#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:40:22 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180191 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/87/7108712.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_7108712
loop_
_publ_author_name
'Mirela Pascu'
'Albert Ruggi'
'Rosario Scopelliti'
'Kay Severin'
_publ_section_title
;
 Synthesis of borasiloxane-based macrocycles by multicomponent
 condensation reactions in solution or in a ball mill
;
_journal_name_full               Chem.Commun.
_journal_page_first              45
_journal_paper_doi               10.1039/c2cc37538a
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C30 H46 B2 O6 Si2'
_chemical_formula_sum            'C30 H46 B2 O6 Si2'
_chemical_formula_weight         580.47
_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
_audit_update_record
;
2012-10-30 # Formatted by publCIF
;
_cell_angle_alpha                109.911(7)
_cell_angle_beta                 94.902(8)
_cell_angle_gamma                109.903(7)
_cell_formula_units_Z            1
_cell_length_a                   8.4713(9)
_cell_length_b                   10.5851(7)
_cell_length_c                   10.6720(11)
_cell_measurement_reflns_used    161
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      3
_cell_volume                     823.76(15)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs, 1990-2000)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10453
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008, Bruker AXS, 2008'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             312
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3753
_refine_ls_number_restraints     330
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0485
_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)+(0.0444P)²+0.4927P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1194
_reflns_number_gt                2981
_reflns_number_total             3753
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc37538a.txt
_cod_data_source_block           mp016
_cod_original_cell_volume        823.76(13)
_cod_database_code               7108712
#BEGIN Tags that were not found in dictionaries:
#END Tags that were not found in dictionaries
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
Si1 Si 0.38093(6) 0.39018(5) 0.11700(5) 0.01594(14) Uani 1 1 d . . .
O1 O 0.31425(16) 0.33333(13) -0.04928(13) 0.0207(3) Uani 1 1 d . A .
O2 O 0.42557(16) 0.47759(13) -0.17642(13) 0.0204(3) Uani 1 1 d . . .
B1 B 0.3021(2) 0.3648(2) -0.1623(2) 0.0156(4) Uani 1 1 d . . .
C1 C 0.4057(2) 0.23112(19) 0.14622(19) 0.0199(4) Uani 1 1 d . . .
C2 C 0.2421(3) 0.0900(2) 0.0774(2) 0.0297(5) Uani 1 1 d . . .
H2A H 0.2615 0.0099 0.0931 0.045 Uiso 1 1 calc R . .
H2B H 0.2146 0.0657 -0.0212 0.045 Uiso 1 1 calc R . .
H2C H 0.1459 0.1044 0.1164 0.045 Uiso 1 1 calc R . .
C3 C 0.5542(3) 0.2060(2) 0.0818(2) 0.0300(5) Uani 1 1 d . . .
H3A H 0.5744 0.1266 0.0983 0.045 Uiso 1 1 calc R . .
H3B H 0.6592 0.2957 0.1231 0.045 Uiso 1 1 calc R . .
H3C H 0.5234 0.1796 -0.0170 0.045 Uiso 1 1 calc R . .
C4 C 0.4542(3) 0.2661(2) 0.3002(2) 0.0349(5) Uani 1 1 d . . .
H4A H 0.3572 0.2746 0.3414 0.052 Uiso 1 1 calc R . .
H4B H 0.5553 0.3586 0.3446 0.052 Uiso 1 1 calc R . .
H4C H 0.4808 0.1874 0.3127 0.052 Uiso 1 1 calc R . .
C5 C 0.2316(2) 0.4725(2) 0.2000(2) 0.0231(4) Uani 1 1 d . . .
C6 C 0.2965(3) 0.5470(2) 0.3570(2) 0.0339(5) Uani 1 1 d . . .
H6A H 0.2234 0.5973 0.3964 0.051 Uiso 1 1 calc R . .
H6B H 0.4157 0.6181 0.3806 0.051 Uiso 1 1 calc R . .
H6C H 0.2915 0.4729 0.3938 0.051 Uiso 1 1 calc R . .
C7 C 0.2304(3) 0.5912(2) 0.1465(2) 0.0339(5) Uani 1 1 d . . .
