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#$Date: 2019-11-25 01:28:53 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239866 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/03/4350384.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_4350384
loop_
_publ_author_name
'Ibrahim, Mohamed M.'
'Olmo, Cristina Pérez'
'Tekeste, Teame'
'Seebacher, Jan'
'He, Guosen'
'Maldonado Calvo, José A'
'Böhmerle, Karin'
'Steinfeld, Gunther'
'Brombacher, Horst'
'Vahrenkamp, Heinrich'
_publ_section_title
;
 Zn-OH2 and Zn-OH complexes with hydroborate-derived tripod ligands: a
 comprehensive study.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7493
_journal_page_last               7502
_journal_paper_doi               10.1021/ic060752f
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C11 H9.33 B0.33 N2 O1.33 S Zn0.33'
_chemical_formula_weight         248.32
_chemical_name_common            'Complex 8 (Seebacher), Tt(Tol)Zn-OH'
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   15.018(4)
_cell_length_b                   15.018(4)
_cell_length_c                   19.752(7)
_cell_measurement_temperature    217(2)
_cell_volume                     3858(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      217(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_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  0.1910
_diffrn_reflns_av_sigmaI/netI    0.1394
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31984
_diffrn_reflns_theta_full        28.88
_diffrn_reflns_theta_max         28.88
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.841
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1532
_refine_diff_density_max         1.049
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.211
_refine_ls_extinction_coef       0.024(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         3249
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.1969
_refine_ls_R_factor_gt           0.0901
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1702P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2434
_refine_ls_wR_factor_ref         0.2998
_reflns_number_gt                1313
_reflns_number_total             3249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060752fsi20060504_033957.cif
_cod_data_source_block           seeby60
_cod_database_code               4350384
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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
Zn1 Zn 0.3333 0.6667 0.10200(6) 0.0455(5) Uani 1 3 d S
O1 O 0.3333 0.6667 0.1985(4) 0.084(3) Uani 1 3 d S
S1 S 0.49000(14) 0.69590(15) 0.05705(8) 0.0477(6) Uani 1 1 d .
B1 B 0.3333 0.6667 -0.0822(6) 0.046(3) Uani 1 3 d S
H1 H 0.3333 0.6667 -0.1323 0.066(10) Uiso 1 3 calc SR
N1 N 0.4365(4) 0.7579(4) -0.0607(2) 0.0430(13) Uani 1 1 d .
N2 N 0.5787(4) 0.8739(4) -0.0123(3) 0.0474(14) Uani 1 1 d .
C1 C 0.4996(5) 0.7765(5) -0.0070(3) 0.0396(15) Uani 1 1 d .
C2 C 0.4794(6) 0.8479(6) -0.0993(3) 0.0502(18) Uani 1 1 d .
H2A H 0.4514 0.8563 -0.1397 0.066(10) Uiso 1 1 calc R
C3 C 0.5644(6) 0.9188(6) -0.0709(3) 0.0519(18) Uani 1 1 d .
H3A H 0.6073 0.9862 -0.0865 0.066(10) Uiso 1 1 calc R
C4 C 0.6574(5) 0.9288(6) 0.0358(3) 0.0498(17) Uani 1 1 d .
C5 C 0.6598(6) 1.0097(6) 0.0690(4) 0.059(2) Uani 1 1 d .
H5A H 0.6080 1.0262 0.0609 0.066(10) Uiso 1 1 calc R
C6 C 0.7370(7) 1.0673(7) 0.1141(4) 0.071(2) Uani 1 1 d .
H6A H 0.7381 1.1231 0.1364 0.066(10) Uiso 1 1 calc R
C7 C 0.8124(7) 1.0438(7) 0.1268(5) 0.077(3) Uani 1 1 d .
C8 C 0.8109(7) 0.9639(7) 0.0916(5) 0.075(3) Uani 1 1 d .
H8A H 0.8638 0.9487 0.0985 0.066(10) Uiso 1 1 calc R
C9 C 0.7341(6) 0.9064(7) 0.0469(5) 0.065(2) Uani 1 1 d .
H9A H 0.7339 0.8515 0.0238 0.066(10) Uiso 1 1 calc R
C10 C 0.9014(6) 1.1067(6) 0.1775(4) 0.117(5) Uani 1 1 d .
H10A H 0.9462 1.0775 0.1796 0.16(3) Uiso 1 1 calc R
H10B H 0.8730 1.1042 0.2221 0.16(3) Uiso 1 1 calc R
H10C H 0.9404 1.1776 0.1625 0.16(3) Uiso 1 1 calc R
O100 O 0.3518(6) 0.8265(6) -0.2476(4) 0.180(4) Uiso 1 1 d R
C100 C 0.2684(6) 0.8340(6) -0.2757(4) 0.333(16) Uiso 1 1 d 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'
S S 0.1246 0.1234 '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
O1 Zn1 S1 112.28(5) . 2_665
O1 Zn1 S1 112.28(5) . 3_565
S1 Zn1 S1 106.52(5) 2_665 3_565
O1 Zn1 S1 112.28(5) . .
S1 Zn1 S1 106.52(5) 2_665 .
S1 Zn1 S1 106.52(5) 3_565 .
C1 S1 Zn1 97.7(2) . .
N1 B1 N1 112.6(4) 2_665 .
N1 B1 N1 112.6(4) 2_665 3_565
N1 B1 N1 112.6(4) . 3_565
C1 N1 C2 107.0(6) . .
C1 N1 B1 133.8(6) . .
C2 N1 B1 119.1(6) . .
C1 N2 C3 108.7(6) . .
C1 N2 C4 127.1(6) . .
C3 N2 C4 123.7(6) . .
N2 C1 N1 107.9(5) . .
N2 C1 S1 122.9(5) . .
N1 C1 S1 129.2(5) . .
C3 C2 N1 110.0(6) . .
C2 C3 N2 106.4(6) . .
C5 C4 C9 119.4(7) . .
C5 C4 N2 118.9(7) . .
C9 C4 N2 121.6(7) . .
C4 C5 C6 120.6(8) . .
C7 C6 C5 120.4(8) . .
C6 C7 C8 118.4(8) . .
C6 C7 C10 122.3(9) . .
C8 C7 C10 119.3(9) . .
C9 C8 C7 121.3(9) . .
C8 C9 C4 119.8(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 1.906(9) .
Zn1 S1 2.3417(19) 2_665
Zn1 S1 2.3417(19) 3_565
Zn1 S1 2.3417(19) .
S1 C1 1.705(6) .
B1 N1 1.528(7) 2_665
B1 N1 1.528(7) .
B1 N1 1.528(7) 3_565
N1 C1 1.356(8) .
N1 C2 1.396(8) .
N2 C1 1.351(8) .
N2 C3 1.408(9) .
N2 C4 1.417(9) .
C2 C3 1.311(10) .
C4 C5 1.366(10) .
C4 C9 1.370(10) .
C5 C6 1.372(11) .
C6 C7 1.366(12) .
C7 C8 1.378(12) .
C7 C10 1.555(11) .
C8 C9 1.363(11) .
O100 C100 1.4239 .
