#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:00:22 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180164 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/60/7106071.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_7106071
loop_
_publ_author_name
'Ahmed Al-Harbi'
'Wesley Sattler'
'Aaron Sattler'
'Gerard Parkin'
_publ_section_title
;
 Synthesis and Structural Characterization of
 Tris(2-oxo-1-t-butylimidazolyl) and Tris(2-oxo-1-methylbenzimidazolyl)
 hydroborato Complexes: A New Class of Tripodal Oxygen Donor Ligand
;
_journal_name_full               Chem.Commun.
_journal_page_first              3123
_journal_paper_doi               10.1039/c0cc03943h
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C42 H68 B2 N12 Na2 O6'
_chemical_formula_weight         904.68
_chemical_name_systematic
;
?
;
_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                104.306(5)
_cell_angle_beta                 92.511(5)
_cell_angle_gamma                108.015(5)
_cell_formula_units_Z            1
_cell_length_a                   10.357(3)
_cell_length_b                   10.900(3)
_cell_length_c                   12.135(4)
_cell_measurement_reflns_used    2702
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.17
_cell_measurement_theta_min      2.30
_cell_volume                     1251.6(7)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0880
_diffrn_reflns_av_sigmaI/netI    0.1137
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15155
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.9974
_exptl_absorpt_correction_T_min  0.9909
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5123
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1517
_refine_ls_R_factor_gt           0.0568
_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)+(0.0200P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0932
_reflns_number_gt                2434
_reflns_number_total             5123
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC03943H.TXT
_cod_data_source_block           nattos10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1251.6(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7106071
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
Na Na 0.65148(10) 0.58627(10) -0.01897(8) 0.0451(3) Uani 1 1 d . . .
B B 0.4359(3) 0.3166(3) -0.2360(3) 0.0367(8) Uani 1 1 d . . .
H1 H 0.4611(19) 0.3406(19) -0.1380(17) 0.029(6) Uiso 1 1 d . . .
O1 O 0.22046(17) 0.20681(17) -0.09714(14) 0.0467(5) Uani 1 1 d . . .
O2 O 0.71638(17) 0.49951(17) -0.18714(15) 0.0476(5) Uani 1 1 d . . .
O3 O 0.42553(17) 0.57305(17) -0.08382(15) 0.0454(5) Uani 1 1 d . . .
N11 N 0.3058(2) 0.1919(2) -0.27490(17) 0.0347(6) Uani 1 1 d . . .
N12 N 0.0999(2) 0.0506(2) -0.26907(17) 0.0355(6) Uani 1 1 d . . .
N21 N 0.5600(2) 0.2910(2) -0.29192(17) 0.0372(6) Uani 1 1 d . . .
N22 N 0.7809(2) 0.3338(2) -0.31295(17) 0.0366(6) Uani 1 1 d . . .
N31 N 0.41116(19) 0.4374(2) -0.26899(18) 0.0356(6) Uani 1 1 d . . .
N32 N 0.3849(2) 0.6365(2) -0.24957(19) 0.0394(6) Uani 1 1 d . . .
C11 C 0.2105(3) 0.1551(3) -0.2026(2) 0.0364(7) Uani 1 1 d . . .
C12 C 0.2497(3) 0.1131(3) -0.3859(2) 0.0387(7) Uani 1 1 d . . .
H12A H 0.2911 0.1208 -0.4533 0.046 Uiso 1 1 calc R . .
C13 C 0.1272(3) 0.0242(3) -0.3822(2) 0.0376(7) Uani 1 1 d . . .
H13A H 0.0698 -0.0442 -0.4455 0.045 Uiso 1 1 calc R . .
C14 C -0.0219(3) -0.0230(2) -0.2234(2) 0.0352(7) Uani 1 1 d . . .
C15 C -0.1228(3) -0.1296(3) -0.3227(2) 0.0532(9) Uani 1 1 d . . .
H15A H -0.0776 -0.1907 -0.3638 0.080 Uiso 1 1 calc R . .
H15B H -0.1533 -0.0860 -0.3754 0.080 Uiso 1 1 calc R . .
H15C H -0.2020 -0.1804 -0.2925 0.080 Uiso 1 1 calc R . .
C16 C -0.0914(2) 0.0750(3) -0.1617(2) 0.0455(8) Uani 1 1 d . . .
H16A H -0.0247 0.1476 -0.1022 0.068 Uiso 1 1 calc R . .
H16B H -0.1674 0.0274 -0.1264 0.068 Uiso 1 1 calc R . .
H16C H -0.1265 0.1126 -0.2172 0.068 Uiso 1 1 calc R . .
C17 C 0.0226(3) -0.0917(3) -0.1414(2) 0.0508(8) Uani 1 1 d . . .
H17A H 0.0921 -0.0248 -0.0804 0.076 Uiso 1 1 calc R . .
H17B H 0.0611 -0.1584 -0.1833 0.076 Uiso 1 1 calc R . .
