#------------------------------------------------------------------------------
#$Date: 2019-11-25 01:28:53 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239866 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/03/4350381.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_4350381
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            'C27.5 H5 B Cl2 D40 N9 O8 Zn'
_chemical_formula_weight         817.04
_chemical_name_common
'Complex 3 (Böhmerle), Tp(CONHtBu,Me)Zn-OH2'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                116.857(2)
_cell_angle_beta                 103.009(2)
_cell_angle_gamma                94.370(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9562(15)
_cell_length_b                   13.4373(17)
_cell_length_c                   13.6557(17)
_cell_measurement_temperature    203(2)
_cell_volume                     1866.7(4)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      203(2)
_diffrn_measured_fraction_theta_full 0.884
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '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  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17076
_diffrn_reflns_theta_full        28.97
_diffrn_reflns_theta_max         28.97
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.857
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             812
_refine_diff_density_max         2.018
_refine_diff_density_min         -1.583
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         8762
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0622
_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)+(0.0825P)²+1.7731P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1567
_refine_ls_wR_factor_ref         0.1798
_reflns_number_gt                5576
_reflns_number_total             8762
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060752fsi20060504_033957.cif
_cod_data_source_block           mgmd
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C27.50 H5 B Cl2 D40 N9 O8 Zn'
_cod_database_code               4350381
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Zn1 Zn 0.57682(4) 0.69997(4) 0.58415(4) 0.03689(16) Uani 1 1 d .
B1 B 0.6518(3) 0.9911(3) 0.7201(3) 0.0249(8) Uani 1 1 d .
H1 H 0.702(3) 1.073(3) 0.758(3) 0.014(8) Uiso 1 1 d .
O1 O 0.6089(2) 0.5942(2) 0.4197(2) 0.0359(6) Uani 1 1 d .
O2 O 0.6693(2) 0.5994(2) 0.6620(2) 0.0355(6) Uani 1 1 d .
O3 O 0.2429(2) 0.7143(2) 0.5871(3) 0.0410(7) Uani 1 1 d .
O4 O 0.4199(3) 0.6202(2) 0.5466(3) 0.0409(7) Uani 1 1 d .
H4B D 0.4009 0.5403 0.5113 0.049 Uiso 1 1 calc R
H4A H 0.374(5) 0.656(4) 0.562(4) 0.053(16) Uiso 1 1 d .
N1 N 0.6636(2) 0.9273(2) 0.5962(2) 0.0265(6) Uani 1 1 d .
N2 N 0.6278(3) 0.8126(2) 0.5345(3) 0.0284(6) Uani 1 1 d .
N3 N 0.6651(3) 0.6034(3) 0.2752(3) 0.0321(7) Uani 1 1 d .
H3 H 0.692(4) 0.645(4) 0.260(4) 0.034(12) Uiso 1 1 d .
N4 N 0.7081(2) 0.9311(2) 0.7879(2) 0.0261(6) Uani 1 1 d .
N5 N 0.6755(2) 0.8171(2) 0.7437(3) 0.0284(6) Uani 1 1 d .
N6 N 0.7834(3) 0.6219(3) 0.8322(3) 0.0363(8) Uani 1 1 d .
H6 H 0.817(4) 0.678(4) 0.899(4) 0.035(12) Uiso 1 1 d .
N7 N 0.5224(2) 0.9849(2) 0.7166(2) 0.0237(6) Uani 1 1 d .
N8 N 0.4465(2) 0.8822(2) 0.6669(2) 0.0253(6) Uani 1 1 d .
N9 N 0.1427(3) 0.8523(3) 0.6638(3) 0.0313(7) Uani 1 1 d .
H9 H 0.147(3) 0.920(3) 0.691(3) 0.024(10) Uiso 1 1 d .
C1 C 0.7703(4) 1.0864(4) 0.5814(4) 0.0481(11) Uani 1 1 d .
H1A D 0.7083 1.1295 0.5898 0.072 Uiso 1 1 calc R
H1B D 0.8068 1.0935 0.5276 0.072 Uiso 1 1 calc R
H1C D 0.8286 1.1159 0.6553 0.072 Uiso 1 1 calc R
C2 C 0.7197(3) 0.9638(3) 0.5376(3) 0.0305(8) Uani 1 1 d .
C3 C 0.7198(3) 0.8688(3) 0.4380(3) 0.0323(8) Uani 1 1 d .
H3A D 0.7519 0.8671 0.3806 0.039 Uiso 1 1 calc R
C4 C 0.6625(3) 0.7762(3) 0.4405(3) 0.0276(7) Uani 1 1 d .
