#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:32:49 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180144 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/41/7104115.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_7104115
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            'C24 H36 N4 Zn2'
_chemical_formula_weight         511.31
_chemical_name_systematic
;
?
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.1357(11)
_cell_angle_beta                 104.473(2)
_cell_angle_gamma                104.829(2)
_cell_formula_units_Z            1
_cell_length_a                   8.3637(2)
_cell_length_b                   8.7342(3)
_cell_length_c                   9.4312(3)
_cell_measurement_reflns_used    20419
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     604.73(3)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
453 frames, ω rotation 0.8° per frame (34s per frame)
130 frames, ω rotation 0.8° per frame (34s per frame)
68 frames, ω rotation 0.8° per frame (34s per frame)
36 frames, ω rotation 0.8° per frame (34s per frame)
32 frames, ω rotation 0.8° per frame (34s 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  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5115
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    2.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepak (Otwinowski, Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             268
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2775
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0254
_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)+(0.0000P)²+0.7260P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0563
_reflns_number_gt                2631
_reflns_number_total             2775
_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 '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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               7104115
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
C1 C 1.1008(2) 0.3809(2) 0.7411(2) 0.0156(3) Uani 1 1 d . . .
C2 C 1.1856(3) 0.4615(3) 0.6399(3) 0.0264(4) Uani 1 1 d . . .
C3 C 1.2403(3) 0.4309(3) 0.9001(3) 0.0278(5) Uani 1 1 d . . .
C4 C 0.9557(3) 0.4517(2) 0.7638(3) 0.0214(4) Uani 1 1 d . . .
C5 C 0.7598(2) 0.0239(2) 0.2611(2) 0.0165(3) Uani 1 1 d . . .
H5 H 0.8334 0.0925 0.2229 0.020 Uiso 1 1 calc R . .
C6 C 0.5838(2) -0.0699(2) 0.1804(2) 0.0178(4) Uani 1 1 d . . .
H6 H 0.5173 -0.0783 0.0792 0.021 Uiso 1 1 calc R . .
C7 C 0.5221(2) -0.1505(2) 0.2777(2) 0.0164(3) Uani 1 1 d . . .
H7 H 0.4061 -0.2234 0.2552 0.020 Uiso 1 1 calc R . .
C8 C 0.6643(2) -0.1024(2) 0.4124(2) 0.0131(3) Uani 1 1 d . . .
C9 C 0.6768(2) -0.1329(2) 0.5563(2) 0.0126(3) Uani 1 1 d . . .
C10 C 0.5356(2) -0.2515(2) 0.5874(2) 0.0151(3) Uani 1 1 d . . .
H10A H 0.4859 -0.3645 0.5048 0.018 Uiso 1 1 calc R . .
H10B H 0.4397 -0.2065 0.5956 0.018 Uiso 1 1 calc R . .
C11 C 0.6372(2) -0.2577(2) 0.7448(2) 0.0191(4) Uani 1 1 d . . .
H11A H 0.5660 -0.2570 0.8143 0.023 Uiso 1 1 calc R . .
H11B H 0.6711 -0.3599 0.7297 0.023 Uiso 1 1 calc R . .
C12 C 0.8004(2) -0.0967(2) 0.8123(2) 0.0181(4) Uani 1 1 d . . .
H12A H 0.7833 -0.0054 0.8882 0.022 Uiso 1 1 calc R . .
H12B H 0.9057 -0.1187 0.8655 0.022 Uiso 1 1 calc R . .
N1 N 0.81440(19) 0.00490(18) 0.40368(17) 0.0142(3) Uani 1 1 d . . .
N2 N 0.82010(19) -0.04981(18) 0.67620(17) 0.0144(3) Uani 1 1 d . . .
Zn1 Zn 0.99511(3) 0.13174(2) 0.63455(2) 0.01422(7) Uani 1 1 d . . .
H2A H 1.224(3) 0.587(3) 0.685(3) 0.040(7) Uiso 1 1 d . . .
H2B H 1.106(3) 0.427(3) 0.532(3) 0.029(6) Uiso 1 1 d . . .
H2C H 1.290(3) 0.430(3) 0.633(3) 0.040(7) Uiso 1 1 d . . .
H3A H 1.288(3) 0.555(3) 0.951(3) 0.032(6) Uiso 1 1 d . . .
H3B H 1.338(3) 0.394(3) 0.893(3) 0.032(6) Uiso 1 1 d . . .
H3C H 1.190(3) 0.380(3) 0.968(3) 0.042(7) Uiso 1 1 d . . .
H4A H 1.002(3) 0.572(3) 0.809(3) 0.028(6) Uiso 1 1 d . . .
H4B H 0.903(3) 0.413(3) 0.836(3) 0.029(6) Uiso 1 1 d . . .
H4C H 0.864(3) 0.425(3) 0.666(3) 0.022(6) Uiso 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'
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
C3 C1 C2 108.46(17) . . ?
C3 C1 C4 108.71(16) . . ?
C2 C1 C4 108.36(15) . . ?
