#------------------------------------------------------------------------------
#$Date: 2024-11-15 14:46:36 +0200 (Fri, 15 Nov 2024) $
#$Revision: 295934 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/88/4308848.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_4308848
loop_
_publ_author_name
'Florian Gross'
'Heinrich Vahrenkamp'
_publ_section_title
;
Zinc Complex Chemistry of N,N,O Ligands Providing a Hydrophobic Cavity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3321
_journal_page_last               3329
_journal_paper_doi               10.1021/ic050042u
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C33 H40 Cl1 N3 O6 Zn, C H2 Cl2'
_chemical_formula_sum            'C34 H42 Cl3 N3 O6 Zn'
_chemical_formula_weight         760.60
_chemical_melting_point          428
_chemical_name_common            tbupypyphZnAqua
_chemical_name_systematic
; 
 (2-Picolyl)(6-phenyl-2-picolyl)(2-hydroxy-3,5-di-tert-butyl-benzyl)amin-
aqua-zink-perchlorat
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.51(8)
_cell_angle_beta                 108.20(7)
_cell_angle_gamma                111.18(8)
_cell_formula_units_Z            2
_cell_length_a                   11.85(5)
_cell_length_b                   12.46(5)
_cell_length_c                   14.44(6)
_cell_measurement_temperature    223(2)
_cell_volume                     1826(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      223(2)
_diffrn_measured_fraction_theta_full 0.770
_diffrn_measured_fraction_theta_max 0.770
_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  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0946
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10878
_diffrn_reflns_theta_full        29.36
_diffrn_reflns_theta_max         29.36
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.938
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       isometric
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.270
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.888
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.888
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0520
_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)+(0.0560P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1252
_reflns_number_gt                4355
_reflns_number_total             7736
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050042usi20050112_050420_1.cif
_cod_data_source_block           grosjm
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_angle_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (83
times).

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (51 time).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4308848
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 1.80368(4) 1.79366(4) 0.66383(3) 0.03027(13) Uani 1 1 d . . .
N1 N 1.9971(3) 1.9052(3) 0.7792(2) 0.0383(8) Uani 1 1 d . . .
N2 N 1.7704(3) 1.6265(2) 0.5814(2) 0.0283(6) Uani 1 1 d . . .
N3 N 1.8175(3) 1.7024(2) 0.7828(2) 0.0302(7) Uani 1 1 d . . .
O1 O 1.6637(2) 1.8207(2) 0.68161(19) 0.0394(6) Uani 1 1 d . . .
O2 O 1.8268(2) 1.8879(2) 0.56045(19) 0.0431(7) Uani 1 1 d . . .
H8A H 1.7733 1.9265 0.5385 0.052 Uiso 1 1 calc R . .
H8B H 1.8910 1.8925 0.5350 0.052 Uiso 1 1 calc R . .
O3 O 1.0235(3) 1.3137(3) 0.6183(2) 0.0665(9) Uani 1 1 d . . .
O4 O 0.8533(3) 1.1230(3) 0.5650(3) 0.0686(9) Uani 1 1 d . . .
O5 O 0.9396(3) 1.2011(3) 0.4476(2) 0.0808(10) Uani 1 1 d . . .
O6 O 1.0647(3) 1.1495(3) 0.5806(2) 0.0543(8) Uani 1 1 d . . .
C1 C 2.0163(3) 1.8885(3) 0.8737(3) 0.0377(9) Uani 1 1 d . . .
C2 C 2.1339(4) 1.9565(4) 0.9575(3) 0.0520(11) Uani 1 1 d . . .
H2A H 2.1425 1.9425 1.0207 0.062 Uiso 1 1 calc R . .
C3 C 2.2356(4) 2.0432(4) 0.9460(4) 0.0608(13) Uani 1 1 d . . .
H3B H 2.3139 2.0894 1.0003 0.073 Uiso 1 1 calc R . .
C4 C 2.2167(4) 2.0593(4) 0.8489(4) 0.0569(12) Uani 1 1 d . . .
H4B H 2.2839 2.1167 0.8378 0.068 Uiso 1 1 calc R . .
C5 C 2.0969(4) 1.9894(3) 0.7679(3) 0.0466(10) Uani 1 1 d . . .
H5B H 2.0867 2.0022 0.7042 0.056 Uiso 1 1 calc R . .
C6 C 1.9013(4) 1.7923(3) 0.8826(3) 0.0387(9) Uani 1 1 d . . .
H6B H 1.9326 1.7534 0.9329 0.046 Uiso 1 1 calc R . .