C5 C 0.6430(3) 0.6502(3) 0.3751(3) 0.0291(8) Uani 1 1 d .
C6 C 0.6632(4) 0.4801(3) 0.2009(3) 0.0376(9) Uani 1 1 d .
C7 C 0.5396(4) 0.4103(4) 0.1640(4) 0.0575(13) Uani 1 1 d .
H7A D 0.5184 0.4183 0.2314 0.086 Uiso 1 1 calc R
H7B D 0.5379 0.3306 0.1142 0.086 Uiso 1 1 calc R
H7C D 0.4842 0.4376 0.1231 0.086 Uiso 1 1 calc R
C8 C 0.7510(5) 0.4409(4) 0.2686(5) 0.0616(14) Uani 1 1 d .
H8A D 0.7272 0.4473 0.3343 0.092 Uiso 1 1 calc R
H8B D 0.8281 0.4884 0.2949 0.092 Uiso 1 1 calc R
H8C D 0.7534 0.3622 0.2198 0.092 Uiso 1 1 calc R
C9 C 0.6998(6) 0.4705(4) 0.0996(4) 0.0695(17) Uani 1 1 d .
H9A D 0.6440 0.4956 0.0567 0.104 Uiso 1 1 calc R
H9B D 0.7021 0.3917 0.0507 0.104 Uiso 1 1 calc R
H9C D 0.7771 0.5178 0.1259 0.104 Uiso 1 1 calc R
C11 C 0.8512(4) 1.0968(4) 0.9601(4) 0.0497(11) Uani 1 1 d .
H11A D 0.8991 1.1163 0.9201 0.074 Uiso 1 1 calc R
H11B D 0.9004 1.1113 1.0340 0.074 Uiso 1 1 calc R
H11C D 0.7918 1.1428 0.9713 0.074 Uiso 1 1 calc R
C12 C 0.7929(3) 0.9728(3) 0.8900(3) 0.0334(8) Uani 1 1 d .
C13 C 0.8140(3) 0.8833(4) 0.9101(3) 0.0366(9) Uani 1 1 d .
H13 D 0.8671 0.8868 0.9744 0.044 Uiso 1 1 calc R
C14 C 0.7399(3) 0.7867(3) 0.8149(3) 0.0301(8) Uani 1 1 d .
C15 C 0.7276(3) 0.6615(3) 0.7657(3) 0.0309(8) Uani 1 1 d .
C16 C 0.8030(4) 0.5038(4) 0.7973(4) 0.0399(9) Uani 1 1 d .
C17 C 0.8639(4) 0.4676(4) 0.7047(4) 0.0521(12) Uani 1 1 d .
H17A D 0.8138 0.4658 0.6371 0.078 Uiso 1 1 calc R
H17B D 0.8799 0.3923 0.6855 0.078 Uiso 1 1 calc R
H17C D 0.9370 0.5215 0.7321 0.078 Uiso 1 1 calc R
C18 C 0.8807(5) 0.5074(5) 0.9045(4) 0.0658(15) Uani 1 1 d .
H18A D 0.8407 0.5306 0.9633 0.099 Uiso 1 1 calc R
H18B D 0.9538 0.5615 0.9324 0.099 Uiso 1 1 calc R
H18C D 0.8969 0.4323 0.8859 0.099 Uiso 1 1 calc R
C19 C 0.6849(5) 0.4203(4) 0.7541(5) 0.0583(13) Uani 1 1 d .
H19A D 0.6465 0.4442 0.8141 0.087 Uiso 1 1 calc R
H19B D 0.6989 0.3442 0.7337 0.087 Uiso 1 1 calc R
H19C D 0.6351 0.4200 0.6872 0.087 Uiso 1 1 calc R
C21 C 0.5277(4) 1.1955(3) 0.8256(4) 0.0416(10) Uani 1 1 d .
H21A D 0.5977 1.2100 0.8861 0.062 Uiso 1 1 calc R
H21B D 0.4745 1.2429 0.8582 0.062 Uiso 1 1 calc R
H21C D 0.5491 1.2134 0.7700 0.062 Uiso 1 1 calc R
C22 C 0.4687(3) 1.0727(3) 0.7675(3) 0.0288(8) Uani 1 1 d .
C23 C 0.3557(3) 1.0256(3) 0.7511(3) 0.0317(8) Uani 1 1 d .
H23 D 0.2973 1.0644 0.7770 0.038 Uiso 1 1 calc R
C24 C 0.3455(3) 0.9083(3) 0.6882(3) 0.0262(7) Uani 1 1 d .
C25 C 0.2404(3) 0.8162(3) 0.6420(3) 0.0283(7) Uani 1 1 d .
