#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:16:34 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180131 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/29/7102915.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_7102915
loop_
_publ_author_name
'Pang, Keliang'
'Tanski, Joseph M'
'Parkin, Gerard'
_publ_section_title
;
 Reactivity of the Ni-->B dative sigma-bond in the nickel boratrane
 compounds [kappa4-B(mimBut)3]NiX (X=Cl, OAc, NCS, N3): synthesis of a
 series of B-functionalized
 tris(2-mercapto-1-tert-butylimidazolyl)borato complexes, [YTmBut)]NiZ.
;
_journal_issue                   8
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1008
_journal_page_last               1010
_journal_paper_doi               10.1039/b714466k
_journal_year                    2008
_chemical_formula_sum            'C25 H39 B N11 Ni S3'
_chemical_formula_weight         659.37
_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                 108.294(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0807(17)
_cell_length_b                   15.395(2)
_cell_length_c                   16.195(2)
_cell_measurement_reflns_used    4218
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      23.33
_cell_measurement_theta_min      2.31
_cell_volume                     3333.3(7)
_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      243(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0760
_diffrn_reflns_av_sigmaI/netI    0.0995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19962
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.804
_exptl_absorpt_correction_T_max  0.9533
_exptl_absorpt_correction_T_min  0.9239
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.068
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.0010(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   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         6814
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1228
_refine_ls_R_factor_gt           0.0561
_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)+(0.0750P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1559
_reflns_number_gt                3848
_reflns_number_total             6814
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b714466k.txt
_cod_data_source_block           tmnins10
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' 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      P2(1)/n
_cod_database_code               7102915
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
Ni Ni 0.78745(4) 0.59513(3) 0.18308(3) 0.03290(18) Uani 1 1 d . . .
S1 S 0.88683(8) 0.52522(7) 0.12047(8) 0.0403(3) Uani 1 1 d . . .
S2 S 0.62323(8) 0.62015(7) 0.15879(8) 0.0403(3) Uani 1 1 d . . .
S3 S 0.87404(9) 0.63720(7) 0.32084(8) 0.0451(3) Uani 1 1 d . . .
N1 N 0.8106(3) 0.7149(2) 0.1334(3) 0.0519(12) Uani 1 1 d . . .
N2 N 0.7818(4) 0.7280(3) 0.0625(5) 0.0756(16) Uani 1 1 d . . .
N3 N 0.7524(7) 0.7471(4) -0.0151(4) 0.145(3) Uani 1 1 d . . .
N11 N 0.8282(2) 0.4057(2) 0.2134(2) 0.0290(7) Uani 1 1 d . . .
N12 N 0.9281(2) 0.3473(2) 0.1488(2) 0.0320(8) Uani 1 1 d . . .
N21 N 0.6508(2) 0.4523(2) 0.1939(2) 0.0297(8) Uani 1 1 d . . .
N22 N 0.4902(2) 0.4825(2) 0.1474(2) 0.0340(8) Uani 1 1 d . . .
N31 N 0.7850(2) 0.4883(2) 0.3328(2) 0.0312(8) Uani 1 1 d . . .
N32 N 0.8413(3) 0.5491(2) 0.4609(2) 0.0374(9) Uani 1 1 d . . .
B B 0.7621(3) 0.4758(3) 0.2343(3) 0.0295(11) Uani 1 1 d . . .
C11 C 0.8829(3) 0.4220(3) 0.1603(3) 0.0308(10) Uani 1 1 d . . .
C12 C 0.8393(3) 0.3193(3) 0.2359(3) 0.0309(9) Uani 1 1 d . . .
H12A H 0.8098 0.2904 0.2728 0.037 Uiso 1 1 calc R . .
C13 C 0.8994(3) 0.2840(3) 0.1960(3) 0.0360(10) Uani 1 1 d . . .
H13A H 0.9191 0.2254 0.1996 0.043 Uiso 1 1 calc R . .
C14 C 0.9944(3) 0.3345(3) 0.0930(3) 0.0424(11) Uani 1 1 d . . .