H7A H 0.1891 0.5462 0.0467 0.051 Uiso 1 1 calc R . .
H7B H 0.3475 0.6662 0.1710 0.051 Uiso 1 1 calc R . .
H7C H 0.1538 0.6363 0.1879 0.051 Uiso 1 1 calc R . .
C8 C 0.0462(3) 0.3589(3) 0.1633(3) 0.0366(5) Uani 1 1 d . . .
H8A H 0.0435 0.2856 0.2006 0.055 Uiso 1 1 calc R . .
H8B H 0.0052 0.3109 0.0636 0.055 Uiso 1 1 calc R . .
H8C H -0.0284 0.4076 0.2024 0.055 Uiso 1 1 calc R . .
C9A C 0.1398(14) 0.2712(14) -0.2935(10) 0.0185(13) Uani 0.298(5) 1 d PGU A 1
C10A C 0.1314(12) 0.3042(12) -0.4087(11) 0.0178(12) Uani 0.298(5) 1 d PGU A 1
H10A H 0.2235 0.3835 -0.4131 0.021 Uiso 0.298(5) 1 calc PR A 1
C11A C -0.0119(12) 0.2211(11) -0.5175(9) 0.0172(12) Uani 0.298(5) 1 d PGU A 1
H11A H -0.0177 0.2437 -0.5963 0.021 Uiso 0.298(5) 1 calc PR A 1
C12A C -0.1467(11) 0.1052(10) -0.5112(8) 0.0184(12) Uani 0.298(5) 1 d PGU A 1
C13A C -0.1383(14) 0.0722(10) -0.3960(9) 0.0180(12) Uani 0.298(5) 1 d PGU A 1
H13A H -0.2305 -0.0071 -0.3916 0.022 Uiso 0.298(5) 1 calc PR A 1
C14A C 0.0050(16) 0.1553(13) -0.2871(9) 0.0171(11) Uani 0.298(5) 1 d PGU A 1
H14A H 0.0107 0.1327 -0.2084 0.021 Uiso 0.298(5) 1 calc PR A 1
O3A O -0.4302(8) -0.0794(7) -0.6313(6) 0.0456(17) Uani 0.298(5) 1 d PU A 1
C15A C -0.2976(13) 0.0163(10) -0.6295(10) 0.0245(14) Uani 0.298(5) 1 d PU A 1
H15A H -0.2905 0.0353 -0.7101 0.029 Uiso 0.298(5) 1 calc PR A 1
C9B C 0.1319(6) 0.2623(6) -0.2818(4) 0.0138(7) Uani 0.702(5) 1 d PGU A 2
C10B C 0.1112(5) 0.2906(5) -0.3988(4) 0.0196(7) Uani 0.702(5) 1 d PGU A 2
H10B H 0.1983 0.3697 -0.4079 0.023 Uiso 0.702(5) 1 calc PR A 2
C11B C -0.0370(5) 0.2030(4) -0.5026(3) 0.0219(7) Uani 0.702(5) 1 d PGU A 2
H11B H -0.0512 0.2223 -0.5825 0.026 Uiso 0.702(5) 1 calc PR A 2
C12B C -0.1644(4) 0.0871(4) -0.4893(3) 0.0196(7) Uani 0.702(5) 1 d PGU A 2
C13B C -0.1437(6) 0.0589(4) -0.3723(4) 0.0203(7) Uani 0.702(5) 1 d PGU A 2
H13B H -0.2308 -0.0203 -0.3633 0.024 Uiso 0.702(5) 1 calc PR A 2
C14B C 0.0045(7) 0.1464(5) -0.2686(4) 0.0183(7) Uani 0.702(5) 1 d PGU A 2
H14B H 0.0186 0.1271 -0.1886 0.022 Uiso 0.702(5) 1 calc PR A 2
O3B O -0.3549(3) -0.0010(3) -0.7097(3) 0.0431(8) Uani 0.702(5) 1 d PU A 2
C15B C -0.3235(5) -0.0101(4) -0.6006(4) 0.0272(8) Uani 0.702(5) 1 d PU A 2
H15B H -0.4076 -0.0857 -0.5846 0.033 Uiso 0.702(5) 1 calc PR A 2
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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
O1 Si1 O2 112.49(7) . 2_665
O1 Si1 C5 107.15(8) . .
