#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:00:22 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180164 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/60/7106077.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_7106077
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            'C25 H23 B Cl6 N6 O3 Zr'
_chemical_formula_weight         770.22
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.384(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.611(3)
_cell_length_b                   12.966(3)
_cell_length_c                   15.764(4)
_cell_measurement_reflns_used    4760
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      23.68
_cell_measurement_theta_min      2.28
_cell_volume                     3104.2(12)
_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      125(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  0.1740
_diffrn_reflns_av_sigmaI/netI    0.1243
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36423
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.910
_exptl_absorpt_correction_T_max  0.9820
_exptl_absorpt_correction_T_min  0.9390
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.763
_refine_diff_density_min         -1.008
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         6363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1321
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0267P)²+2.2020P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.1052
_reflns_number_gt                3527
_reflns_number_total             6363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC03943H.TXT
_cod_data_source_block           zrtos10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        3104.4(12)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7106077
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr Zr 0.59197(3) 0.83647(4) 0.83260(3) 0.01906(13) Uani 1 1 d . . .
B B 0.4109(4) 0.7522(5) 0.6178(4) 0.0192(13) Uani 1 1 d . . .
H1 H 0.362(3) 0.734(4) 0.556(3) 0.040 Uiso 1 1 d . . .
O1 O 0.5711(2) 0.6940(2) 0.7675(2) 0.0203(8) Uani 1 1 d . . .
O2 O 0.5702(2) 0.8919(3) 0.7035(2) 0.0202(8) Uani 1 1 d . . .
O3 O 0.4548(2) 0.8378(3) 0.8057(2) 0.0205(8) Uani 1 1 d . . .
N11 N 0.4961(2) 0.6890(3) 0.6200(2) 0.0151(9) Uani 1 1 d . . .
N12 N 0.6309(3) 0.6224(3) 0.6590(3) 0.0205(10) Uani 1 1 d . . .
N21 N 0.4308(2) 0.8700(3) 0.6097(2) 0.0156(10) Uani 1 1 d . . .
N22 N 0.4954(3) 1.0236(3) 0.6184(3) 0.0173(10) Uani 1 1 d . . .
N31 N 0.3713(2) 0.7319(3) 0.6975(3) 0.0153(9) Uani 1 1 d . . .
N32 N 0.3392(3) 0.7377(3) 0.8277(3) 0.0217(10) Uani 1 1 d . . .
C11 C 0.5653(3) 0.6703(4) 0.6873(3) 0.0173(11) Uani 1 1 d . . .
C12 C 0.6048(3) 0.6112(4) 0.5694(3) 0.0208(12) Uani 1 1 d . . .
C13 C 0.6481(3) 0.5712(4) 0.5095(3) 0.0235(13) Uani 1 1 d . . .
H13A H 0.7062 0.5447 0.5270 0.028 Uiso 1 1 calc R . .
C14 C 0.6032(4) 0.5715(4) 0.4231(4) 0.0270(13) Uani 1 1 d . . .
H14A H 0.6309 0.5456 0.3798 0.032 Uiso 1 1 calc R . .
C15 C 0.5172(4) 0.6096(4) 0.3987(3) 0.0252(13) Uani 1 1 d . . .
H15A H 0.4877 0.6079 0.3388 0.030 Uiso 1 1 calc R . .
C16 C 0.4733(3) 0.6498(4) 0.4580(3) 0.0219(12) Uani 1 1 d . . .
H16A H 0.4148 0.6753 0.4405 0.026 Uiso 1 1 calc R . .
C17 C 0.5191(3) 0.6508(4) 0.5439(3) 0.0166(11) Uani 1 1 d . . .
C18 C 0.7154(3) 0.5918(4) 0.7142(4) 0.0334(15) Uani 1 1 d . . .
H18A H 0.7160 0.6071 0.7753 0.050 Uiso 1 1 calc R . .
H18B H 0.7628 0.6300 0.6970 0.050 Uiso 1 1 calc R . .
H18C H 0.7242 0.5176 0.7077 0.050 Uiso 1 1 calc R . .
C21 C 0.5030(3) 0.9247(4) 0.6479(3) 0.0155(11) Uani 1 1 d . . .
C22 C 0.4149(3) 1.0329(4) 0.5573(3) 0.0152(11) Uani 1 1 d . . .
C23 C 0.3764(3) 1.1171(4) 0.5078(3) 0.0254(13) Uani 1 1 d . . .
H23A H 0.4053 1.1819 0.5108 0.031 Uiso 1 1 calc R . .
C24 C 0.2943(3) 1.1011(4) 0.4544(3) 0.0279(14) Uani 1 1 d . . .
H24A H 0.2662 1.1560 0.4187 0.033 Uiso 1 1 calc R . .
C25 C 0.2515(4) 1.0067(4) 0.4514(3) 0.0274(13) Uani 1 1 d . . .