C15 C 1.0305(4) 0.2411(3) 0.1016(4) 0.0673(16) Uani 1 1 d . . .
H15A H 0.9735 0.2024 0.0812 0.101 Uiso 1 1 calc R . .
H15B H 1.0661 0.2286 0.1621 0.101 Uiso 1 1 calc R . .
H15C H 1.0748 0.2325 0.0671 0.101 Uiso 1 1 calc R . .
C16 C 1.0844(3) 0.3947(4) 0.1245(4) 0.0627(15) Uani 1 1 d . . .
H16A H 1.1214 0.3811 0.1844 0.094 Uiso 1 1 calc R . .
H16B H 1.0617 0.4545 0.1205 0.094 Uiso 1 1 calc R . .
H16C H 1.1273 0.3868 0.0885 0.094 Uiso 1 1 calc R . .
C17 C 0.9349(4) 0.3534(4) -0.0012(3) 0.0588(14) Uani 1 1 d . . .
H17A H 0.8752 0.3175 -0.0183 0.088 Uiso 1 1 calc R . .
H17B H 0.9756 0.3405 -0.0381 0.088 Uiso 1 1 calc R . .
H17C H 0.9158 0.4142 -0.0072 0.088 Uiso 1 1 calc R . .
C21 C 0.5836(3) 0.5166(3) 0.1679(3) 0.0310(9) Uani 1 1 d . . .
C22 C 0.5986(3) 0.3755(3) 0.1887(3) 0.0419(11) Uani 1 1 d . . .
H22A H 0.6270 0.3200 0.2029 0.050 Uiso 1 1 calc R . .
C23 C 0.5011(3) 0.3934(3) 0.1601(3) 0.0455(12) Uani 1 1 d . . .
H23A H 0.4489 0.3528 0.1502 0.055 Uiso 1 1 calc R . .
C24 C 0.3935(3) 0.5314(3) 0.1149(3) 0.0383(10) Uani 1 1 d . . .
C25 C 0.3084(3) 0.4687(3) 0.1122(4) 0.0618(15) Uani 1 1 d . . .
H25A H 0.3190 0.4444 0.1696 0.093 Uiso 1 1 calc R . .
H25B H 0.3068 0.4223 0.0713 0.093 Uiso 1 1 calc R . .
H25C H 0.2452 0.4998 0.0940 0.093 Uiso 1 1 calc R . .
C26 C 0.3826(3) 0.5641(3) 0.0242(3) 0.0504(13) Uani 1 1 d . . .
H26A H 0.4387 0.6015 0.0261 0.076 Uiso 1 1 calc R . .
H26B H 0.3208 0.5967 0.0024 0.076 Uiso 1 1 calc R . .
H26C H 0.3812 0.5152 -0.0138 0.076 Uiso 1 1 calc R . .
C27 C 0.3936(4) 0.6053(3) 0.1774(3) 0.0531(13) Uani 1 1 d . . .
H27A H 0.4457 0.6465 0.1776 0.080 Uiso 1 1 calc R . .
H27B H 0.4058 0.5821 0.2355 0.080 Uiso 1 1 calc R . .
H27C H 0.3292 0.6343 0.1589 0.080 Uiso 1 1 calc R . .
C31 C 0.8345(3) 0.5577(3) 0.3757(3) 0.0331(10) Uani 1 1 d . . .
C32 C 0.7589(3) 0.4357(3) 0.3917(3) 0.0411(11) Uani 1 1 d . . .
H32A H 0.7233 0.3831 0.3788 0.049 Uiso 1 1 calc R . .
C33 C 0.7937(4) 0.4730(3) 0.4701(3) 0.0480(12) Uani 1 1 d . . .
H33A H 0.7869 0.4512 0.5222 0.058 Uiso 1 1 calc R . .
C34 C 0.8797(4) 0.6168(3) 0.5311(3) 0.0483(12) Uani 1 1 d . . .