H6C H 1.8498 1.8273 0.9042 0.046 Uiso 1 1 calc R . .
C7 C 1.8338(3) 1.5775(3) 0.6437(3) 0.0313(8) Uani 1 1 d . . .
C8 C 1.8578(4) 1.4850(3) 0.6051(3) 0.0421(10) Uani 1 1 d . . .
H8C H 1.9044 1.4525 0.6484 0.051 Uiso 1 1 calc R . .
C9 C 1.8112(4) 1.4398(3) 0.4995(3) 0.0455(10) Uani 1 1 d . . .
H9A H 1.8307 1.3799 0.4736 0.055 Uiso 1 1 calc R . .
C10 C 1.7374(4) 1.4839(3) 0.4350(3) 0.0396(9) Uani 1 1 d . . .
H10A H 1.7016 1.4520 0.3656 0.048 Uiso 1 1 calc R . .
C11 C 1.7186(3) 1.5780(3) 0.4780(3) 0.0310(8) Uani 1 1 d . . .
C12 C 1.6350(4) 1.6233(3) 0.4113(3) 0.0341(8) Uani 1 1 d . . .
C13 C 1.5430(4) 1.6500(3) 0.4382(3) 0.0403(9) Uani 1 1 d . . .
H13A H 1.5374 1.6429 0.5002 0.048 Uiso 1 1 calc R . .
C14 C 1.4603(4) 1.6869(3) 0.3729(3) 0.0491(11) Uani 1 1 d . . .
H14A H 1.3994 1.7050 0.3911 0.059 Uiso 1 1 calc R . .
C15 C 1.4681(5) 1.6970(3) 0.2791(3) 0.0560(12) Uani 1 1 d . . .
H15A H 1.4115 1.7209 0.2350 0.067 Uiso 1 1 calc R . .
C16 C 1.5594(4) 1.6716(4) 0.2518(3) 0.0535(11) Uani 1 1 d . . .
H16A H 1.5651 1.6796 0.1899 0.064 Uiso 1 1 calc R . .
C17 C 1.6422(4) 1.6344(3) 0.3168(3) 0.0426(10) Uani 1 1 d . . .
H17A H 1.7030 1.6165 0.2982 0.051 Uiso 1 1 calc R . .
C18 C 1.8806(4) 1.6282(3) 0.7585(3) 0.0365(9) Uani 1 1 d . . .
H18A H 1.8622 1.5628 0.7902 0.044 Uiso 1 1 calc R . .
H18B H 1.9746 1.6751 0.7860 0.044 Uiso 1 1 calc R . .
C19 C 1.6041(3) 1.6973(3) 0.7890(3) 0.0290(8) Uani 1 1 d . . .
C20 C 1.5266(3) 1.6605(3) 0.8458(3) 0.0323(8) Uani 1 1 d . . .
H20A H 1.5350 1.6028 0.8794 0.039 Uiso 1 1 calc R . .
C21 C 1.4391(3) 1.7054(3) 0.8541(3) 0.0329(8) Uani 1 1 d . . .
C22 C 1.4357(3) 1.7946(3) 0.8071(3) 0.0335(8) Uani 1 1 d . . .
H22A H 1.3794 1.8287 0.8129 0.040 Uiso 1 1 calc R . .
C23 C 1.5109(3) 1.8370(3) 0.7514(3) 0.0312(8) Uani 1 1 d . . .
C24 C 1.5970(3) 1.7853(3) 0.7403(3) 0.0302(8) Uani 1 1 d . . .
C25 C 1.6824(3) 1.6301(3) 0.7746(3) 0.0331(8) Uani 1 1 d . . .
H25A H 1.6875 1.5838 0.8241 0.040 Uiso 1 1 calc R . .
H25B H 1.6349 1.5745 0.7086 0.040 Uiso 1 1 calc R . .
C26 C 1.3458(4) 1.6613(3) 0.9098(3) 0.0403(9) Uani 1 1 d . . .
C27 C 1.3751(5) 1.7629(4) 0.9987(3) 0.0676(14) Uani 1 1 d . . .
H27A H 1.4638 1.7901 1.0454 0.101 Uiso 1 1 calc R . .
H27B H 1.3163 1.7337 1.0323 0.101 Uiso 1 1 calc R . .
H27C H 1.3634 1.8276 0.9733 0.101 Uiso 1 1 calc R . .
C28 C 1.3611(5) 1.5619(4) 0.9542(3) 0.0643(13) Uani 1 1 d . . .
