#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:54:20 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179735 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/31/7003143.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_7003143
loop_
_publ_author_name
'Escudero-Adán, Eduardo C.'
'Benet-Buchholz, Jordi'
'Kleij, Arjan W.'
_publ_section_title
;
 Autocatalytic demetalation of a Zn(salphen) complex provoked by
 unprotected N-heterocycles
;
_journal_issue                   6
_journal_name_full               'Dalton Transactions'
_journal_page_first              734
_journal_page_last               737
_journal_paper_doi               10.1039/b713039b
_journal_year                    2008
_chemical_formula_sum            'C40 H52 N4 O2 Zn'
_chemical_formula_weight         686.23
_chemical_name_systematic
;
?
;
_space_group_IT_number           72
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2 2c'
_symmetry_space_group_name_H-M   'I b a m'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.9872(19)
_cell_length_b                   9.8259(6)
_cell_length_c                   23.0204(13)
_cell_measurement_reflns_used    8767
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.17
_cell_measurement_theta_min      3.04
_cell_volume                     7461.6(8)
_computing_cell_refinement       'Bruker-Nonius Apex v1.0-22 2002'
_computing_data_collection       'Bruker-Nonius Apex v1.0-22 2002'
_computing_data_reduction        'SAINT+ Version 7.06A Bruker-Nonius, 2004'
_computing_molecular_graphics    'Shelxtl Version 6.12 (Sheldrick, 2001)'
_computing_publication_material  'Shelxtl Version 6.12 (Sheldrick, 2001)'
_computing_structure_refinement  'Shelxtl Version 6.12 (Sheldrick, 2001)'
_computing_structure_solution    'Shelxtl Version 6.12 (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Kappa 4-axis goniometer bruker-nonius'
_diffrn_measurement_method
;
Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support
'magnetic support whith 10 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  'Multilayer Montel 200 mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            45014
_diffrn_reflns_theta_full        39.87
_diffrn_reflns_theta_max         39.87
_diffrn_reflns_theta_min         2.79
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_current           90
_diffrn_source_power             50
_diffrn_source_size              '3 mm x 0.3 mm fine focus'
_diffrn_source_type              'Bruker-Nonius FR 591'
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.848602
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Version 2.1 2003 Bruker-Nonius
Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.834
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         11013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0492P)²+2.3282P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0899
_reflns_number_gt                9450
_reflns_number_total             11013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b713039b.txt
_cod_data_source_block           awk221_0
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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      Ibam
_cod_database_code               7003143
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1, y+1, -z+1/2'
'x+1, -y+1, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x, -y, z+1/2'
'-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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.655777(3) 0.605813(11) 0.5000 0.01079(3) Uani 1 2 d S . .
C1 C 0.630782(19) 0.70501(6) 0.38228(2) 0.01147(9) Uani 1 1 d . . .
O1 O 0.623486(14) 0.69178(5) 0.437398(19) 0.01428(8) Uani 1 1 d . . .
N1 N 0.704931(17) 0.59657(6) 0.44292(2) 0.01201(8) Uani 1 1 d . . .
N2 N 0.63324(3) 0.40970(8) 0.5000 0.01418(12) Uani 1 2 d S . .
C2 C 0.598680(19) 0.74659(6) 0.34358(2) 0.01257(9) Uani 1 1 d . . .
N3 N 0.58526(3) 0.25411(8) 0.5000 0.01587(13) Uani 1 2 d S . .
C3 C 0.60691(2) 0.75895(7) 0.28499(2) 0.01452(10) Uani 1 1 d . . .
H3 H 0.5853 0.7852 0.2601 0.017 Uiso 1 1 calc R . .
C4 C 0.64531(2) 0.73525(7) 0.25943(2) 0.01382(9) Uani 1 1 d . . .
C5 C 0.67606(2) 0.69878(7) 0.29645(2) 0.01392(10) Uani 1 1 d . . .
H5 H 0.7024 0.6845 0.2810 0.017 Uiso 1 1 calc R . .
C6 C 0.669844(19) 0.68166(6) 0.35702(2) 0.01224(9) Uani 1 1 d . . .
C7 C 0.55593(2) 0.77237(7) 0.36770(3) 0.01527(10) Uani 1 1 d . . .
C8 C 0.53951(2) 0.64186(9) 0.39604(4) 0.02477(14) Uani 1 1 d . . .
H8A H 0.5114 0.6566 0.4084 0.037 Uiso 1 1 calc R . .