C35 C 0.8913(5) 0.5743(4) 0.6195(3) 0.0812(19) Uani 1 1 d . . .
H35A H 0.8266 0.5539 0.6209 0.122 Uiso 1 1 calc R . .
H35B H 0.9174 0.6166 0.6655 0.122 Uiso 1 1 calc R . .
H35C H 0.9372 0.5257 0.6281 0.122 Uiso 1 1 calc R . .
C36 C 0.8020(5) 0.6876(4) 0.5135(4) 0.083(2) Uani 1 1 d . . .
H36A H 0.7972 0.7157 0.4587 0.125 Uiso 1 1 calc R . .
H36B H 0.8210 0.7300 0.5601 0.125 Uiso 1 1 calc R . .
H36C H 0.7377 0.6626 0.5104 0.125 Uiso 1 1 calc R . .
C37 C 0.9808(4) 0.6495(4) 0.5309(4) 0.0751(18) Uani 1 1 d . . .
H37A H 0.9732 0.6825 0.4781 0.113 Uiso 1 1 calc R . .
H37B H 1.0250 0.6006 0.5332 0.113 Uiso 1 1 calc R . .
H37C H 1.0092 0.6865 0.5811 0.113 Uiso 1 1 calc R . .
N1S N 0.8012(6) 0.2265(5) -0.2107(5) 0.138(3) Uani 1 1 d . . .
C11S C 0.8293(6) 0.2802(6) -0.2422(5) 0.089(2) Uani 1 1 d . . .
C12S C 0.8606(7) 0.3514(6) -0.2849(5) 0.138(3) Uani 1 1 d . . .
H12B H 0.8095 0.3630 -0.3400 0.207 Uiso 1 1 calc R . .
H12C H 0.9228 0.3365 -0.2953 0.207 Uiso 1 1 calc R . .
H12D H 0.8704 0.4026 -0.2484 0.207 Uiso 1 1 calc R . .
N2S N 0.3647(7) 0.5110(7) 0.3947(6) 0.155(3) Uani 1 1 d . . .
C21S C 0.4286(7) 0.4626(8) 0.3947(5) 0.116(3) Uani 1 1 d . . .
C22S C 0.5057(6) 0.4026(7) 0.3937(5) 0.148(4) Uani 1 1 d . . .
H22B H 0.4759 0.3475 0.3701 0.222 Uiso 1 1 calc R . .
H22C H 0.5500 0.3940 0.4525 0.222 Uiso 1 1 calc R . .
H22D H 0.5435 0.4256 0.3578 0.222 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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
N1 Ni B 178.79(19) . . ?
N1 Ni S1 93.13(14) . . ?
B Ni S1 88.08(13) . . ?
N1 Ni S2 93.30(13) . . ?
B Ni S2 85.75(13) . . ?
S1 Ni S2 138.96(5) . . ?
N1 Ni S3 91.52(12) . . ?
B Ni S3 88.08(13) . . ?
S1 Ni S3 111.19(5) . . ?
S2 Ni S3 109.10(5) . . ?
C11 S1 Ni 100.08(14) . . ?
C21 S2 Ni 99.78(14) . . ?
C31 S3 Ni 98.33(15) . . ?
N2 N1 Ni 120.8(4) . . ?
N1 N2 N3 176.3(7) . . ?
C11 N11 C12 108.0(3) . . ?
C11 N11 B 121.3(3) . . ?
C12 N11 B 130.5(3) . . ?
C11 N12 C13 107.0(3) . . ?
C11 N12 C14 127.0(3) . . ?
C13 N12 C14 126.0(3) . . ?
C21 N21 C22 107.7(3) . . ?
C21 N21 B 118.9(3) . . ?
C22 N21 B 132.6(3) . . ?
C21 N22 C23 106.9(3) . . ?
C21 N22 C24 126.6(3) . . ?
C23 N22 C24 126.5(3) . . ?
C31 N31 C32 108.4(3) . . ?
C31 N31 B 122.8(3) . . ?
C32 N31 B 128.8(3) . . ?
