#------------------------------------------------------------------------------
#$Date: 2016-03-24 17:11:17 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179680 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/02/7000252.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_7000252
loop_
_publ_author_name
'Chisholm, Malcolm H.'
'Gallucci, Judith C.'
'Yaman, Gulsah'
_publ_section_title
;
 Synthesis and coordination chemistry of TpC*MI complexes where M = Mg,
 Ca, Sr, Ba and Zn and TpC* =
 tris[3-(2-methoxy-1,1-dimethyl)pyrazolyl]hydroborate
;
_journal_issue                   2
_journal_name_full               'Dalton Transactions'
_journal_page_first              368
_journal_page_last               374
_journal_paper_doi               10.1039/b812228h
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C27 H49 B1 N6 O4 Si1 Zn1'
_chemical_formula_sum            'C27 H49 B N6 O4 Si Zn'
_chemical_formula_weight         625.99
_chemical_name_common            'Chisholm 1614'
_chemical_name_systematic
;
?
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      146
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2008-05-30T15:08:58-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   16.0519(4)
_cell_length_b                   16.0519(4)
_cell_length_c                   11.0188(2)
_cell_measurement_reflns_used    1255
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.037
_cell_measurement_wavelength     0.71073
_cell_volume                     2458.77(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans''
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.70645E-1
_diffrn_orient_matrix_UB_12      -0.464233E-1
_diffrn_orient_matrix_UB_13      -0.55985E-2
_diffrn_orient_matrix_UB_21      0.2412E-2
_diffrn_orient_matrix_UB_22      0.109816E-1
_diffrn_orient_matrix_UB_23      -0.89578E-1
_diffrn_orient_matrix_UB_31      0.133484E-1
_diffrn_orient_matrix_UB_32      -0.538422E-1
_diffrn_orient_matrix_UB_33      -0.134432E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11122
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.36
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular-shaped wedge'
_exptl_crystal_F_000             1002
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.152
_refine_diff_density_min         -0.21
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.004(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2498
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0201
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0194P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0424
_refine_ls_wR_factor_ref         0.0427
_reflns_number_gt                2456
_reflns_number_total             2498
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b812228h.txt
_cod_data_source_block           Chisholm1614
_cod_original_sg_symbol_H-M      R3
_cod_database_code               7000252
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
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
Zn Zn 0 0 0.048497(5) 0.01322(8) Uani 1 3 d S . .
Si Si 0 0 0.35964(7) 0.01722(18) Uani 1 3 d S . .
O1 O -0.27200(12) -0.00061(12) 0.10689(13) 0.0284(4) Uani 1 1 d . . .
O2 O 0 0 0.21490(17) 0.0203(4) Uani 1 3 d S . .
N1 N -0.05414(19) 0.0503(2) -0.17397(10) 0.0148(3) Uani 1 1 d . . .
N2 N -0.05806(19) 0.06637(19) -0.05226(12) 0.0143(3) Uani 1 1 d . . .
C1 C -0.1068(2) 0.1142(2) -0.04119(14) 0.0157(3) Uani 1 1 d . . .
C2 C -0.1320(3) 0.1302(3) -0.15652(14) 0.0199(3) Uani 1 1 d . . .
H2 H -0.1659 0.163 -0.1756 0.024 Uiso 1 1 calc R . .
C3 C -0.0980(2) 0.0888(2) -0.23672(14) 0.0183(4) Uani 1 1 d . . .
H3 H -0.1044 0.0877 -0.3225 0.022 Uiso 1 1 calc R . .
C4 C -0.12199(18) 0.14749(18) 0.08172(17) 0.0198(6) Uani 1 1 d . . .
C5 C -0.17388(19) 0.20532(18) 0.0644(2) 0.0296(7) Uani 1 1 d . . .
H5A H -0.1352 0.2608 0.0118 0.044 Uiso 1 1 calc R . .
H5B H -0.1827 0.2278 0.1434 0.044 Uiso 1 1 calc R . .
H5C H -0.2368 0.1642 0.0268 0.044 Uiso 1 1 calc R . .
C6 C -0.02423(19) 0.2118(2) 0.1416(3) 0.0269(6) Uani 1 1 d . . .
H6A H 0.0147 0.2675 0.0894 0.04 Uiso 1 1 calc R . .
H6B H 0.009 0.1752 0.1533 0.04 Uiso 1 1 calc R . .
H6C H -0.0338 0.2341 0.2204 0.04 Uiso 1 1 calc R . .
C7 C -0.18211(18) 0.06168(19) 0.1633(2) 0.0217(6) Uani 1 1 d . . .
H7A H -0.1473 0.0263 0.1788 0.026 Uiso 1 1 calc R . .
H7B H -0.1931 0.0842 0.2422 0.026 Uiso 1 1 calc R . .
C8 C -0.33467(17) -0.07542(17) 0.1861(2) 0.0318(5) Uani 1 1 d . . .
H8A H -0.3059 -0.1147 0.2079 0.048 Uiso 1 1 calc R . .
H8B H -0.3964 -0.1158 0.1454 0.048 Uiso 1 1 calc R . .
H8C H -0.345 -0.0475 0.2597 0.048 Uiso 1 1 calc R . .
C9 C -0.12169(16) -0.08763(17) 0.4226(2) 0.0299(6) Uani 1 1 d . . .
