#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:00:22 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180164 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/60/7106075.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_7106075
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 H52 B N6 O6 Re'
_chemical_formula_weight         933.91
_chemical_name_systematic
;
?
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   16.131(2)
_cell_length_b                   16.131(2)
_cell_length_c                   9.6857(14)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.77
_cell_measurement_theta_min      2.53
_cell_volume                     2182.7(5)
_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      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0818
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            34854
_diffrn_reflns_theta_full        30.71
_diffrn_reflns_theta_max         30.71
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    2.835
_exptl_absorpt_correction_T_max  0.9722
_exptl_absorpt_correction_T_min  0.8712
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         4.813
_refine_diff_density_min         -6.921
_refine_diff_density_rms         0.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         4523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0363
_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)+(0.0147P)²+2.0982P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0714
_reflns_number_gt                3279
_reflns_number_total             4523
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC03943H.TXT
_cod_data_source_block           ttores10
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_exptl_absorpt_correction_type' value 'EMPIRICAL'
changed to 'empirical' 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        2182.6(6)
_cod_original_sg_symbol_H-M      P-3
_cod_database_code               7106075
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -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
Re Re 0.6667 0.3333 0.38047(3) 0.03708(8) Uani 1 3 d S . .
B B 0.6667 0.3333 -0.0297(7) 0.0334(15) Uani 1 3 d S . .
H1 H 0.6667 0.3333 -0.126(8) 0.049(17) Uiso 1 3 d S . .
N11 N 0.5712(2) 0.3255(2) 0.0184(3) 0.0322(7) Uani 1 1 d . . .
N12 N 0.4627(2) 0.3456(2) 0.1294(4) 0.0375(7) Uani 1 1 d . . .
O1 O 0.7302(3) 0.5029(3) 0.5762(3) 0.0647(10) Uani 1 1 d . . .
O11 O 0.61054(19) 0.39638(19) 0.2381(3) 0.0367(6) Uani 1 1 d . . .
C1 C 0.7071(3) 0.4387(3) 0.5000(4) 0.0481(11) Uani 1 1 d . . .
C11 C 0.5534(3) 0.3578(2) 0.1375(4) 0.0328(8) Uani 1 1 d . . .
C12 C 0.4906(3) 0.2912(3) -0.0647(4) 0.0363(9) Uani 1 1 d . . .
H12A H 0.4833 0.2636 -0.1537 0.044 Uiso 1 1 calc R . .
C13 C 0.4249(3) 0.3036(3) 0.0018(4) 0.0410(9) Uani 1 1 d . . .
H13A H 0.3632 0.2868 -0.0321 0.049 Uiso 1 1 calc R . .
C14 C 0.4204(3) 0.3857(3) 0.2272(4) 0.0455(10) Uani 1 1 d . . .
C15 C 0.4700(5) 0.4912(4) 0.2095(7) 0.105(3) Uani 1 1 d . . .
H15A H 0.4580 0.5065 0.1163 0.157 Uiso 1 1 calc R . .
H15B H 0.5389 0.5180 0.2228 0.157 Uiso 1 1 calc R . .
H15C H 0.4457 0.5187 0.2777 0.157 Uiso 1 1 calc R . .
C16 C 0.3137(4) 0.3407(5) 0.1978(7) 0.0867(19) Uani 1 1 d . . .
H16A H 0.3045 0.3613 0.1067 0.130 Uiso 1 1 calc R . .
H16B H 0.2841 0.3611 0.2684 0.130 Uiso 1 1 calc R . .
H16C H 0.2839 0.2708 0.1994 0.130 Uiso 1 1 calc R . .
C17 C 0.4301(5) 0.3600(5) 0.3743(6) 0.0885(19) Uani 1 1 d . . .
H17A H 0.4981 0.3892 0.3980 0.133 Uiso 1 1 calc R . .
H17B H 0.3993 0.2903 0.3832 0.133 Uiso 1 1 calc R . .
H17C H 0.3992 0.3841 0.4371 0.133 Uiso 1 1 calc R . .
C100 C 0.7481(7) 0.7024(7) 0.3361(9) 0.139(4) Uani 1 1 d . . .
H10F H 0.7096 0.6490 0.3936 0.167 Uiso 1 1 calc R . .
C101 C 0.7745(8) 0.7943(7) 0.3806(11) 0.160(4) Uani 1 1 d . . .
H10D H 0.7533 0.8033 0.4679 0.192 Uiso 1 1 calc R . .
C102 C 0.8308(6) 0.8720(6) 0.2994(9) 0.108(2) Uani 1 1 d . . .
H10E H 0.8488 0.9351 0.3282 0.130 Uiso 1 1 calc R . .
C103 C 0.8600(5) 0.8552(6) 0.1756(8) 0.097(2) Uani 1 1 d . . .
H10C H 0.9002 0.9076 0.1175 0.116 Uiso 1 1 calc R . .
C104 C 0.8325(4) 0.7646(6) 0.1341(8) 0.0898(19) Uani 1 1 d . . .
H10A H 0.8534 0.7548 0.0471 0.108 Uiso 1 1 calc R . .