H8B H 0.5562 0.6187 0.4299 0.037 Uiso 1 1 calc R . .
H8C H 0.5405 0.5671 0.3679 0.037 Uiso 1 1 calc R . .
C9 C 0.55714(2) 0.88835(8) 0.41243(3) 0.02038(12) Uani 1 1 d . . .
H9A H 0.5675 0.9711 0.3939 0.031 Uiso 1 1 calc R . .
H9B H 0.5750 0.8628 0.4447 0.031 Uiso 1 1 calc R . .
H9C H 0.5297 0.9051 0.4272 0.031 Uiso 1 1 calc R . .
C10 C 0.52594(3) 0.81357(12) 0.32002(3) 0.02995(19) Uani 1 1 d . . .
H10A H 0.5356 0.8963 0.3007 0.045 Uiso 1 1 calc R . .
H10B H 0.4993 0.8309 0.3374 0.045 Uiso 1 1 calc R . .
H10C H 0.5237 0.7399 0.2915 0.045 Uiso 1 1 calc R . .
C11 C 0.65008(2) 0.74930(7) 0.19355(3) 0.01641(11) Uani 1 1 d . . .
C12 C 0.69277(3) 0.70988(9) 0.17350(3) 0.02306(14) Uani 1 1 d . . .
H12A H 0.7127 0.7702 0.1918 0.035 Uiso 1 1 calc R . .
H12B H 0.6946 0.7187 0.1312 0.035 Uiso 1 1 calc R . .
H12C H 0.6984 0.6155 0.1847 0.035 Uiso 1 1 calc R . .
C13 C 0.61949(3) 0.65481(9) 0.16313(3) 0.02320(14) Uani 1 1 d . . .
H13A H 0.6235 0.5612 0.1767 0.035 Uiso 1 1 calc R . .
H13B H 0.6237 0.6588 0.1210 0.035 Uiso 1 1 calc R . .
H13C H 0.5918 0.6843 0.1723 0.035 Uiso 1 1 calc R . .
C14 C 0.64186(3) 0.89700(8) 0.17520(3) 0.02644(16) Uani 1 1 d . . .
H14A H 0.6149 0.9244 0.1886 0.040 Uiso 1 1 calc R . .
H14B H 0.6431 0.9040 0.1328 0.040 Uiso 1 1 calc R . .
H14C H 0.6623 0.9568 0.1925 0.040 Uiso 1 1 calc R . .
C15 C 0.704486(19) 0.63489(7) 0.38898(2) 0.01277(9) Uani 1 1 d . . .
H15A H 0.7295 0.6316 0.3687 0.015 Uiso 1 1 calc R . .
C16 C 0.740481(18) 0.54628(6) 0.46919(2) 0.01173(9) Uani 1 1 d . . .
C17 C 0.77364(2) 0.49172(7) 0.43938(3) 0.01472(10) Uani 1 1 d . . .
H17A H 0.7736 0.4899 0.3981 0.018 Uiso 1 1 calc R . .
C18 C 0.80665(2) 0.44007(7) 0.46975(3) 0.01531(10) Uani 1 1 d . . .
H18A H 0.8293 0.4047 0.4492 0.018 Uiso 1 1 calc R . .
C19 C 0.59365(3) 0.38785(9) 0.5000 0.01495(14) Uani 1 2 d S . .
H19 H 0.5738 0.4577 0.5000 0.018 Uiso 1 2 calc SR . .
C20 C 0.65104(3) 0.28253(11) 0.5000 0.01714(15) Uani 1 2 d S . .
H20 H 0.6794 0.2654 0.5000 0.021 Uiso 1 2 calc SR . .
C21 C 0.62161(3) 0.18552(10) 0.5000 0.01824(16) Uani 1 2 d S . .
H21 H 0.6254 0.0897 0.5000 0.022 Uiso 1 2 calc SR . .
C22 C 0.54489(4) 0.19448(14) 0.5000 0.0364(3) Uani 1 2 d S . .
H22A H 0.5437 0.1209 0.5287 0.055 Uiso 0.50 1 calc PR A -1
H22B H 0.5389 0.1579 0.4613 0.055 Uiso 0.50 1 calc PR A -1
H22C H 0.5249 0.2645 0.5100 0.055 Uiso 0.50 1 calc PR A -1
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'
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 O1 93.34(3) 10_556 . ?
O1 Zn1 N2 101.79(2) 10_556 . ?
O1 Zn1 N2 101.79(2) . . ?
