#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:32:49 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180144 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/41/7104117.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_7104117
loop_
_publ_author_name
'Lewiński, Janusz'
'Suwała, Karolina'
'Kaczorowski, Tomasz'
'Gałezowski, Michał'
'Gryko, Daniel T'
'Justyniak, Iwona'
'Lipkowski, Janusz'
_publ_section_title
;
 Oxygenation of alkylzinc complexes with pyrrolylketiminate ligand:
 access to alkylperoxide versus oxo-encapsulated complexes.
;
_journal_issue                   2
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              215
_journal_page_last               217
_journal_paper_doi               10.1039/b813315h
_journal_volume                  34
_journal_year                    2008
_chemical_formula_sum            'C48 H54 N12 O Zn4'
_chemical_formula_weight         1076.17
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 122.651(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.1870(13)
_cell_length_b                   17.1310(12)
_cell_length_c                   19.3830(12)
_cell_measurement_reflns_used    68064
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.407
_cell_volume                     6203.0(7)
_computing_cell_refinement       'Denzo & Scalepak (Otwinowski, Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction        'Denzo & Scalepak (Otwinowski, Minor, 1997)'
_computing_molecular_graphics
;
DIAMOND v2.1 (Brandenburg, 1999)
Ortep-3 for Windows, L.J.Farrugia (1997) J.Appl.Cryst. 30, 565,
ORTEP III (Burnett, Johnson, 1996)
;
_computing_publication_material
;
SHELXL-97 (Sheldrick, 1997),
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
259 frames, ω rotation 0.7° per frame (184s per frame)
78 frames, ω rotation 0.7° per frame (184s per frame)

;
_diffrn_measurement_device       'κ-geometry diffractometr'
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'area detector 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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5664
_diffrn_reflns_theta_full        21.97
_diffrn_reflns_theta_max         21.97
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    1.566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepak (Otwinowski, Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         3721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0543
_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)+(0.0561P)²+52.2726P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1395
_reflns_number_gt                3093
_reflns_number_total             3721
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b813315h.txt
_cod_data_source_block           shelxl2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      'C 2/c'
_cod_database_code               7104117
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
C1 C 0.1044(3) -0.0865(4) 0.7741(4) 0.0327(16) Uani 1 1 d . . .
H1 H 0.0662 -0.1115 0.7743 0.039 Uiso 1 1 calc R . .
C2 C 0.1684(4) -0.1223(4) 0.7975(4) 0.0390(17) Uani 1 1 d . . .
H2 H 0.1817 -0.1747 0.8152 0.047 Uiso 1 1 calc R . .
C3 C 0.2096(4) -0.0655(4) 0.7898(4) 0.0361(17) Uani 1 1 d . . .
H3 H 0.2570 -0.0718 0.8021 0.043 Uiso 1 1 calc R . .
C4 C 0.1693(3) 0.0004(4) 0.7614(4) 0.0308(16) Uani 1 1 d . . .
C5 C 0.1781(3) 0.0759(4) 0.7346(4) 0.0299(16) Uani 1 1 d . . .
C6 C 0.2435(4) 0.1024(4) 0.7353(4) 0.0407(18) Uani 1 1 d . . .
H6A H 0.2504 0.0708 0.6973 0.049 Uiso 1 1 calc R . .
H6B H 0.2872 0.0990 0.7910 0.049 Uiso 1 1 calc R . .
C7 C 0.2259(4) 0.1871(4) 0.7066(4) 0.0425(18) Uani 1 1 d . . .
H7A H 0.2338 0.1971 0.6617 0.051 Uiso 1 1 calc R . .
H7B H 0.2560 0.2234 0.7523 0.051 Uiso 1 1 calc R . .
C8 C 0.1459(3) 0.1970(4) 0.6760(4) 0.0355(16) Uani 1 1 d . . .
H8A H 0.1387 0.2444 0.7000 0.043 Uiso 1 1 calc R . .
H8B H 0.1163 0.2014 0.6156 0.043 Uiso 1 1 calc R . .
C9 C -0.0628(4) -0.0299(4) 0.5667(4) 0.0441(19) Uani 1 1 d . . .
H9A H -0.0957 -0.0434 0.5847 0.053 Uiso 1 1 calc R . .
H9B H -0.0206 -0.0647 0.5954 0.053 Uiso 1 1 calc R . .
C10 C -0.1002(4) -0.0399(5) 0.4752(4) 0.049(2) Uani 1 1 d . . .
H10A H -0.0736 -0.0765 0.4616 0.059 Uiso 1 1 calc R . .
