#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:12:40 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180128 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/26/7102644.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_7102644
loop_
_publ_author_name
N.Christinat
R.Scopelliti
K.Severin
_publ_section_title
;
A new method for the synthesis of boronate macrocycles
;
_journal_issue                   10
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1158
_journal_page_last               1159
_journal_paper_doi               10.1039/b402510e
_journal_year                    2004
_chemical_formula_moiety         'C44 H32 B4 N4 O8'
_chemical_formula_sum            'C44 H32 B4 N4 O8'
_chemical_formula_weight         787.98
_chemical_name_systematic
;
?
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.7128(8)
_cell_length_b                   16.7128(8)
_cell_length_c                   13.9916(11)
_cell_measurement_reflns_used    4771
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      26.81185
_cell_measurement_theta_min      3.058
_cell_volume                     3908.1(4)
_computing_cell_refinement       'Oxford Diffraction CrysAlis RED'
_computing_data_collection       'Oxford Diffraction CrysAlis CCD'
_computing_data_reduction        'Oxford Diffraction CrysAlis RED'
_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      140(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Diffraction KM4/Sapphire 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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11750
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.555
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.177
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.0004(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0347
_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)+(0.0553P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0943
_reflns_number_gt                1445
_reflns_number_total             1729
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b402510e.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      I4(1)/a
_cod_database_code               7102644
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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
O1 O 0.38001(6) -0.23523(6) 0.08966(7) 0.0175(3) Uani 1 1 d .
O2 O 0.34729(6) -0.10489(6) 0.14639(7) 0.0190(3) Uani 1 1 d .
N1 N 0.37030(7) -0.30133(7) 0.23745(8) 0.0170(3) Uani 1 1 d .
C1 C 0.36622(8) -0.23555(8) 0.18279(10) 0.0158(3) Uani 1 1 d .
C2 C 0.34634(8) -0.15913(8) 0.21845(10) 0.0169(3) Uani 1 1 d .
C3 C 0.32879(9) -0.14964(9) 0.31337(11) 0.0206(4) Uani 1 1 d .
H3 H 0.3154 -0.0988 0.3393 0.025 Uiso 1 1 calc R
C4 C 0.33151(9) -0.21901(9) 0.37080(10) 0.0227(4) Uani 1 1 d .
H4 H 0.3189 -0.2151 0.4368 0.027 Uiso 1 1 calc R
C5 C 0.35192(9) -0.29155(9) 0.33349(10) 0.0202(4) Uani 1 1 d .
H5 H 0.3536 -0.3368 0.3745 0.024 Uiso 1 1 calc R
C6 C 0.29263(8) -0.14383(9) -0.01929(10) 0.0177(4) Uani 1 1 d .
C7 C 0.27489(9) -0.20499(9) -0.08481(11) 0.0230(4) Uani 1 1 d .
H7 H 0.3094 -0.2501 -0.0889 0.028 Uiso 1 1 calc R
C8 C 0.20794(10) -0.20106(10) -0.14382(11) 0.0271(4) Uani 1 1 d .
H8 H 0.1972 -0.2433 -0.1874 0.033 Uiso 1 1 calc R
C9 C 0.15682(10) -0.13565(10) -0.13920(11) 0.0281(4) Uani 1 1 d .
H9 H 0.1110 -0.1331 -0.1792 0.034 Uiso 1 1 calc R
C10 C 0.17320(9) -0.07397(10) -0.07567(12) 0.0255(4) Uani 1 1 d .
H10 H 0.1388 -0.0288 -0.0726 0.031 Uiso 1 1 calc R
C11 C 0.24029(9) -0.07826(9) -0.01629(11) 0.0213(4) Uani 1 1 d .
H11 H 0.2507 -0.0358 0.0271 0.026 Uiso 1 1 calc R
B1 B 0.36505(10) -0.14949(10) 0.05611(12) 0.0181(4) Uani 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'
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'
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
C1 O1 B1 106.12(11) . .
C2 O2 B1 107.28(11) . .
C1 N1 C5 116.38(12) . .
C1 N1 B1 120.93(12) . 12_656
C5 N1 B1 122.61(12) . 12_656
O1 C1 N1 123.79(13) . .
O1 C1 C2 112.68(12) . .
N1 C1 C2 123.54(13) . .
O2 C2 C3 130.26(13) . .
O2 C2 C1 109.85(12) . .
C3 C2 C1 119.89(13) . .
C2 C3 C4 116.75(14) . .