O1 Zn1 N1 88.76(2) 10_556 10_556 ?
O1 Zn1 N1 153.30(2) . 10_556 ?
N2 Zn1 N1 103.82(2) . 10_556 ?
O1 Zn1 N1 153.30(2) 10_556 . ?
O1 Zn1 N1 88.76(2) . . ?
N2 Zn1 N1 103.82(2) . . ?
N1 Zn1 N1 77.96(3) 10_556 . ?
O1 C1 C6 123.21(5) . . ?
O1 C1 C2 119.73(5) . . ?
C6 C1 C2 117.06(5) . . ?
C1 O1 Zn1 130.85(4) . . ?
C15 N1 C16 121.46(5) . . ?
C15 N1 Zn1 125.49(4) . . ?
C16 N1 Zn1 113.04(4) . . ?
C19 N2 C20 105.83(8) . . ?
C19 N2 Zn1 120.43(6) . . ?
C20 N2 Zn1 133.74(7) . . ?
C3 C2 C1 118.92(6) . . ?
C3 C2 C7 121.25(5) . . ?
C1 C2 C7 119.80(5) . . ?
C19 N3 C21 107.44(8) . . ?
C19 N3 C22 125.65(9) . . ?
C21 N3 C22 126.91(9) . . ?
C2 C3 C4 124.55(6) . . ?
C5 C4 C3 116.49(5) . . ?
C5 C4 C11 124.24(6) . . ?
C3 C4 C11 119.26(6) . . ?
C4 C5 C6 122.28(6) . . ?
C5 C6 C1 120.66(5) . . ?
C5 C6 C15 115.25(5) . . ?
C1 C6 C15 124.03(5) . . ?
C10 C7 C9 107.51(7) . . ?
C10 C7 C2 112.17(5) . . ?
C9 C7 C2 109.91(6) . . ?
C10 C7 C8 107.27(7) . . ?
C9 C7 C8 110.08(6) . . ?
C2 C7 C8 109.83(6) . . ?
C4 C11 C12 111.72(6) . . ?
C4 C11 C14 109.85(6) . . ?
C12 C11 C14 108.57(7) . . ?
C4 C11 C13 109.20(6) . . ?
C12 C11 C13 108.24(6) . . ?
C14 C11 C13 109.21(7) . . ?
N1 C15 C6 126.35(6) . . ?
C17 C16 N1 125.11(5) . . ?
C17 C16 C16 119.40(3) . 10_556 ?
N1 C16 C16 115.41(3) . 10_556 ?
C18 C17 C16 120.41(5) . . ?
C17 C18 C18 120.19(4) . 10_556 ?
N2 C19 N3 111.23(8) . . ?
C21 C20 N2 109.31(9) . . ?
C20 C21 N3 106.18(9) . . ?
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 1.9812(5) 10_556 ?
Zn1 O1 1.9812(5) . ?
Zn1 N2 2.0654(8) . ?
Zn1 N1 2.0890(5) 10_556 ?
Zn1 N1 2.0890(5) . ?
C1 O1 1.2980(7) . ?
C1 C6 1.4322(9) . ?
C1 C2 1.4430(8) . ?
N1 C15 1.2975(8) . ?
N1 C16 1.4089(8) . ?
N2 C19 1.3234(13) . ?
N2 C20 1.3806(13) . ?
C2 C3 1.3810(8) . ?
C2 C7 1.5366(9) . ?
N3 C19 1.3430(12) . ?
N3 C21 1.3756(13) . ?
N3 C22 1.4549(15) . ?
C3 C4 1.4161(9) . ?
C4 C5 1.3725(9) . ?
C4 C11 1.5310(8) . ?
C5 C6 1.4193(8) . ?
C6 C15 1.4348(9) . ?
C7 C10 1.5322(10) . ?
C7 C9 1.5365(10) . ?
C7 C8 1.5374(11) . ?
C11 C12 1.5316(11) . ?
C11 C14 1.5357(10) . ?
C11 C13 1.5396(11) . ?
C16 C17 1.3981(9) . ?
C16 C16 1.4187(11) 10_556 ?
C17 C18 1.3899(9) . ?
C18 C18 1.3928(13) 10_556 ?
C20 C21 1.3604(15) . ?
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
C6 C1 O1 Zn1 -13.69(9) . . . . ?
C2 C1 O1 Zn1 167.03(4) . . . . ?
O1 Zn1 O1 C1 165.17(5) 10_556 . . . ?
N2 Zn1 O1 C1 -92.05(6) . . . . ?