C26 C 0.0225(3) 0.7828(3) 0.6196(4) 0.0361(9) Uani 1 1 d .
C27 C -0.0538(4) 0.8609(4) 0.6765(4) 0.0476(11) Uani 1 1 d .
H27A D -0.0254 0.8910 0.7589 0.071 Uiso 1 1 calc R
H27B D -0.1339 0.8188 0.6482 0.071 Uiso 1 1 calc R
H27C D -0.0511 0.9233 0.6590 0.071 Uiso 1 1 calc R
C28 C -0.0205(4) 0.7355(6) 0.4912(4) 0.080(2) Uani 1 1 d .
H28A D 0.0291 0.6853 0.4553 0.119 Uiso 1 1 calc R
H28B D -0.0178 0.7977 0.4734 0.119 Uiso 1 1 calc R
H28C D -0.1006 0.6930 0.4623 0.119 Uiso 1 1 calc R
C29 C 0.0220(5) 0.6885(5) 0.6526(7) 0.090(2) Uani 1 1 d .
H29A D 0.0709 0.6375 0.6163 0.135 Uiso 1 1 calc R
H29B D -0.0576 0.6460 0.6271 0.135 Uiso 1 1 calc R
H29C D 0.0523 0.7218 0.7353 0.135 Uiso 1 1 calc R
Cl1 Cl 0.88386(9) 0.78369(8) 1.18583(9) 0.0379(2) Uani 1 1 d .
O5 O 0.9098(3) 0.8956(3) 1.2834(3) 0.0664(10) Uani 1 1 d .
O6 O 0.7631(3) 0.7327(3) 1.1602(4) 0.0752(12) Uani 1 1 d .
O7 O 0.9024(4) 0.7892(4) 1.0915(3) 0.0940(15) Uani 1 1 d .
O8 O 0.9550(4) 0.7151(4) 1.2129(4) 0.0914(15) Uani 1 1 d .
Cl3 Cl 0.4021(3) 0.89844(16) 0.94789(16) 0.1198(8) Uani 1 1 d .
C30 C 0.5209(10) 0.9398(9) 0.9584(9) 0.058(2) Uiso 0.50 1 d P
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'
Cl Cl 0.1484 0.1585 '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'
D D 0.0000 0.0000 '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
O4 Zn1 N5 124.87(13) . .
O4 Zn1 N2 127.08(13) . .
N5 Zn1 N2 85.98(12) . .
O4 Zn1 O1 97.32(12) . .
N5 Zn1 O1 136.21(11) . .
N2 Zn1 O1 75.73(11) . .
O4 Zn1 O2 96.51(12) . .
N5 Zn1 O2 74.43(11) . .
N2 Zn1 O2 135.36(11) . .
O1 Zn1 O2 91.19(10) . .
H1 B1 N7 115.1(18) . .
H1 B1 N1 106.0(18) . .
N7 B1 N1 110.5(3) . .
H1 B1 N4 108.2(18) . .
N7 B1 N4 108.6(3) . .
N1 B1 N4 108.1(3) . .
C5 O1 Zn1 113.7(2) . .
C15 O2 Zn1 112.4(2) . .
H4A O4 Zn1 117(4) . .
N2 N1 C2 108.7(3) . .
N2 N1 B1 119.3(3) . .
C2 N1 B1 131.4(3) . .
C4 N2 N1 108.4(3) . .
C4 N2 Zn1 119.5(2) . .
N1 N2 Zn1 129.6(2) . .
H3 N3 C5 115(3) . .
H3 N3 C6 117(3) . .
C5 N3 C6 127.3(3) . .
N5 N4 C12 108.4(3) . .
N5 N4 B1 120.2(3) . .
C12 N4 B1 131.4(3) . .
C14 N5 N4 108.4(3) . .
C14 N5 Zn1 121.4(2) . .
N4 N5 Zn1 128.8(2) . .
H6 N6 C15 109(3) . .
H6 N6 C16 123(3) . .
C15 N6 C16 127.9(4) . .
C22 N7 N8 110.8(3) . .
C22 N7 B1 127.9(3) . .
N8 N7 B1 121.0(3) . .
C24 N8 N7 105.0(3) . .
H9 N9 C25 115(3) . .
H9 N9 C26 116(3) . .
C25 N9 C26 127.6(3) . .
N1 C2 C3 107.6(3) . .
N1 C2 C1 122.8(3) . .
C3 C2 C1 129.6(4) . .
C2 C3 C4 105.7(3) . .
N2 C4 C3 109.6(3) . .
N2 C4 C5 112.7(3) . .