C2 C3 H3 121.6 . .
C4 C3 H3 121.6 . .
C5 C4 C3 121.37(14) . .
C5 C4 H4 119.3 . .
C3 C4 H4 119.3 . .
C4 C5 N1 122.06(14) . .
C4 C5 H5 119.0 . .
N1 C5 H5 119.0 . .
C11 C6 C7 117.15(14) . .
C11 C6 B1 119.71(13) . .
C7 C6 B1 122.97(14) . .
C8 C7 C6 121.50(15) . .
C8 C7 H7 119.2 . .
C6 C7 H7 119.2 . .
C9 C8 C7 120.25(15) . .
C9 C8 H8 119.9 . .
C7 C8 H8 119.9 . .
C10 C9 C8 119.54(14) . .
C10 C9 H9 120.2 . .
C8 C9 H9 120.2 . .
C9 C10 C11 120.05(15) . .
C9 C10 H10 120.0 . .
C11 C10 H10 120.0 . .
C10 C11 C6 121.52(14) . .
C10 C11 H11 119.2 . .
C6 C11 H11 119.2 . .
O2 B1 O1 103.90(11) . .
O2 B1 N1 110.05(12) . 15_655
O1 B1 N1 105.07(11) . 15_655
O2 B1 C6 112.03(12) . .
O1 B1 C6 112.31(12) . .
N1 B1 C6 112.91(12) 15_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C1 1.3233(16) .
O1 B1 1.5285(19) .
O2 C2 1.3559(17) .
O2 B1 1.4964(19) .
N1 C1 1.3409(18) .
N1 C5 1.3880(18) .
N1 B1 1.601(2) 12_656
C1 C2 1.4108(19) .
C2 C3 1.369(2) .
C3 C4 1.411(2) .
C3 H3 0.9500 .
C4 C5 1.363(2) .
C4 H4 0.9500 .
C5 H5 0.9500 .
C6 C11 1.403(2) .
C6 C7 1.405(2) .
C6 B1 1.608(2) .
C7 C8 1.392(2) .
C7 H7 0.9500 .
C8 C9 1.389(2) .
C8 H8 0.9500 .
C9 C10 1.388(2) .
C9 H9 0.9500 .
C10 C11 1.397(2) .
C10 H10 0.9500 .
C11 H11 0.9500 .
B1 N1 1.601(2) 15_655
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_4
B1 O1 C1 N1 177.46(13) . .
B1 O1 C1 C2 -2.27(15) . .
C5 N1 C1 O1 -178.30(13) . .
B1 N1 C1 O1 4.9(2) 12_656 .
C5 N1 C1 C2 1.4(2) . .
B1 N1 C1 C2 -175.44(13) 12_656 .
B1 O2 C2 C3 -176.07(15) . .
B1 O2 C2 C1 2.96(16) . .
O1 C1 C2 O2 -0.41(17) . .
N1 C1 C2 O2 179.86(12) . .
O1 C1 C2 C3 178.73(12) . .
N1 C1 C2 C3 -1.0(2) . .
O2 C2 C3 C4 178.69(14) . .
C1 C2 C3 C4 -0.3(2) . .
C2 C3 C4 C5 1.0(2) . .
C3 C4 C5 N1 -0.6(2) . .
C1 N1 C5 C4 -0.6(2) . .
B1 N1 C5 C4 176.19(13) 12_656 .
C11 C6 C7 C8 -0.4(2) . .
B1 C6 C7 C8 174.73(14) . .
C6 C7 C8 C9 0.2(2) . .
C7 C8 C9 C10 0.4(2) . .
C8 C9 C10 C11 -0.6(2) . .
C9 C10 C11 C6 0.3(2) . .
C7 C6 C11 C10 0.2(2) . .
B1 C6 C11 C10 -175.14(13) . .
C2 O2 B1 O1 -4.10(14) . .
C2 O2 B1 N1 -116.14(12) . 15_655
C2 O2 B1 C6 117.37(13) . .
C1 O1 B1 O2 3.83(14) . .
C1 O1 B1 N1 119.45(11) . 15_655
C1 O1 B1 C6 -117.45(13) . .
C11 C6 B1 O2 25.96(19) . .
C7 C6 B1 O2 -149.10(13) . .
C11 C6 B1 O1 142.45(13) . .
C7 C6 B1 O1 -32.61(19) . .
C11 C6 B1 N1 -98.97(15) . 15_655
C7 C6 B1 N1 85.97(17) . 15_655
