28 C25 103.1(7) . . ?
C29 C28 C25 115.1(10) . . ?
C30 C28 C25 113.4(10) . . ?
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 N1 1.648(6) . ?
P1 C5 1.844(8) . ?
P1 C9 1.859(8) . ?
P1 C1 1.874(9) . ?
C1 C2 1.512(10) . ?
C1 C3 1.563(9) . ?
C1 C4 1.565(10) . ?
C5 C6 1.517(9) . ?
C5 C7 1.536(10) . ?
C5 C8 1.554(10) . ?
C9 C12 1.532(9) . ?
C9 C10 1.535(9) . ?
C9 C11 1.568(9) . ?
B1 O6 1.454(9) . ?
B1 O2 1.455(8) . ?
B1 O3 1.466(9) . ?
B1 O1 1.492(8) . ?
B2 O3 1.308(8) . ?
B2 O4 1.368(8) . ?
B2 O5 1.372(8) . ?
B3 O6 1.289(10) . ?
B3 O7 1.342(9) . ?
B3 O8 1.401(10) . ?
O1 C13 1.407(7) . ?
O2 C16 1.417(7) . ?
O4 C19 1.447(9) . ?
O5 C22 1.427(8) . ?
O7 C25 1.436(9) . ?
O8 C28 1.416(9) . ?
C13 C14 1.527(9) . ?
C13 C15 1.534(9) . ?
C13 C16 1.567(8) . ?
C16 C17 1.522(8) . ?
C16 C18 1.526(8) . ?
C19 C20 1.499(11) . ?
C19 C21 1.524(11) . ?
C19 C22 1.553(11) . ?
C22 C24 1.486(10) . ?
C22 C23 1.533(10) . ?
C25 C26 1.475(11) . ?
C25 C27 1.496(11) . ?
C25 C28 1.519(11) . ?
C28 C29 1.496(12) . ?
C28 C30 1.496(11) . ?