H25A H 0.1941 0.9993 0.4149 0.033 Uiso 1 1 calc R . .
C26 C 0.2903(3) 0.9229(4) 0.5002(3) 0.0222(12) Uani 1 1 d . . .
H26A H 0.2610 0.8584 0.4975 0.027 Uiso 1 1 calc R . .
C27 C 0.3742(3) 0.9374(4) 0.5535(3) 0.0162(11) Uani 1 1 d . . .
C28 C 0.5594(3) 1.1041(4) 0.6501(3) 0.0269(13) Uani 1 1 d . . .
H28A H 0.6047 1.0777 0.6990 0.040 Uiso 1 1 calc R . .
H28B H 0.5297 1.1632 0.6695 0.040 Uiso 1 1 calc R . .
H28C H 0.5869 1.1258 0.6031 0.040 Uiso 1 1 calc R . .
C31 C 0.3926(3) 0.7728(4) 0.7781(3) 0.0163(11) Uani 1 1 d . . .
C32 C 0.2779(3) 0.6713(4) 0.7761(3) 0.0229(12) Uani 1 1 d . . .
C33 C 0.2075(3) 0.6192(4) 0.7963(4) 0.0315(14) Uani 1 1 d . . .
H33A H 0.1958 0.6217 0.8527 0.038 Uiso 1 1 calc R . .
C34 C 0.1556(4) 0.5632(4) 0.7286(4) 0.0342(15) Uani 1 1 d . . .
H34A H 0.1061 0.5266 0.7385 0.041 Uiso 1 1 calc R . .
C35 C 0.1740(3) 0.5592(4) 0.6470(4) 0.0303(14) Uani 1 1 d . . .
H35A H 0.1370 0.5193 0.6026 0.036 Uiso 1 1 calc R . .
C36 C 0.2445(3) 0.6112(4) 0.6277(3) 0.0205(12) Uani 1 1 d . . .
H36A H 0.2561 0.6087 0.5711 0.025 Uiso 1 1 calc R . .
C37 C 0.2975(3) 0.6670(4) 0.6947(3) 0.0174(11) Uani 1 1 d . . .
C38 C 0.3440(4) 0.7667(5) 0.9178(3) 0.0363(15) Uani 1 1 d . . .
H38A H 0.3950 0.8116 0.9386 0.054 Uiso 1 1 calc R . .
H38B H 0.3501 0.7045 0.9541 0.054 Uiso 1 1 calc R . .
H38C H 0.2902 0.8034 0.9216 0.054 Uiso 1 1 calc R . .
Cl1 Cl 0.74861(8) 0.82236(11) 0.83925(9) 0.0337(4) Uani 1 1 d . . .
Cl2 Cl 0.59749(9) 1.01066(10) 0.88990(9) 0.0298(3) Uani 1 1 d . . .
Cl3 Cl 0.59612(9) 0.74722(11) 0.96725(8) 0.0304(3) Uani 1 1 d . . .
C40 C 0.5529(4) 0.6035(5) 1.1318(4) 0.0470(18) Uani 1 1 d . . .
H40A H 0.5568 0.6095 1.0695 0.056 Uiso 1 1 calc R . .
Cl41 Cl 0.50779(12) 0.48353(14) 1.14651(16) 0.0783(7) Uani 1 1 d . . .
Cl42 Cl 0.48459(16) 0.70281(15) 1.15406(12) 0.0791(7) Uani 1 1 d . . .
Cl43 Cl 0.65926(13) 0.61214(16) 1.19818(12) 0.0689(6) 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 '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
_geom_angle_publ_flag
O3 Zr O1 82.64(13) . . ?
O3 Zr O2 82.68(12) . . ?
O1 Zr O2 81.74(12) . . ?
O3 Zr Cl3 90.01(10) . . ?
O1 Zr Cl3 88.71(10) . . ?
O2 Zr Cl3 168.62(10) . . ?
O3 Zr Cl2 90.83(10) . . ?
O1 Zr Cl2 171.12(10) . . ?
O2 Zr Cl2 91.49(10) . . ?
Cl3 Zr Cl2 97.35(5) . . ?
O3 Zr Cl1 170.21(10) . . ?
O1 Zr Cl1 89.75(10) . . ?
O2 Zr Cl1 90.16(9) . . ?
Cl3 Zr Cl1 95.99(5) . . ?
Cl2 Zr Cl1 96.04(5) . . ?
H1 B N31 111(3) . . ?
H1 B N11 109(3) . . ?
N31 B N11 113.1(4) . . ?
H1 B N21 104(3) . . ?
N31 B N21 110.7(4) . . ?
N11 B N21 109.3(4) . . ?
C11 O1 Zr 131.2(3) . . ?
C21 O2 Zr 134.4(3) . . ?
C31 O3 Zr 136.4(3) . . ?
C11 N11 C17 106.8(4) . . ?
C11 N11 B 129.6(4) . . ?
C17 N11 B 123.1(4) . . ?