H17C H -0.0567 -0.1363 -0.1076 0.076 Uiso 1 1 calc R . .
C21 C 0.6883(3) 0.3858(3) -0.2571(2) 0.0378(7) Uani 1 1 d . . .
C22 C 0.5761(3) 0.1773(3) -0.3652(2) 0.0428(8) Uani 1 1 d . . .
H22A H 0.5051 0.0943 -0.3981 0.051 Uiso 1 1 calc R . .
C23 C 0.7093(3) 0.2048(3) -0.3818(2) 0.0405(7) Uani 1 1 d . . .
H23A H 0.7472 0.1467 -0.4313 0.049 Uiso 1 1 calc R . .
C24 C 0.9293(3) 0.4085(3) -0.3016(2) 0.0393(7) Uani 1 1 d . . .
C25 C 0.9917(3) 0.4460(3) -0.1770(2) 0.0590(9) Uani 1 1 d . . .
H25A H 0.9736 0.3647 -0.1510 0.088 Uiso 1 1 calc R . .
H25B H 0.9509 0.5071 -0.1293 0.088 Uiso 1 1 calc R . .
H25C H 1.0908 0.4904 -0.1703 0.088 Uiso 1 1 calc R . .
C26 C 0.9989(3) 0.3208(3) -0.3771(2) 0.0562(9) Uani 1 1 d . . .
H26A H 0.9884 0.2403 -0.3512 0.084 Uiso 1 1 calc R . .
H26B H 1.0965 0.3712 -0.3717 0.084 Uiso 1 1 calc R . .
H26C H 0.9565 0.2945 -0.4569 0.084 Uiso 1 1 calc R . .
C27 C 0.9460(3) 0.5335(3) -0.3415(2) 0.0563(9) Uani 1 1 d . . .
H27A H 0.9029 0.5908 -0.2920 0.084 Uiso 1 1 calc R . .
H27B H 0.9021 0.5075 -0.4208 0.084 Uiso 1 1 calc R . .
H27C H 1.0436 0.5828 -0.3375 0.084 Uiso 1 1 calc R . .
C31 C 0.4083(2) 0.5505(3) -0.1905(3) 0.0378(7) Uani 1 1 d . . .
C32 C 0.3936(3) 0.4550(3) -0.3786(2) 0.0441(8) Uani 1 1 d . . .
H32A H 0.3879 0.3906 -0.4492 0.053 Uiso 1 1 calc R . .
C33 C 0.3859(3) 0.5812(3) -0.3668(2) 0.0530(8) Uani 1 1 d . . .
H33A H 0.3820 0.6229 -0.4265 0.064 Uiso 1 1 calc R . .
C34 C 0.3992(3) 0.7793(3) -0.1941(3) 0.0501(8) Uani 1 1 d . . .
C35 C 0.3527(3) 0.8388(3) -0.2832(3) 0.0768(11) Uani 1 1 d . . .
H35A H 0.4167 0.8449 -0.3403 0.115 Uiso 1 1 calc R . .
H35B H 0.3506 0.9285 -0.2455 0.115 Uiso 1 1 calc R . .
H35C H 0.2609 0.7811 -0.3212 0.115 Uiso 1 1 calc R . .
C36 C 0.3082(3) 0.7855(3) -0.0983(2) 0.0561(9) Uani 1 1 d . . .
H36A H 0.3408 0.7525 -0.0381 0.084 Uiso 1 1 calc R . .
H36B H 0.2136 0.7294 -0.1296 0.084 Uiso 1 1 calc R . .
H36C H 0.3119 0.8784 -0.0659 0.084 Uiso 1 1 calc R . .
C37 C 0.5474(3) 0.8569(3) -0.1446(3) 0.0994(14) Uani 1 1 d . . .
H37A H 0.5724 0.8244 -0.0812 0.149 Uiso 1 1 calc R . .
H37B H 0.5591 0.9526 -0.1162 0.149 Uiso 1 1 calc R . .
H37C H 0.6064 0.8441 -0.2043 0.149 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'
Na Na 0.0362 0.0249 '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
O2 Na O1 120.97(7) . 2_665 ?
O2 Na O3 112.28(7) . 2_665 ?
O1 Na O3 112.56(8) 2_665 2_665 ?
O2 Na O3 99.95(7) . . ?
O1 Na O3 113.37(7) 2_665 . ?
O3 Na O3 93.58(7) 2_665 . ?
O2 Na C31 78.08(7) . . ?
O1 Na C31 121.53(8) 2_665 . ?
O3 Na C31 106.74(8) 2_665 . ?
O3 Na C31 22.49(6) . . ?
O2 Na Na 113.69(6) . 2_665 ?
O1 Na Na 124.74(6) 2_665 2_665 ?
O3 Na Na 47.29(5) 2_665 2_665 ?
O3 Na Na 46.30(5) . 2_665 ?
C31 Na Na 61.86(6) . 2_665 ?
H1 B N11 107.8(10) . . ?