H10B H -0.1495 -0.0599 0.4514 0.059 Uiso 1 1 calc R . .
C11 C -0.1013(4) 0.0393(4) 0.4444(4) 0.0430(19) Uani 1 1 d . . .
H11A H -0.1512 0.0570 0.4065 0.052 Uiso 1 1 calc R . .
H11B H -0.0763 0.0398 0.4149 0.052 Uiso 1 1 calc R . .
C12 C -0.0643(3) 0.0905(4) 0.5172(4) 0.0330(16) Uani 1 1 d . . .
C13 C -0.0543(3) 0.1712(4) 0.5156(4) 0.0339(17) Uani 1 1 d . . .
C14 C -0.0549(4) 0.2128(5) 0.4503(4) 0.0404(18) Uani 1 1 d . . .
H14 H -0.0674 0.1926 0.3986 0.049 Uiso 1 1 calc R . .
C15 C -0.0325(4) 0.2921(5) 0.4807(4) 0.049(2) Uani 1 1 d . . .
H15 H -0.0244 0.3335 0.4540 0.059 Uiso 1 1 calc R . .
C16 C -0.0250(3) 0.2951(4) 0.5586(4) 0.0391(18) Uani 1 1 d . . .
H16 H -0.0131 0.3402 0.5920 0.047 Uiso 1 1 calc R . .
C17 C -0.1052(4) 0.3627(4) 0.7125(4) 0.0408(18) Uani 1 1 d . . .
H17 H -0.0600 0.3881 0.7422 0.049 Uiso 1 1 calc R . .
C18 C -0.1686(4) 0.3928(5) 0.7012(5) 0.050(2) Uani 1 1 d . . .
H18 H -0.1744 0.4411 0.7210 0.060 Uiso 1 1 calc R . .
C19 C -0.2213(4) 0.3380(5) 0.6554(5) 0.051(2) Uani 1 1 d . . .
H19 H -0.2704 0.3419 0.6374 0.061 Uiso 1 1 calc R . .
C20 C -0.1891(4) 0.2760(4) 0.6403(4) 0.0375(18) Uani 1 1 d . . .
C21 C -0.2151(4) 0.2042(4) 0.5982(4) 0.0368(17) Uani 1 1 d . . .
C22 C -0.2911(4) 0.1764(5) 0.5552(4) 0.049(2) Uani 1 1 d . . .
H22A H -0.3235 0.2114 0.5091 0.059 Uiso 1 1 calc R . .
H22B H -0.3076 0.1730 0.5934 0.059 Uiso 1 1 calc R . .
C23 C -0.2874(4) 0.0956(5) 0.5243(4) 0.051(2) Uani 1 1 d . . .
H23A H -0.3203 0.0926 0.4640 0.061 Uiso 1 1 calc R . .
H23B H -0.3010 0.0549 0.5496 0.061 Uiso 1 1 calc R . .
C24 C -0.2098(4) 0.0843(5) 0.5487(4) 0.0424(18) Uani 1 1 d . . .
H24A H -0.1888 0.0372 0.5833 0.051 Uiso 1 1 calc R . .
H24B H -0.2072 0.0788 0.4996 0.051 Uiso 1 1 calc R . .
O1 O 0.0000 0.1426(3) 0.7500 0.0274(14) Uani 1 2 d S . .
Zn1 Zn 0.03926(4) 0.08132(4) 0.69794(4) 0.0269(2) Uani 1 1 d . . .
Zn2 Zn -0.07098(4) 0.20298(4) 0.65454(4) 0.0279(2) Uani 1 1 d . . .
N1 N 0.1024(3) -0.0122(3) 0.7510(3) 0.0282(12) Uani 1 1 d . . .
N2 N 0.1268(3) 0.1273(3) 0.7030(3) 0.0284(13) Uani 1 1 d . . .
N3 N -0.0411(3) 0.0496(3) 0.5855(3) 0.0294(13) Uani 1 1 d . . .
N4 N -0.0381(3) 0.2206(3) 0.5780(3) 0.0287(13) Uani 1 1 d . . .
N5 N -0.1171(3) 0.2926(3) 0.6752(3) 0.0329(13) Uani 1 1 d . . .
N6 N -0.1713(3) 0.1558(3) 0.5955(3) 0.0335(14) 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'
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'
N N 0.0061 0.0033 '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
N1 C1 C2 111.9(6) . . ?
N1 C1 H1 124.1 . . ?
C2 C1 H1 124.1 . . ?
C1 C2 C3 105.9(6) . . ?
C1 C2 H2 127.1 . . ?