N1 Zn1 O1 C1 71.29(8) 10_556 . . . ?
N1 Zn1 O1 C1 11.81(6) . . . . ?
O1 Zn1 N1 C15 -97.48(7) 10_556 . . . ?
O1 Zn1 N1 C15 -2.52(6) . . . . ?
N2 Zn1 N1 C15 99.31(6) . . . . ?
N1 Zn1 N1 C15 -159.21(5) 10_556 . . . ?
O1 Zn1 N1 C16 81.00(6) 10_556 . . . ?
O1 Zn1 N1 C16 175.96(4) . . . . ?
N2 Zn1 N1 C16 -82.21(4) . . . . ?
N1 Zn1 N1 C16 19.27(5) 10_556 . . . ?
O1 Zn1 N2 C19 47.991(14) 10_556 . . . ?
O1 Zn1 N2 C19 -47.994(14) . . . . ?
N1 Zn1 N2 C19 139.626(15) 10_556 . . . ?
N1 Zn1 N2 C19 -139.627(15) . . . . ?
O1 Zn1 N2 C20 -132.009(14) 10_556 . . . ?
O1 Zn1 N2 C20 132.006(15) . . . . ?
N1 Zn1 N2 C20 -40.374(16) 10_556 . . . ?
N1 Zn1 N2 C20 40.373(15) . . . . ?
O1 C1 C2 C3 -179.43(6) . . . . ?
C6 C1 C2 C3 1.24(9) . . . . ?
O1 C1 C2 C7 -1.12(9) . . . . ?
C6 C1 C2 C7 179.56(6) . . . . ?
C1 C2 C3 C4 -0.87(10) . . . . ?
C7 C2 C3 C4 -179.16(6) . . . . ?
C2 C3 C4 C5 -0.62(10) . . . . ?
C2 C3 C4 C11 178.54(6) . . . . ?
C3 C4 C5 C6 1.72(10) . . . . ?
C11 C4 C5 C6 -177.39(6) . . . . ?
C4 C5 C6 C1 -1.34(10) . . . . ?
C4 C5 C6 C15 176.14(6) . . . . ?
O1 C1 C6 C5 -179.51(6) . . . . ?
C2 C1 C6 C5 -0.21(9) . . . . ?
O1 C1 C6 C15 3.24(10) . . . . ?
C2 C1 C6 C15 -177.46(6) . . . . ?
C3 C2 C7 C10 -0.91(10) . . . . ?
C1 C2 C7 C10 -179.18(7) . . . . ?
C3 C2 C7 C9 -120.46(7) . . . . ?
C1 C2 C7 C9 61.27(8) . . . . ?
C3 C2 C7 C8 118.29(7) . . . . ?
C1 C2 C7 C8 -59.98(8) . . . . ?
C5 C4 C11 C12 3.22(10) . . . . ?
C3 C4 C11 C12 -175.87(6) . . . . ?
C5 C4 C11 C14 -117.33(8) . . . . ?
C3 C4 C11 C14 63.58(9) . . . . ?
C5 C4 C11 C13 122.93(7) . . . . ?
C3 C4 C11 C13 -56.16(8) . . . . ?
C16 N1 C15 C6 176.97(6) . . . . ?
Zn1 N1 C15 C6 -4.68(10) . . . . ?
C5 C6 C15 N1 -171.24(6) . . . . ?
C1 C6 C15 N1 6.15(11) . . . . ?
C15 N1 C16 C17 -21.43(10) . . . . ?
Zn1 N1 C16 C17 160.03(5) . . . . ?
C15 N1 C16 C16 162.05(5) . . . 10_556 ?
Zn1 N1 C16 C16 -16.50(4) . . . 10_556 ?
N1 C16 C17 C18 -177.52(6) . . . . ?
C16 C16 C17 C18 -1.13(8) 10_556 . . . ?
C16 C17 C18 C18 1.13(8) . . . 10_556 ?
C20 N2 C19 N3 0.0 . . . . ?
Zn1 N2 C19 N3 180.0 . . . . ?
C21 N3 C19 N2 0.0 . . . . ?
C22 N3 C19 N2 180.0 . . . . ?
C19 N2 C20 C21 0.0 . . . . ?
Zn1 N2 C20 C21 180.0 . . . . ?
N2 C20 C21 N3 0.0 . . . . ?
C19 N3 C21 C20 0.0 . . . . ?
C22 N3 C21 C20 180.0 . . . . ?