C105 C 0.7764(5) 0.6888(5) 0.2131(7) 0.0886(19) Uani 1 1 d . . .
H10B H 0.7570 0.6258 0.1818 0.106 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'
Re Re -1.0185 7.2310 '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
C1 Re C1 86.1(2) 3_665 2_655 ?
C1 Re C1 86.1(2) 3_665 . ?
C1 Re C1 86.1(2) 2_655 . ?
C1 Re O11 172.38(16) 3_665 . ?
C1 Re O11 100.36(15) 2_655 . ?
C1 Re O11 90.31(15) . . ?
C1 Re O11 100.36(15) 3_665 2_655 ?
C1 Re O11 90.31(15) 2_655 2_655 ?
C1 Re O11 172.38(16) . 2_655 ?
O11 Re O11 83.69(10) . 2_655 ?
C1 Re O11 90.31(15) 3_665 3_665 ?
C1 Re O11 172.38(16) 2_655 3_665 ?
C1 Re O11 100.36(15) . 3_665 ?
O11 Re O11 83.69(10) . 3_665 ?
O11 Re O11 83.69(10) 2_655 3_665 ?
H1 B N11 107.5(3) . 2_655 ?
H1 B N11 107.5(3) . 3_665 ?
N11 B N11 111.4(2) 2_655 3_665 ?
H1 B N11 107.5(3) . . ?
N11 B N11 111.4(2) 2_655 . ?
N11 B N11 111.4(2) 3_665 . ?
H1 B H1 0.000(6) . . ?
N11 B H1 107.5(3) 2_655 . ?
N11 B H1 107.5(3) 3_665 . ?
N11 B H1 107.5(3) . . ?
C11 N11 C12 108.2(3) . . ?
C11 N11 B 128.1(3) . . ?
C12 N11 B 123.5(3) . . ?
C11 N12 C13 107.1(3) . . ?
C11 N12 C14 125.9(3) . . ?
C13 N12 C14 126.2(3) . . ?
C11 O11 Re 129.1(2) . . ?
O1 C1 Re 178.3(4) . . ?
O11 C11 N11 126.9(3) . . ?
O11 C11 N12 124.9(3) . . ?
N11 C11 N12 108.1(3) . . ?
C13 C12 N11 108.4(3) . . ?
C13 C12 H12A 125.8 . . ?
N11 C12 H12A 125.8 . . ?
C12 C13 N12 108.2(3) . . ?
C12 C13 H13A 125.9 . . ?
N12 C13 H13A 125.9 . . ?
C15 C14 N12 108.8(4) . . ?
C15 C14 C17 110.6(5) . . ?
N12 C14 C17 110.3(4) . . ?
C15 C14 C16 110.9(5) . . ?
N12 C14 C16 109.1(4) . . ?
C17 C14 C16 107.0(4) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C105 C100 C101 120.3(8) . . ?
C105 C100 H10F 119.8 . . ?
C101 C100 H10F 119.8 . . ?
C102 C101 C100 120.5(8) . . ?
C102 C101 H10D 119.7 . . ?
C100 C101 H10D 119.7 . . ?
C103 C102 C101 117.4(8) . . ?
C103 C102 H10E 121.3 . . ?
C101 C102 H10E 121.3 . . ?
C104 C103 C102 120.9(7) . . ?
C104 C103 H10C 119.5 . . ?
C102 C103 H10C 119.5 . . ?
C105 C104 C103 121.4(7) . . ?
C105 C104 H10A 119.3 . . ?
C103 C104 H10A 119.3 . . ?
C100 C105 C104 119.4(8) . . ?
C100 C105 H10B 120.3 . . ?
C104 C105 H10B 120.3 . . ?
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
Re C1 1.883(5) 3_665 ?
Re C1 1.883(5) 2_655 ?
Re C1 1.883(5) . ?
Re O11 2.162(3) . ?
Re O11 2.162(3) 2_655 ?
Re O11 2.162(3) 3_665 ?
B H1 0.94(8) . ?
B N11 1.553(4) 2_655 ?
B N11 1.553(4) 3_665 ?
B N11 1.553(4) . ?
B H1 0.94(8) . ?
N11 C11 1.354(5) . ?
N11 C12 1.388(5) . ?
N12 C11 1.378(5) . ?
N12 C13 1.395(5) . ?
N12 C14 1.490(5) . ?
O1 C1 1.171(5) . ?
O11 C11 1.270(4) . ?
C12 C13 1.338(6) . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9500 . ?
C14 C15 1.485(7) . ?
C14 C17 1.514(7) . ?
C14 C16 1.523(7) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C100 C105 1.332(10) . ?
C100 C101 1.391(11) . ?
C100 H10F 0.9500 . ?
C101 C102 1.369(11) . ?
C101 H10D 0.9500 . ?
C102 C103 1.365(10) . ?
C102 H10E 0.9500 . ?
C103 C104 1.358(9) . ?
C103 H10C 0.9500 . ?
C104 C105 1.340(9) . ?
C104 H10A 0.9500 . ?
C105 H10B 0.9500 . ?