H28A H 1.3434 1.4966 0.9016 0.097 Uiso 1 1 calc R . .
H28B H 1.3008 1.5362 0.9871 0.097 Uiso 1 1 calc R . .
H28C H 1.4490 1.5894 1.0024 0.097 Uiso 1 1 calc R . .
C29 C 1.2025(4) 1.6119(4) 0.8320(3) 0.0607(13) Uani 1 1 d . . .
H29A H 1.1878 1.5487 0.7788 0.091 Uiso 1 1 calc R . .
H29B H 1.1882 1.6745 0.8042 0.091 Uiso 1 1 calc R . .
H29C H 1.1430 1.5822 0.8649 0.091 Uiso 1 1 calc R . .
C30 C 1.5025(4) 1.9356(3) 0.7013(3) 0.0387(9) Uani 1 1 d . . .
C31 C 1.4058(4) 1.9794(4) 0.7237(3) 0.0539(12) Uani 1 1 d . . .
H31A H 1.4348 2.0095 0.7951 0.081 Uiso 1 1 calc R . .
H31B H 1.3205 1.9145 0.6990 0.081 Uiso 1 1 calc R . .
H31C H 1.4018 2.0416 0.6910 0.081 Uiso 1 1 calc R . .
C32 C 1.6378(4) 2.0421(3) 0.7428(4) 0.0580(12) Uani 1 1 d . . .
H32A H 1.6666 2.0689 0.8146 0.087 Uiso 1 1 calc R . .
H32B H 1.6317 2.1056 0.7127 0.087 Uiso 1 1 calc R . .
H32C H 1.6995 2.0181 0.7271 0.087 Uiso 1 1 calc R . .
C33 C 1.4510(4) 1.8888(4) 0.5830(3) 0.0514(11) Uani 1 1 d . . .
H33A H 1.3666 1.8228 0.5590 0.077 Uiso 1 1 calc R . .
H33B H 1.5112 1.8636 0.5660 0.077 Uiso 1 1 calc R . .
H33C H 1.4440 1.9515 0.5520 0.077 Uiso 1 1 calc R . .
C34 C 1.9513(5) 2.2922(4) 0.8078(4) 0.0740(15) Uani 1 1 d . . .
H34A H 1.8682 2.2333 0.7580 0.089 Uiso 1 1 calc R . .
H34B H 1.9912 2.3498 0.7748 0.089 Uiso 1 1 calc R . .
Cl1 Cl 0.96882(10) 1.19684(9) 0.55181(8) 0.0461(3) Uani 1 1 d . . .
Cl2 Cl 1.92301(16) 2.36457(14) 0.90375(12) 0.0972(5) Uani 1 1 d . . .
Cl3 Cl 2.0494(2) 2.22475(19) 0.85230(14) 0.1428(9) Uani 1 1 d . . .
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'
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'
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
O1 Zn1 O2 98.16(18) . . y
O1 Zn1 N2 120.57(17) . . y
O2 Zn1 N2 99.1(3) . . y
O1 Zn1 N3 90.99(18) . . y
O2 Zn1 N3 169.38(12) . . y
N2 Zn1 N3 80.6(3) . . y
O1 Zn1 N1 115.5(3) . . y
O2 Zn1 N1 95.2(3) . . y
N2 Zn1 N1 118.9(2) . . y
N3 Zn1 N1 75.9(3) . . y
C5 N1 C1 117.0(4) . . y
C5 N1 Zn1 127.2(4) . . y
C1 N1 Zn1 115.8(3) . . y
C7 N2 C11 120.0(4) . . y
C7 N2 Zn1 108.7(4) . . y
C11 N2 Zn1 130.0(2) . . y
C18 N3 C25 112.0(4) . . y
C18 N3 C6 111.5(4) . . y
C25 N3 C6 113.2(3) . . y
C18 N3 Zn1 102.5(3) . . y
C25 N3 Zn1 107.7(3) . . y
C6 N3 Zn1 109.2(4) . . y
C24 O1 Zn1 132.0(3) . . y
N1 C1 C2 122.9(4) . . y
N1 C1 C6 115.1(3) . . y
C2 C1 C6 122.0(5) . . y
C3 C2 C1 120.0(5) . . y
C2 C3 C4 117.1(4) . . y
C3 C4 C5 120.5(5) . . y
N1 C5 C4 122.4(5) . . y
N3 C6 C1 110.0(4) . . y
N2 C7 C8 119.9(4) . . y
N2 C7 C18 118.3(4) . . y
C8 C7 C18 121.7(3) . . y
