#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:30:31 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179582 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/47/4504714.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_4504714
loop_
_publ_author_name
'Visi, Mandana Z.'
'Knobler, Carolyn B.'
'Owen, Jonathan J.'
'Khan, M. Ishaque'
'Schubert, David M.'
_publ_section_title
;
 Structures of Self-Assembled Nonmetal Borates Derived from
 α,ω-Diaminoalkanes
;
_journal_issue                   2
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              538
_journal_paper_doi               10.1021/cg0504915
_journal_volume                  6
_journal_year                    2006
_chemical_formula_moiety         'C10 H26 N2, 2(B5 H4 O10)'
_chemical_formula_sum            'C10 H34 B10 N2 O20'
_chemical_formula_weight         610.50
_chemical_name_common            '1,10-diammoniodecane bispentaborate'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 90.0720(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3759(6)
_cell_length_b                   14.0370(9)
_cell_length_c                   10.5878(7)
_cell_measurement_reflns_used    6559
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.17
_cell_volume                     1393.45(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      298(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0173
_diffrn_reflns_av_sigmaI/netI    0.0146
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12285
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.717
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.717
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0350
_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)+(0.1407P)²+0.2511P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1320
_reflns_number_gt                2836
_reflns_number_total             3385
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0504915si20051107_091537.cif
_cod_data_source_block           compound_6
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4504714
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
B1 B 0.79353(10) 0.13686(8) 0.11673(10) 0.0248(2) Uani 1 1 d .
B2A B 0.62058(12) 0.20670(9) -0.03336(11) 0.0289(2) Uani 1 1 d .
B2B B 0.54061(11) 0.08755(8) 0.11103(11) 0.0262(2) Uani 1 1 d .
B2C B 1.05356(11) 0.10958(8) 0.11176(11) 0.0272(2) Uani 1 1 d .
B2D B 0.96122(12) 0.22626(9) 0.25088(11) 0.0302(2) Uani 1 1 d .
O1A O 0.67712(7) 0.07254(5) 0.14967(7) 0.02771(18) Uani 1 1 d .
O2A O 0.43808(8) 0.02887(6) 0.15534(9) 0.0397(2) Uani 1 1 d .
H2A H 0.3544(19) 0.0442(12) 0.1321(16) 0.048 Uiso 1 1 d .
O3A O 0.50870(7) 0.15958(5) 0.02572(7) 0.02953(19) Uani 1 1 d .
O1B O 0.75707(7) 0.19384(5) 0.00485(7) 0.03110(19) Uani 1 1 d .
O2B O 1.16873(8) 0.06343(6) 0.06376(8) 0.0370(2) Uani 1 1 d .
H2B H 1.1414(16) 0.0223(12) 0.0187(15) 0.044 Uiso 1 1 d .
O3B O 1.07666(8) 0.18676(6) 0.18870(8) 0.0348(2) Uani 1 1 d .
O1C O 0.91939(7) 0.07897(5) 0.08500(7) 0.02907(19) Uani 1 1 d .
O2C O 0.99419(9) 0.29287(7) 0.33958(9) 0.0449(2) Uani 1 1 d .
H2C H 0.928(2) 0.3050(12) 0.3792(18) 0.054 Uiso 1 1 d .
O1D O 0.82598(7) 0.19926(5) 0.22428(7) 0.03060(19) Uani 1 1 d .
O2D O 0.58374(9) 0.26375(8) -0.13077(9) 0.0478(3) Uani 1 1 d .
H2D H 0.6581(19) 0.2859(13) -0.1693(18) 0.057 Uiso 1 1 d .
N1C N 0.69978(11) 0.87011(8) 0.19332(10) 0.0394(2) Uani 1 1 d .
H1C1 H 0.6438(19) 0.8487(13) 0.1243(18) 0.059 Uiso 1 1 d .
H1C2 H 0.7935(19) 0.8465(12) 0.1847(17) 0.059 Uiso 1 1 d .
H1C3 H 0.7039(18) 0.9344(14) 0.1849(17) 0.059 Uiso 1 1 d .
C2C C 0.63135(16) 0.84097(12) 0.31407(14) 0.0552(4) Uani 1 1 d .
H2C1 H 0.6238 0.7721 0.3165 0.066 Uiso 1 1 calc R
H2C2 H 0.5356 0.8670 0.3175 0.066 Uiso 1 1 calc R
C3C C 0.71442(18) 0.87465(12) 0.42817(14) 0.0577(4) Uani 1 1 d .
H3C1 H 0.6735 0.8457 0.5030 0.069 Uiso 1 1 calc R
H3C2 H 0.8118 0.8521 0.4209 0.069 Uiso 1 1 calc R
C4C C 0.71717(17) 0.98134(12) 0.44617(15) 0.0592(4) Uani 1 1 d .
H4C1 H 0.6200 1.0041 0.4555 0.071 Uiso 1 1 calc R
H4C2 H 0.7566 1.0106 0.3709 0.071 Uiso 1 1 calc R
C5C C 0.80434(14) 1.01336(11) 0.56080(11) 0.0722(5) Uani 1 1 d .