H1 B N21 108.3(10) . . ?
N11 B N21 111.7(2) . . ?
H1 B N31 110.4(10) . . ?
N11 B N31 110.1(2) . . ?
N21 B N31 108.5(2) . . ?
C11 O1 Na 132.05(17) . 2_665 ?
C21 O2 Na 136.67(17) . . ?
C31 O3 Na 125.81(17) . 2_665 ?
C31 O3 Na 110.66(16) . . ?
Na O3 Na 86.41(7) 2_665 . ?
C11 N11 C12 107.6(2) . . ?
C11 N11 B 122.9(2) . . ?
C12 N11 B 128.5(2) . . ?
C11 N12 C13 108.3(2) . . ?
C11 N12 C14 124.5(2) . . ?
C13 N12 C14 127.1(2) . . ?
C21 N21 C22 107.4(2) . . ?
C21 N21 B 119.6(2) . . ?
C22 N21 B 132.3(2) . . ?
C21 N22 C23 108.1(2) . . ?
C21 N22 C24 124.0(2) . . ?
C23 N22 C24 127.9(2) . . ?
C31 N31 C32 107.9(2) . . ?
C31 N31 B 123.7(2) . . ?
C32 N31 B 128.4(2) . . ?
C31 N32 C33 108.4(2) . . ?
C31 N32 C34 123.8(2) . . ?
C33 N32 C34 125.5(3) . . ?
O1 C11 N11 126.9(2) . . ?
O1 C11 N12 125.9(2) . . ?
N11 C11 N12 107.2(2) . . ?
C13 C12 N11 109.0(2) . . ?
C12 C13 N12 107.8(2) . . ?
N12 C14 C17 109.1(2) . . ?
N12 C14 C15 109.3(2) . . ?
C17 C14 C15 108.9(2) . . ?
N12 C14 C16 109.7(2) . . ?
C17 C14 C16 110.5(2) . . ?
C15 C14 C16 109.3(2) . . ?
O2 C21 N21 126.3(2) . . ?
O2 C21 N22 125.9(2) . . ?
N21 C21 N22 107.9(2) . . ?
C23 C22 N21 108.8(2) . . ?
C22 C23 N22 107.7(2) . . ?
N22 C24 C27 108.1(2) . . ?
N22 C24 C25 109.5(2) . . ?
C27 C24 C25 110.7(2) . . ?
N22 C24 C26 109.4(2) . . ?
C27 C24 C26 109.5(2) . . ?
C25 C24 C26 109.7(2) . . ?
O3 C31 N31 126.1(3) . . ?
O3 C31 N32 125.8(2) . . ?
N31 C31 N32 108.1(2) . . ?
O3 C31 Na 46.85(13) . . ?
N31 C31 Na 98.31(16) . . ?
N32 C31 Na 130.60(17) . . ?
C33 C32 N31 108.5(2) . . ?
C32 C33 N32 106.7(3) . . ?
N32 C34 C37 109.4(2) . . ?
N32 C34 C35 109.0(2) . . ?
C37 C34 C35 110.5(3) . . ?
N32 C34 C36 109.4(2) . . ?
C37 C34 C36 109.7(3) . . ?
C35 C34 C36 108.8(2) . . ?
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
Na O2 2.2518(19) . ?
Na O1 2.291(2) 2_665 ?
Na O3 2.347(2) 2_665 ?
Na O3 2.385(2) . ?
Na C31 3.059(3) . ?
Na Na 3.240(2) 2_665 ?
B H1 1.152(19) . ?
B N11 1.543(3) . ?
B N21 1.548(3) . ?
B N31 1.556(4) . ?
O1 C11 1.250(3) . ?
O1 Na 2.291(2) 2_665 ?
O2 C21 1.256(3) . ?
O3 C31 1.251(3) . ?
O3 Na 2.347(2) 2_665 ?
N11 C11 1.382(3) . ?
N11 C12 1.393(3) . ?
N12 C11 1.385(3) . ?
N12 C13 1.391(3) . ?
N12 C14 1.482(3) . ?
N21 C21 1.377(3) . ?
N21 C22 1.396(3) . ?
N22 C21 1.380(3) . ?
N22 C23 1.395(3) . ?
N22 C24 1.482(3) . ?
N31 C31 1.368(3) . ?
N31 C32 1.403(3) . ?
N32 C31 1.382(3) . ?
N32 C33 1.404(3) . ?
N32 C34 1.493(3) . ?
C12 C13 1.348(3) . ?
C14 C17 1.519(3) . ?
C14 C15 1.529(3) . ?
C14 C16 1.531(3) . ?
C22 C23 1.353(3) . ?
C24 C27 1.519(3) . ?
C24 C25 1.523(3) . ?
C24 C26 1.524(3) . ?
C32 C33 1.375(3) . ?
C34 C37 1.515(4) . ?
C34 C35 1.521(4) . ?
C34 C36 1.530(3) . ?