C3 C1 Zn1 112.24(13) . . ?
C2 C1 Zn1 109.88(13) . . ?
C4 C1 Zn1 109.11(12) . . ?
C1 C2 H2A 110.5(15) . . ?
C1 C2 H2B 113.3(14) . . ?
H2A C2 H2B 107(2) . . ?
C1 C2 H2C 111.0(15) . . ?
H2A C2 H2C 108(2) . . ?
H2B C2 H2C 107(2) . . ?
C1 C3 H3A 110.2(14) . . ?
C1 C3 H3B 112.8(15) . . ?
H3A C3 H3B 107(2) . . ?
C1 C3 H3C 110.3(16) . . ?
H3A C3 H3C 109(2) . . ?
H3B C3 H3C 107(2) . . ?
C1 C4 H4A 110.8(14) . . ?
C1 C4 H4B 112.5(14) . . ?
H4A C4 H4B 105.6(19) . . ?
C1 C4 H4C 112.3(13) . . ?
H4A C4 H4C 105.8(19) . . ?
H4B C4 H4C 109.5(19) . . ?
N1 C5 C6 111.26(15) . . ?
N1 C5 H5 124.4 . . ?
C6 C5 H5 124.4 . . ?
C5 C6 C7 106.66(16) . . ?
C5 C6 H6 126.7 . . ?
C7 C6 H6 126.7 . . ?
C8 C7 C6 106.36(15) . . ?
C8 C7 H7 126.8 . . ?
C6 C7 H7 126.8 . . ?
C7 C8 N1 110.82(15) . . ?
C7 C8 C9 131.29(16) . . ?
N1 C8 C9 117.68(15) . . ?
N2 C9 C8 119.38(15) . . ?
N2 C9 C10 114.25(15) . . ?
C8 C9 C10 126.35(15) . . ?
C9 C10 C11 101.95(14) . . ?
C9 C10 H10A 111.4 . . ?
C11 C10 H10A 111.4 . . ?
C9 C10 H10B 111.4 . . ?
C11 C10 H10B 111.4 . . ?
H10A C10 H10B 109.2 . . ?
C12 C11 C10 103.80(14) . . ?
C12 C11 H11A 111.0 . . ?
C10 C11 H11A 111.0 . . ?
C12 C11 H11B 111.0 . . ?
C10 C11 H11B 111.0 . . ?
H11A C11 H11B 109.0 . . ?
N2 C12 C11 105.19(14) . . ?
N2 C12 H12A 110.7 . . ?
C11 C12 H12A 110.7 . . ?
N2 C12 H12B 110.7 . . ?
C11 C12 H12B 110.7 . . ?
H12A C12 H12B 108.8 . . ?
C5 N1 C8 104.89(14) . . ?
C5 N1 Zn1 142.67(12) . . ?
C8 N1 Zn1 107.24(11) . . ?
C5 N1 Zn1 100.29(10) . 2_756 ?
C8 N1 Zn1 110.78(10) . 2_756 ?
Zn1 N1 Zn1 85.66(5) . 2_756 ?
C9 N2 C12 109.84(14) . . ?
C9 N2 Zn1 112.25(11) . . ?
C12 N2 Zn1 137.19(11) . . ?
C1 Zn1 N2 131.31(6) . . ?
C1 Zn1 N1 125.59(7) . . ?
N2 Zn1 N1 81.44(6) . . ?
C1 Zn1 N1 115.96(6) . 2_756 ?
N2 Zn1 N1 98.61(5) . 2_756 ?
N1 Zn1 N1 94.34(5) . 2_756 ?
C1 Zn1 Zn1 138.24(5) . 2_756 ?
N2 Zn1 Zn1 90.45(4) . 2_756 ?
N1 Zn1 Zn1 49.22(4) . 2_756 ?
N1 Zn1 Zn1 45.12(4) 2_756 2_756 ?
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 C3 1.525(3) . ?
C1 C2 1.530(3) . ?
C1 C4 1.531(2) . ?
C1 Zn1 1.9893(17) . ?
C2 H2A 1.00(3) . ?
C2 H2B 0.98(2) . ?
C2 H2C 1.00(3) . ?
C3 H3A 0.99(3) . ?
C3 H3B 0.96(2) . ?
C3 H3C 0.99(3) . ?
C4 H4A 0.95(2) . ?
C4 H4B 0.98(2) . ?
C4 H4C 0.97(2) . ?
C5 N1 1.376(2) . ?
C5 C6 1.384(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.412(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.383(2) . ?
C7 H7 0.9500 . ?
C8 N1 1.397(2) . ?
C8 C9 1.434(2) . ?
C9 N2 1.300(2) . ?
C9 C10 1.503(2) . ?
C10 C11 1.538(2) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.537(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N2 1.480(2) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
N1 Zn1 2.1192(15) . ?
N1 Zn1 2.2645(14) 2_756 ?
N2 Zn1 2.0580(14) . ?
Zn1 N1 2.2645(15) 2_756 ?
Zn1 Zn1 2.9822(4) 2_756 ?