C3 C2 H2 127.1 . . ?
C4 C3 C2 107.2(6) . . ?
C4 C3 H3 126.4 . . ?
C2 C3 H3 126.4 . . ?
C3 C4 N1 110.2(6) . . ?
C3 C4 C5 134.5(6) . . ?
N1 C4 C5 115.1(5) . . ?
N2 C5 C4 121.3(6) . . ?
N2 C5 C6 113.1(6) . . ?
C4 C5 C6 125.5(6) . . ?
C5 C6 C7 103.1(6) . . ?
C5 C6 H6A 111.1 . . ?
C7 C6 H6A 111.1 . . ?
C5 C6 H6B 111.1 . . ?
C7 C6 H6B 111.1 . . ?
H6A C6 H6B 109.1 . . ?
C6 C7 C8 105.0(6) . . ?
C6 C7 H7A 110.8 . . ?
C8 C7 H7A 110.8 . . ?
C6 C7 H7B 110.8 . . ?
C8 C7 H7B 110.8 . . ?
H7A C7 H7B 108.8 . . ?
N2 C8 C7 105.6(5) . . ?
N2 C8 H8A 110.6 . . ?
C7 C8 H8A 110.6 . . ?
N2 C8 H8B 110.6 . . ?
C7 C8 H8B 110.6 . . ?
H8A C8 H8B 108.7 . . ?
N3 C9 C10 107.7(6) . . ?
N3 C9 H9A 110.2 . . ?
C10 C9 H9A 110.2 . . ?
N3 C9 H9B 110.2 . . ?
C10 C9 H9B 110.2 . . ?
H9A C9 H9B 108.5 . . ?
C11 C10 C9 104.5(6) . . ?
C11 C10 H10A 110.9 . . ?
C9 C10 H10A 110.9 . . ?
C11 C10 H10B 110.9 . . ?
C9 C10 H10B 110.9 . . ?
H10A C10 H10B 108.9 . . ?
C10 C11 C12 106.3(6) . . ?
C10 C11 H11A 110.5 . . ?
C12 C11 H11A 110.5 . . ?
C10 C11 H11B 110.5 . . ?
C12 C11 H11B 110.5 . . ?
H11A C11 H11B 108.7 . . ?
N3 C12 C13 124.0(6) . . ?
N3 C12 C11 110.7(6) . . ?
C13 C12 C11 125.3(6) . . ?
N4 C13 C12 124.3(6) . . ?
N4 C13 C14 110.2(6) . . ?
C12 C13 C14 125.3(6) . . ?
C13 C14 C15 105.5(6) . . ?
C13 C14 H14 127.3 . . ?
C15 C14 H14 127.3 . . ?
C16 C15 C14 106.2(7) . . ?
C16 C15 H15 126.9 . . ?
C14 C15 H15 126.9 . . ?
N4 C16 C15 109.1(7) . . ?
N4 C16 H16 125.4 . . ?
C15 C16 H16 125.4 . . ?
N5 C17 C18 110.7(7) . . ?
N5 C17 H17 124.6 . . ?
C18 C17 H17 124.6 . . ?
C19 C18 C17 106.2(7) . . ?
C19 C18 H18 126.9 . . ?
C17 C18 H18 126.9 . . ?
C18 C19 C20 107.5(7) . . ?
C18 C19 H19 126.3 . . ?
C20 C19 H19 126.3 . . ?
N5 C20 C19 109.1(7) . . ?
N5 C20 C21 117.6(6) . . ?
C19 C20 C21 133.3(7) . . ?
N6 C21 C20 119.8(6) . . ?
N6 C21 C22 114.6(7) . . ?
C20 C21 C22 125.6(6) . . ?
C21 C22 C23 102.9(6) . . ?
C21 C22 H22A 111.2 . . ?
C23 C22 H22A 111.2 . . ?
C21 C22 H22B 111.2 . . ?
C23 C22 H22B 111.2 . . ?
H22A C22 H22B 109.1 . . ?
C22 C23 C24 106.5(6) . . ?
C22 C23 H23A 110.4 . . ?
C24 C23 H23A 110.4 . . ?
C22 C23 H23B 110.4 . . ?
C24 C23 H23B 110.4 . . ?
H23A C23 H23B 108.6 . . ?
N6 C24 C23 105.2(6) . . ?
N6 C24 H24A 110.7 . . ?
C23 C24 H24A 110.7 . . ?
N6 C24 H24B 110.7 . . ?
C23 C24 H24B 110.7 . . ?
H24A C24 H24B 108.8 . . ?