H5C1 H 0.8002 1.0823 0.5665 0.087 Uiso 1 1 calc R
H5C2 H 0.7606 0.9877 0.6365 0.087 Uiso 1 1 calc R
C6C C 0.95926(14) 0.98307(11) 0.55762(11) 0.0659(5) Uani 1 1 d R
H6C1 H 0.9636 0.9141 0.5608 0.079 Uiso 1 1 calc R
H6C2 H 1.0064 1.0072 0.6327 0.079 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'
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_3
O1A B1 O1D 109.76(8) .
O1A B1 O1B 110.87(7) .
O1D B1 O1B 110.38(9) .
O1A B1 O1C 108.25(8) .
O1D B1 O1C 109.93(7) .
O1B B1 O1C 107.59(7) .
O2D B2A O1B 123.24(10) .
O2D B2A O3A 115.70(9) .
O1B B2A O3A 121.06(9) .
O2A B2B O1A 118.11(9) .
O2A B2B O3A 121.16(9) .
O1A B2B O3A 120.71(9) .
O2B B2C O1C 120.49(9) .
O2B B2C O3B 118.27(9) .
O1C B2C O3B 121.24(9) .
O1D B2D O2C 123.26(10) .
O1D B2D O3B 121.49(9) .
O2C B2D O3B 115.26(9) .
B2B O1A B1 122.44(8) .
B2B O3A B2A 118.52(8) .
B2A O1B B1 122.16(8) .
B2C O3B B2D 118.42(8) .
B2C O1C B1 121.34(8) .
B2D O1D B1 121.46(8) .
N1C C2C C3C 112.21(11) .
C4C C3C C2C 114.81(13) .
C3C C4C C5C 113.61(13) .
C6C C5C C4C 114.30(8) .
C5C C6C C6C 114.46(11) 3_776
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
B1 O1A 1.4590(12) .
B1 O1D 1.4682(12) .
B1 O1B 1.4694(13) .
B1 O1C 1.4719(12) .
B2A O2D 1.3503(14) .
B2A O1B 1.3538(13) .
B2A O3A 1.3894(13) .
B2B O2A 1.3505(13) .
B2B O1A 1.3597(12) .
B2B O3A 1.3882(13) .
B2C O2B 1.3584(13) .
B2C O1C 1.3588(12) .
B2C O3B 1.3725(13) .
B2D O1D 1.3528(13) .
B2D O2C 1.3605(14) .
B2D O3B 1.3835(14) .
N1C C2C 1.4885(17) .
C2C C3C 1.512(2) .
C3C C4C 1.510(2) .
C4C C5C 1.5298(19) .
C5C C6C 1.5139 .
C6C C6C 1.517(2) 3_776
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2A H2A O2B 0.849(18) 1.904(18) 2.7472(11) 171.8(16) 1_455
O2B H2B O1C 0.792(17) 1.884(17) 2.6750(11) 177.8(17) 3_755
O2C H2C O1B 0.769(19) 2.083(19) 2.8371(11) 166.4(17) 4_566
O2D H2D O1D 0.866(18) 1.948(18) 2.7915(11) 164.2(17) 4_565
N1C H1C1 O3A 0.948(19) 2.139(19) 3.0597(13) 163.4(15) 3_665
N1C H1C2 O2C 0.943(18) 2.144(18) 3.0874(14) 178.6(16) 2_755
N1C H1C3 O1A 0.908(19) 1.99(2) 2.8867(13) 169.0(16) 1_565
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_4
O2A B2B O1A B1 -174.27(9) .
O3A B2B O1A B1 7.48(15) .
O1D B1 O1A B2B 101.15(10) .
O1B B1 O1A B2B -21.05(13) .
O1C B1 O1A B2B -138.85(9) .
O2A B2B O3A B2A -168.88(10) .
O1A B2B O3A B2A 9.32(15) .
O2D B2A O3A B2B 168.77(10) .
O1B B2A O3A B2B -10.23(15) .
O2D B2A O1B B1 175.51(10) .
O3A B2A O1B B1 -5.56(15) .
O1A B1 O1B B2A 20.09(13) .
O1D B1 O1B B2A -101.76(10) .
O1C B1 O1B B2A 138.28(9) .
O2B B2C O3B B2D -171.69(10) .
O1C B2C O3B B2D 7.56(16) .
O1D B2D O3B B2C -9.18(17) .
O2C B2D O3B B2C 170.55(10) .
O2B B2C O1C B1 -169.06(9) .
O3B B2C O1C B1 11.71(15) .
O1A B1 O1C B2C -146.39(9) .
O1D B1 O1C B2C -26.50(13) .
O1B B1 O1C B2C 93.74(10) .
O2C B2D O1D B1 171.71(10) .
O3B B2D O1D B1 -8.58(16) .
O1A B1 O1D B2D 143.88(9) .
O1B B1 O1D B2D -93.62(11) .
O1C B1 O1D B2D 24.91(13) .
N1C C2C C3C C4C 66.87(19) .
C2C C3C C4C C5C -178.88(13) .
C3C C4C C5C C6C 59.01(14) .
C4C C5C C6C C6C 57.37(11) 3_776