C7 C8 C9 119.9(4) . . y
C10 C9 C8 120.3(4) . . y
C9 C10 C11 117.1(4) . . y
C10 C11 N2 122.4(4) . . y
C10 C11 C12 118.2(4) . . y
N2 C11 C12 119.3(3) . . y
C13 C12 C17 119.3(4) . . y
C13 C12 C11 120.3(4) . . y
C17 C12 C11 120.3(4) . . y
C14 C13 C12 120.0(5) . . y
C13 C14 C15 120.1(4) . . y
C16 C15 C14 120.4(4) . . y
C17 C16 C15 119.7(5) . . y
C16 C17 C12 120.5(4) . . y
N3 C18 C7 112.6(3) . . y
C24 C19 C20 120.0(3) . . y
C24 C19 C25 121.6(3) . . y
C20 C19 C25 118.1(4) . . y
C21 C20 C19 123.4(4) . . y
C20 C21 C22 115.6(4) . . y
C20 C21 C26 124.8(4) . . y
C22 C21 C26 119.5(3) . . y
C21 C22 C23 124.2(3) . . y
C22 C23 C24 119.0(4) . . y
C22 C23 C30 121.6(3) . . y
C24 C23 C30 119.4(3) . . y
O1 C24 C19 123.0(3) . . y
O1 C24 C23 119.3(4) . . y
C19 C24 C23 117.7(3) . . y
N3 C25 C19 116.5(4) . . y
C28 C26 C21 112.0(4) . . y
C28 C26 C27 106.5(5) . . y
C21 C26 C27 110.7(4) . . y
C28 C26 C29 107.4(4) . . y
C21 C26 C29 108.3(5) . . y
C27 C26 C29 112.0(4) . . y
C23 C30 C31 110.9(3) . . y
C23 C30 C32 109.5(4) . . y
C31 C30 C32 107.7(5) . . y
C23 C30 C33 110.3(4) . . y
C31 C30 C33 107.2(4) . . y
C32 C30 C33 111.2(3) . . y
Cl3 C34 Cl2 112.1(4) . . y
O4 Cl1 O6 109.4(4) . . y
O4 Cl1 O3 108.9(3) . . y
O6 Cl1 O3 107.3(3) . . y
O4 Cl1 O5 110.7(3) . . y
O6 Cl1 O5 108.8(2) . . y
O3 Cl1 O5 111.7(3) . . y
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
Zn1 O1 1.893(7) . y
Zn1 O2 2.026(7) . y
Zn1 N2 2.113(8) . y
Zn1 N3 2.162(7) . y
Zn1 N1 2.179(8) . y
N1 C5 1.337(6) . y
N1 C1 1.365(7) . y
N2 C7 1.335(5) . y
N2 C11 1.387(7) . y
N3 C18 1.458(6) . y
N3 C25 1.485(7) . y
N3 C6 1.501(7) . y
O1 C24 1.338(5) . y
O3 Cl1 1.440(6) . y
O4 Cl1 1.432(6) . y
O5 Cl1 1.447(7) . y
O6 Cl1 1.434(5) . y
C1 C2 1.409(7) . y
C1 C6 1.508(7) . y
C2 C3 1.368(7) . y
C3 C4 1.399(8) . y
C4 C5 1.407(7) . y
C7 C8 1.382(6) . y
C7 C18 1.546(8) . y
C8 C9 1.416(8) . y
C9 C10 1.374(6) . y
C10 C11 1.387(6) . y
C11 C12 1.470(6) . y
C12 C13 1.395(7) . y
C12 C17 1.413(8) . y
C13 C14 1.382(6) . y
C14 C15 1.403(8) . y
C15 C16 1.383(7) . y
C16 C17 1.383(6) . y
C19 C24 1.382(6) . y
C19 C20 1.406(6) . y
C19 C25 1.499(6) . y
C20 C21 1.372(6) . y
C21 C22 1.373(7) . y
C21 C26 1.544(6) . y
C22 C23 1.387(6) . y
C23 C24 1.426(6) . y
C23 C30 1.513(7) . y
C26 C28 1.499(7) . y
C26 C27 1.551(7) . y
C26 C29 1.556(8) . y
C30 C31 1.535(7) . y
C30 C32 1.541(7) . y
C30 C33 1.581(9) . y
C34 Cl3 1.683(7) . y
C34 Cl2 1.752(7) . y
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2024-11-15T14:40:08+02:00
;
 Removed multiple data items that had the 'Y' placeholder value.
;