Zn1 O1 Zn1 115.1(3) . 2_556 ?
Zn1 O1 Zn2 114.59(3) . 2_556 ?
Zn1 O1 Zn2 98.69(3) 2_556 2_556 ?
Zn1 O1 Zn2 98.69(3) . . ?
Zn1 O1 Zn2 114.59(3) 2_556 . ?
Zn2 O1 Zn2 116.2(3) 2_556 . ?
O1 Zn1 N3 108.86(14) . . ?
O1 Zn1 N1 123.07(17) . . ?
N3 Zn1 N1 107.8(2) . . ?
O1 Zn1 N2 116.28(19) . . ?
N3 Zn1 N2 114.8(2) . . ?
N1 Zn1 N2 84.3(2) . . ?
O1 Zn1 Zn2 40.66(8) . . ?
N3 Zn1 Zn2 76.64(14) . . ?
N1 Zn1 Zn2 161.03(14) . . ?
N2 Zn1 Zn2 110.98(15) . . ?
O1 Zn2 N4 110.58(15) . . ?
O1 Zn2 N5 116.98(18) . . ?
N4 Zn2 N5 117.6(2) . . ?
O1 Zn2 N6 113.50(19) . . ?
N4 Zn2 N6 111.6(2) . . ?
N5 Zn2 N6 84.0(2) . . ?
O1 Zn2 Zn1 40.65(8) . . ?
N4 Zn2 Zn1 74.99(15) . . ?
N5 Zn2 Zn1 156.02(15) . . ?
N6 Zn2 Zn1 111.34(16) . . ?
C1 N1 C4 104.8(5) . . ?
C1 N1 Zn1 144.6(4) . . ?
C4 N1 Zn1 110.1(4) . . ?
C5 N2 C8 111.9(5) . . ?
C5 N2 Zn1 109.2(4) . . ?
C8 N2 Zn1 138.7(4) . . ?
C12 N3 C9 110.7(5) . . ?
C12 N3 Zn1 125.2(5) . . ?
C9 N3 Zn1 121.0(4) . . ?
C13 N4 C16 108.8(5) . . ?
C13 N4 Zn2 122.7(4) . . ?
C16 N4 Zn2 123.1(4) . . ?
C17 N5 C20 106.5(6) . . ?
C17 N5 Zn2 144.6(5) . . ?
C20 N5 Zn2 108.9(5) . . ?
C21 N6 C24 110.8(6) . . ?
C21 N6 Zn2 109.7(5) . . ?
C24 N6 Zn2 139.4(4) . . ?
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
C1 N1 1.342(8) . ?
C1 C2 1.380(9) . ?
C1 H1 0.9500 . ?
C2 C3 1.396(10) . ?
C2 H2 0.9500 . ?
C3 C4 1.359(9) . ?
C3 H3 0.9500 . ?
C4 N1 1.401(8) . ?
C4 C5 1.447(9) . ?
C5 N2 1.302(8) . ?
C5 C6 1.513(9) . ?
C6 C7 1.526(10) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.548(9) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 N2 1.455(8) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 N3 1.426(9) . ?
C9 C10 1.509(10) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.477(11) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.478(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N3 1.332(8) . ?
C12 C13 1.402(10) . ?
C13 N4 1.356(8) . ?
C13 C14 1.445(9) . ?
C14 C15 1.458(11) . ?
C14 H14 0.9500 . ?
C15 C16 1.428(10) . ?
C15 H15 0.9500 . ?
C16 N4 1.404(9) . ?
C16 H16 0.9500 . ?
C17 N5 1.352(9) . ?
C17 C18 1.401(10) . ?
C17 H17 0.9500 . ?
C18 C19 1.384(11) . ?
C18 H18 0.9500 . ?
C19 C20 1.396(10) . ?
C19 H19 0.9500 . ?
C20 N5 1.386(9) . ?
C20 C21 1.416(10) . ?
C21 N6 1.297(8) . ?
C21 C22 1.500(10) . ?
C22 C23 1.528(11) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.532(10) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 N6 1.489(9) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
O1 Zn1 1.956(3) . ?
O1 Zn1 1.956(3) 2_556 ?
O1 Zn2 1.957(3) 2_556 ?
O1 Zn2 1.957(3) . ?
Zn1 N3 2.008(5) . ?
Zn1 N1 2.008(5) . ?
Zn1 N2 2.048(5) . ?
Zn1 Zn2 2.9688(10) . ?
Zn2 N4 1.999(5) . ?
Zn2 N5 2.002(5) . ?
Zn2 N6 2.042(5) . ?