C3 C4 C5 137.2(3) . .
O1 C5 N3 123.8(3) . .
O1 C5 C4 117.8(3) . .
N3 C5 C4 118.4(3) . .
N3 C6 C9 107.1(3) . .
N3 C6 C8 108.9(3) . .
C9 C6 C8 109.5(4) . .
N3 C6 C7 109.5(3) . .
C9 C6 C7 111.4(4) . .
C8 C6 C7 110.3(4) . .
N4 C12 C13 108.4(3) . .
N4 C12 C11 122.1(4) . .
C13 C12 C11 129.5(4) . .
C12 C13 C14 105.3(3) . .
N5 C14 C13 109.4(3) . .
N5 C14 C15 113.2(3) . .
C13 C14 C15 136.6(3) . .
O2 C15 N6 123.8(4) . .
O2 C15 C14 118.1(3) . .
N6 C15 C14 118.0(4) . .
N6 C16 C17 110.1(3) . .
N6 C16 C18 106.3(4) . .
C17 C16 C18 110.2(4) . .
N6 C16 C19 110.2(3) . .
C17 C16 C19 110.1(4) . .
C18 C16 C19 109.9(4) . .
N7 C22 C23 107.2(3) . .
N7 C22 C21 123.5(3) . .
C23 C22 C21 129.3(3) . .
C22 C23 C24 105.6(3) . .
N8 C24 C23 111.4(3) . .
N8 C24 C25 119.9(3) . .
C23 C24 C25 128.7(3) . .
O3 C25 N9 122.7(3) . .
O3 C25 C24 122.4(3) . .
N9 C25 C24 114.9(3) . .
N9 C26 C27 107.1(3) . .
N9 C26 C28 109.2(3) . .
C27 C26 C28 110.1(4) . .
N9 C26 C29 109.9(4) . .
C27 C26 C29 108.8(4) . .
C28 C26 C29 111.8(5) . .
O7 Cl1 O8 109.8(3) . .
O7 Cl1 O5 110.8(3) . .
O8 Cl1 O5 109.7(2) . .
O7 Cl1 O6 110.1(3) . .
O8 Cl1 O6 107.9(3) . .
O5 Cl1 O6 108.4(2) . .
C30 Cl3 C30 57.4(7) . 2_677
Cl3 C30 C30 77.2(8) . 2_677
Cl3 C30 Cl3 122.6(6) . 2_677
C30 C30 Cl3 45.4(6) 2_677 2_677
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O4 1.922(3) .
Zn1 N5 2.019(3) .
Zn1 N2 2.024(3) .
Zn1 O1 2.190(3) .
Zn1 O2 2.276(3) .
B1 H1 1.04(3) .
B1 N7 1.532(5) .
B1 N1 1.559(5) .
B1 N4 1.561(5) .
O1 C5 1.259(4) .
O2 C15 1.259(5) .
O3 C25 1.236(4) .
O4 H4A 0.77(5) .
N1 N2 1.354(4) .
N1 C2 1.370(5) .
N2 C4 1.328(4) .
N3 H3 0.76(4) .
N3 C5 1.319(5) .
N3 C6 1.496(5) .
N4 N5 1.353(4) .
N4 C12 1.363(5) .
N5 C14 1.332(5) .
N6 H6 0.85(4) .
N6 C15 1.332(5) .
N6 C16 1.491(5) .
N7 C22 1.365(4) .
N7 N8 1.369(4) .
N8 C24 1.340(4) .
N9 H9 0.81(4) .
N9 C25 1.341(5) .
N9 C26 1.483(5) .
C1 C2 1.495(5) .
C2 C3 1.383(5) .
C3 C4 1.392(5) .
C4 C5 1.482(5) .
C6 C9 1.497(6) .
C6 C8 1.524(7) .
C6 C7 1.531(6) .
C11 C12 1.503(6) .
C12 C13 1.378(6) .
C13 C14 1.394(5) .
C14 C15 1.482(5) .
C16 C17 1.509(6) .
C16 C18 1.524(6) .
C16 C19 1.545(7) .
C21 C22 1.496(5) .
C22 C23 1.372(5) .
C23 C24 1.392(5) .
C24 C25 1.487(5) .
C26 C27 1.504(6) .
C26 C28 1.510(7) .
C26 C29 1.526(6) .
Cl1 O7 1.388(4) .
Cl1 O8 1.413(4) .
Cl1 O5 1.437(3) .
Cl1 O6 1.443(4) .
Cl3 C30 1.436(11) .
Cl3 C30 1.965(11) 2_677
C30 C30 1.70(2) 2_677
C30 Cl3 1.965(11) 2_677