C31 N32 C33 108.1(4) . . ?
C31 N32 C34 126.3(4) . . ?
C33 N32 C34 125.0(4) . . ?
N11 B N31 112.0(3) . . ?
N11 B N21 110.4(3) . . ?
N31 B N21 108.9(3) . . ?
N11 B Ni 109.9(3) . . ?
N31 B Ni 107.2(3) . . ?
N21 B Ni 108.4(3) . . ?
N11 C11 N12 108.5(3) . . ?
N11 C11 S1 120.2(3) . . ?
N12 C11 S1 131.2(3) . . ?
C13 C12 N11 107.6(3) . . ?
C12 C13 N12 108.8(4) . . ?
N12 C14 C15 108.8(4) . . ?
N12 C14 C17 109.1(3) . . ?
C15 C14 C17 109.7(4) . . ?
N12 C14 C16 109.2(4) . . ?
C15 C14 C16 109.1(4) . . ?
C17 C14 C16 111.0(4) . . ?
N21 C21 N22 109.0(3) . . ?
N21 C21 S2 119.8(3) . . ?
N22 C21 S2 131.0(3) . . ?
C23 C22 N21 108.2(4) . . ?
C22 C23 N22 108.1(4) . . ?
N22 C24 C26 108.2(3) . . ?
N22 C24 C27 109.3(3) . . ?
C26 C24 C27 112.0(4) . . ?
N22 C24 C25 108.2(4) . . ?
C26 C24 C25 110.1(4) . . ?
C27 C24 C25 109.0(4) . . ?
N31 C31 N32 107.9(4) . . ?
N31 C31 S3 120.2(3) . . ?
N32 C31 S3 132.0(3) . . ?
C33 C32 N31 107.7(4) . . ?
C32 C33 N32 107.9(4) . . ?
C36 C34 C37 112.8(5) . . ?
C36 C34 N32 106.8(4) . . ?
C37 C34 N32 110.0(4) . . ?
C36 C34 C35 110.1(5) . . ?
C37 C34 C35 108.7(4) . . ?
N32 C34 C35 108.5(4) . . ?
N1S C11S C12S 177.0(10) . . ?
N2S C21S C22S 179.1(12) . . ?
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
Ni N1 2.078(4) . ?
Ni B 2.092(5) . ?
Ni S1 2.2440(13) . ?
Ni S2 2.2536(13) . ?
Ni S3 2.2750(13) . ?
S1 C11 1.723(4) . ?
S2 C21 1.711(4) . ?
S3 C31 1.705(4) . ?
N1 N2 1.109(6) . ?
N2 N3 1.229(8) . ?
N11 C11 1.344(5) . ?
N11 C12 1.375(5) . ?
N11 B 1.532(6) . ?
N12 C11 1.355(5) . ?
N12 C13 1.376(5) . ?
N12 C14 1.502(5) . ?
N21 C21 1.341(5) . ?
N21 C22 1.381(5) . ?
N21 B 1.541(5) . ?
N22 C21 1.358(5) . ?
N22 C23 1.389(5) . ?
N22 C24 1.498(5) . ?
N31 C31 1.345(5) . ?
N31 C32 1.385(5) . ?
N31 B 1.537(6) . ?
N32 C31 1.358(5) . ?
N32 C33 1.382(6) . ?
N32 C34 1.512(5) . ?
C12 C13 1.331(5) . ?
C14 C15 1.516(6) . ?
C14 C17 1.521(6) . ?
C14 C16 1.522(6) . ?
C22 C23 1.333(6) . ?
C24 C26 1.513(6) . ?
C24 C27 1.523(6) . ?
C24 C25 1.529(6) . ?
C32 C33 1.339(6) . ?
C34 C36 1.507(7) . ?
C34 C37 1.512(7) . ?
C34 C35 1.535(7) . ?
N1S C11S 1.107(9) . ?
C11S C12S 1.437(10) . ?
N2S C21S 1.168(11) . ?
C21S C22S 1.429(12) . ?