C11 N12 C12 108.4(4) . . ?
C11 N12 C18 125.1(4) . . ?
C12 N12 C18 126.4(4) . . ?
C21 N21 C27 107.0(4) . . ?
C21 N21 B 129.5(4) . . ?
C27 N21 B 123.4(4) . . ?
C21 N22 C22 108.0(4) . . ?
C21 N22 C28 124.3(4) . . ?
C22 N22 C28 127.7(4) . . ?
C31 N31 C37 106.6(4) . . ?
C31 N31 B 130.0(4) . . ?
C37 N31 B 123.4(4) . . ?
C31 N32 C32 107.7(4) . . ?
C31 N32 C38 125.5(4) . . ?
C32 N32 C38 126.8(4) . . ?
O1 C11 N11 126.3(4) . . ?
O1 C11 N12 123.1(4) . . ?
N11 C11 N12 110.6(4) . . ?
C13 C12 N12 131.4(5) . . ?
C13 C12 C17 121.7(5) . . ?
N12 C12 C17 106.9(4) . . ?
C14 C13 C12 117.1(5) . . ?
C13 C14 C15 120.6(5) . . ?
C16 C15 C14 122.8(5) . . ?
C17 C16 C15 116.3(5) . . ?
C16 C17 C12 121.5(5) . . ?
C16 C17 N11 131.3(4) . . ?
C12 C17 N11 107.2(4) . . ?
O2 C21 N21 126.9(4) . . ?
O2 C21 N22 122.8(4) . . ?
N21 C21 N22 110.3(4) . . ?
C27 C22 C23 122.7(5) . . ?
C27 C22 N22 106.4(4) . . ?
C23 C22 N22 130.9(5) . . ?
C24 C23 C22 116.4(5) . . ?
C23 C24 C25 121.7(5) . . ?
C26 C25 C24 121.7(5) . . ?
C25 C26 C27 117.2(5) . . ?
C22 C27 C26 120.2(5) . . ?
C22 C27 N21 108.3(4) . . ?
C26 C27 N21 131.5(5) . . ?
O3 C31 N31 125.5(4) . . ?
O3 C31 N32 123.2(4) . . ?
N31 C31 N32 111.3(4) . . ?
C33 C32 C37 123.3(5) . . ?
C33 C32 N32 129.6(5) . . ?
C37 C32 N32 107.1(4) . . ?
C34 C33 C32 115.6(5) . . ?
C35 C34 C33 121.6(5) . . ?
C36 C35 C34 122.3(5) . . ?
C35 C36 C37 116.9(5) . . ?
C36 C37 C32 120.3(4) . . ?
C36 C37 N31 132.1(4) . . ?
C32 C37 N31 107.4(4) . . ?
Cl41 C40 Cl43 109.5(3) . . ?
Cl41 C40 Cl42 110.2(4) . . ?
Cl43 C40 Cl42 111.7(4) . . ?
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
Zr O3 2.084(3) . ?
Zr O1 2.102(3) . ?
Zr O2 2.110(3) . ?
Zr Cl3 2.4054(15) . ?
Zr Cl2 2.4267(15) . ?
Zr Cl1 2.4301(15) . ?
B H1 1.11(5) . ?
B N31 1.547(7) . ?
B N11 1.555(7) . ?
B N21 1.570(7) . ?
O1 C11 1.283(5) . ?
O2 C21 1.276(5) . ?
O3 C31 1.283(5) . ?
N11 C11 1.349(6) . ?
N11 C17 1.419(6) . ?
N12 C11 1.359(6) . ?
N12 C12 1.384(6) . ?
N12 C18 1.457(6) . ?
N21 C21 1.349(6) . ?
N21 C27 1.403(6) . ?
N22 C21 1.360(6) . ?
N22 C22 1.400(6) . ?
N22 C28 1.451(6) . ?
N31 C31 1.345(6) . ?
N31 C37 1.418(6) . ?
N32 C31 1.346(6) . ?
N32 C32 1.400(6) . ?
N32 C38 1.456(6) . ?
C12 C13 1.384(7) . ?
C12 C17 1.402(6) . ?
C13 C14 1.380(7) . ?
C14 C15 1.398(7) . ?
C15 C16 1.383(7) . ?
C16 C17 1.377(6) . ?
C22 C27 1.387(6) . ?
C22 C23 1.394(7) . ?
C23 C24 1.377(7) . ?
C24 C25 1.391(7) . ?
C25 C26 1.387(7) . ?
C26 C27 1.395(6) . ?
C32 C33 1.388(7) . ?
C32 C37 1.388(7) . ?
C33 C34 1.387(7) . ?
C34 C35 1.384(7) . ?
C35 C36 1.383(7) . ?
C36 C37 1.386(6) . ?
C40 Cl41 1.745(6) . ?
C40 Cl43 1.750(6) . ?
C40 Cl42 1.758(7) . ?