O2 Si1 C5 105.74(8) 2_665 .
O1 Si1 C1 105.83(8) . .
O2 Si1 C1 105.23(8) 2_665 .
C5 Si1 C1 120.55(8) . .
B1 O1 Si1 149.22(12) . .
B1 O2 Si1 148.54(13) . 2_665
O2 B1 O1 123.15(17) . .
O2 B1 C9B 119.8(2) . .
O1 B1 C9B 117.0(2) . .
O2 B1 C9A 113.3(4) . .
O1 B1 C9A 123.5(4) . .
C2 C1 C4 109.67(16) . .
C2 C1 C3 108.34(16) . .
C4 C1 C3 108.41(17) . .
C2 C1 Si1 112.18(13) . .
C4 C1 Si1 111.10(13) . .
C3 C1 Si1 107.00(12) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C1 C3 H3A 109.5 . .
C1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C1 C4 H4A 109.5 . .
C1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C8 C5 C6 109.37(17) . .
C8 C5 C7 108.30(17) . .
C6 C5 C7 108.00(17) . .
C8 C5 Si1 112.25(14) . .
C6 C5 Si1 111.32(14) . .
C7 C5 Si1 107.44(13) . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C5 C7 H7A 109.5 . .
C5 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C5 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C5 C8 H8A 109.5 . .
C5 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C5 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C10A C9A C14A 120.0 . .
C10A C9A B1 122.5(6) . .
C14A C9A B1 117.5(6) . .
C11A C10A C9A 120.0 . .
C11A C10A H10A 120.0 . .
C9A C10A H10A 120.0 . .
C12A C11A C10A 120.0 . .
C12A C11A H11A 120.0 . .
C10A C11A H11A 120.0 . .
C11A C12A C13A 120.0 . .
C11A C12A C15A 119.2(6) . .
C13A C12A C15A 120.8(6) . .
C14A C13A C12A 120.0 . .
C14A C13A H13A 120.0 . .
C12A C13A H13A 120.0 . .
C13A C14A C9A 120.0 . .
C13A C14A H14A 120.0 . .
C9A C14A H14A 120.0 . .
O3A C15A C12A 125.2(9) . .
O3A C15A H15A 117.4 . .
C12A C15A H15A 117.4 . .
C10B C9B C14B 120.0 . .
C10B C9B B1 119.6(3) . .
C14B C9B B1 120.4(3) . .
C11B C10B C9B 120.0 . .
C11B C10B H10B 120.0 . .
C9B C10B H10B 120.0 . .
C12B C11B C10B 120.0 . .
C12B C11B H11B 120.0 . .
C10B C11B H11B 120.0 . .
C11B C12B C13B 120.0 . .
C11B C12B C15B 120.9(2) . .
C13B C12B C15B 119.1(2) . .
C14B C13B C12B 120.0 . .
C14B C13B H13B 120.0 . .
C12B C13B H13B 120.0 . .
C13B C14B C9B 120.0 . .
C13B C14B H14B 120.0 . .
C9B C14B H14B 120.0 . .
O3B C15B C12B 125.8(4) . .
O3B C15B H15B 117.1 . .
C12B C15B H15B 117.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 O1 1.6431(13) .
Si1 O2 1.6443(13) 2_665
Si1 C5 1.8864(19) .
Si1 C1 1.8876(18) .
O1 B1 1.361(2) .
O2 B1 1.357(2) .
O2 Si1 1.6443(13) 2_665
B1 C9B 1.601(3) .
B1 C9A 1.622(7) .
C1 C2 1.536(3) .
C1 C4 1.541(3) .
C1 C3 1.542(3) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 C8 1.534(3) .
C5 C6 1.543(3) .
C5 C7 1.550(3) .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9A C10A 1.3900 .
C9A C14A 1.3900 .
C10A C11A 1.3900 .
C10A H10A 0.9500 .
C11A C12A 1.3900 .