H9A H -0.1712 -0.0811 0.3788 0.045 Uiso 1 1 calc R . .
H9B H -0.124 -0.0742 0.5089 0.045 Uiso 1 1 calc R . .
H9C H -0.1333 -0.1533 0.4131 0.045 Uiso 1 1 calc R . .
B B 0 0 -0.2214(3) 0.0149(7) Uani 1 3 d S . .
H0 H 0 0 -0.3122 0.018 Uiso 1 3 calc SR . .
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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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 Zn N2 122.68(4) . . ?
N2 Zn N2 93.60(5) 2 . ?
O2 Si C9 111.69(7) . . ?
C9 Si C9 107.17(8) 3 . ?
C8 O1 C7 111.54(17) . . ?
Si O2 Zn 180 . . ?
C3 N1 N2 109.53(12) . . ?
C3 N1 B 129.07(14) . . ?
N2 N1 B 121.30(14) . . ?
C1 N2 N1 106.82(13) . . ?
C1 N2 Zn 142.05(11) . . ?
N1 N2 Zn 110.79(9) . . ?
N2 C1 C2 109.12(14) . . ?
N2 C1 C4 121.49(15) . . ?
C2 C1 C4 129.28(14) . . ?
C3 C2 C1 105.88(13) . . ?
C3 C2 H2 127.1 . . ?
C1 C2 H2 127.1 . . ?
N1 C3 C2 108.64(13) . . ?
N1 C3 H3 125.7 . . ?
C2 C3 H3 125.7 . . ?
C7 C4 C1 110.4(2) . . ?
C7 C4 C6 109.2(2) . . ?
C1 C4 C6 109.3(2) . . ?
C7 C4 C5 109.31(19) . . ?
C1 C4 C5 109.43(16) . . ?
C6 C4 C5 109.1(2) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O1 C7 C4 109.86(19) . . ?
O1 C7 H7A 109.7 . . ?
C4 C7 H7A 109.7 . . ?
O1 C7 H7B 109.7 . . ?
C4 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
O1 C8 H8A 109.5 . . ?
O1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si C9 H9A 109.5 . . ?
Si C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 B N1 109.15(11) 3 . ?
N1 B N1 109.15(11) 3 2 ?
N1 B N1 109.15(11) . 2 ?
N1 B H0 109.8 3 . ?
N1 B H0 109.8 . . ?
N1 B H0 109.8 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
Zn O2 1.8336(19) . ?
Zn N2 2.0565(12) . ?
Si O2 1.595(2) . ?
Si C9 1.878(2) . ?
O1 C8 1.417(3) . ?
O1 C7 1.423(3) . ?
N1 C3 1.337(2) . ?
N1 N2 1.3730(17) . ?
N1 B 1.5437(16) . ?
N2 C1 1.3470(19) . ?
C1 C2 1.397(2) . ?
C1 C4 1.520(2) . ?
C2 C3 1.373(2) . ?
C2 H2 0.95 . ?
C3 H3 0.95 . ?
C4 C7 1.519(4) . ?
C4 C6 1.531(4) . ?
C4 C5 1.538(3) . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C7 H7A 0.99 . ?
C7 H7B 0.99 . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C9 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
B N1 1.5437(16) 3 ?
B N1 1.5437(16) 2 ?
B H0 1 . ?
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_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N1 N2 C1 1.0(4) . . . . ?
B N1 N2 C1 177.7(3) . . . . ?
C3 N1 N2 Zn 176.0(2) . . . . ?
B N1 N2 Zn -7.4(3) . . . . ?
O2 Zn N2 C1 -4.1(5) . . . . ?
N2 Zn N2 C1 129.0(5) 2 . . . ?
N2 Zn N2 C1 -137.2(5) 3 . . . ?
O2 Zn N2 N1 -176.13(17) . . . . ?
N2 Zn N2 N1 -43.05(17) 2 . . . ?
N2 Zn N2 N1 50.79(17) 3 . . . ?
N1 N2 C1 C2 -1.2(4) . . . . ?
Zn N2 C1 C2 -173.5(3) . . . . ?
N1 N2 C1 C4 -177.7(3) . . . . ?
Zn N2 C1 C4 10.0(6) . . . . ?
N2 C1 C2 C3 1.0(4) . . . . ?
C4 C1 C2 C3 177.1(3) . . . . ?
N2 N1 C3 C2 -0.4(4) . . . . ?
B N1 C3 C2 -176.8(3) . . . . ?
C1 C2 C3 N1 -0.3(4) . . . . ?
N2 C1 C4 C7 -63.3(4) . . . . ?
C2 C1 C4 C7 121.0(4) . . . . ?
N2 C1 C4 C6 56.8(4) . . . . ?
C2 C1 C4 C6 -118.9(4) . . . . ?
N2 C1 C4 C5 176.3(3) . . . . ?
C2 C1 C4 C5 0.6(5) . . . . ?
C8 O1 C7 C4 -172.94(18) . . . . ?
C1 C4 C7 O1 -57.8(2) . . . . ?
C6 C4 C7 O1 -178.0(2) . . . . ?
C5 C4 C7 O1 62.7(2) . . . . ?
C3 N1 B N1 121.4(4) . . . 3 ?
N2 N1 B N1 -54.6(3) . . . 3 ?
C3 N1 B N1 -119.4(4) . . . 2 ?
N2 N1 B N1 64.7(3) . . . 2 ?