C11A H11A 0.9500 .
C12A C13A 1.3900 .
C12A C15A 1.486(12) .
C13A C14A 1.3900 .
C13A H13A 0.9500 .
C14A H14A 0.9500 .
O3A C15A 1.223(11) .
C15A H15A 0.9500 .
C9B C10B 1.3900 .
C9B C14B 1.3900 .
C10B C11B 1.3900 .
C10B H10B 0.9500 .
C11B C12B 1.3900 .
C11B H11B 0.9500 .
C12B C13B 1.3900 .
C12B C15B 1.495(5) .
C13B C14B 1.3900 .
C13B H13B 0.9500 .
C14B H14B 0.9500 .
O3B C15B 1.215(5) .
C15B H15B 0.9500 .
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
O2 Si1 O1 B1 -40.1(3) 2_665
C5 Si1 O1 B1 75.7(3) .
C1 Si1 O1 B1 -154.5(2) .
Si1 O2 B1 O1 7.2(4) 2_665
Si1 O2 B1 C9B -173.2(3) 2_665
Si1 O2 B1 C9A -172.5(7) 2_665
Si1 O1 B1 O2 32.8(4) .
Si1 O1 B1 C9B -146.8(3) .
Si1 O1 B1 C9A -147.5(8) .
O1 Si1 C1 C2 -52.29(15) .
O2 Si1 C1 C2 -171.59(13) 2_665
C5 Si1 C1 C2 69.25(16) .
O1 Si1 C1 C4 -175.46(13) .
O2 Si1 C1 C4 65.25(15) 2_665
C5 Si1 C1 C4 -53.91(17) .
O1 Si1 C1 C3 66.38(14) .
O2 Si1 C1 C3 -52.91(14) 2_665
C5 Si1 C1 C3 -172.07(13) .
O1 Si1 C5 C8 64.23(16) .
O2 Si1 C5 C8 -175.57(14) 2_665
C1 Si1 C5 C8 -56.67(18) .
O1 Si1 C5 C6 -172.79(13) .
O2 Si1 C5 C6 -52.59(15) 2_665
C1 Si1 C5 C6 66.31(16) .
O1 Si1 C5 C7 -54.73(15) .
O2 Si1 C5 C7 65.47(15) 2_665
C1 Si1 C5 C7 -175.63(13) .
O2 B1 C9A C10A 0.7(10) .
O1 B1 C9A C10A -179.1(5) .
C9B B1 C9A C10A 175(8) .
O2 B1 C9A C14A -178.6(5) .
O1 B1 C9A C14A 1.6(11) .
C9B B1 C9A C14A -4(7) .
C14A C9A C10A C11A 0.0 .
B1 C9A C10A C11A -179.3(12) .
C9A C10A C11A C12A 0.0 .
C10A C11A C12A C13A 0.0 .
C10A C11A C12A C15A -179.1(10) .
C11A C12A C13A C14A 0.0 .
C15A C12A C13A C14A 179.1(10) .
C12A C13A C14A C9A 0.0 .
C10A C9A C14A C13A 0.0 .
B1 C9A C14A C13A 179.3(12) .
C11A C12A C15A O3A -173.0(9) .
C13A C12A C15A O3A 7.9(14) .
O2 B1 C9B C10B -0.6(5) .
O1 B1 C9B C10B 179.0(2) .
C9A B1 C9B C10B -6(7) .
O2 B1 C9B C14B -180.0(2) .
O1 B1 C9B C14B -0.4(4) .
C9A B1 C9B C14B 174(8) .
C14B C9B C10B C11B 0.0 .
B1 C9B C10B C11B -179.4(5) .
C9B C10B C11B C12B 0.0 .
C10B C11B C12B C13B 0.0 .
C10B C11B C12B C15B -179.0(4) .
C11B C12B C13B C14B 0.0 .
C15B C12B C13B C14B 179.0(4) .
C12B C13B C14B C9B 0.0 .
C10B C9B C14B C13B 0.0 .
B1 C9B C14B C13B 179.4(5) .
C11B C12B C15B O3B 1.8(6) .
C13B C12B C15B O3B -177.2(4) .
