#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:50:34 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178584 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/95/4069592.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_4069592
loop_
_publ_author_name
'Fedushkin, Igor L.'
'Eremenko, Olga V.'
'Skatova, Alexandra A.'
'Piskunov, Alexander V.'
'Fukin, Georgi K.'
'Ketkov, Sergey Yu.'
'Irran, Elisabeth'
'Schumann, Herbert'
_publ_section_title
;
 Binuclear Zinc Complexes with Radical-Anionic Diimine Ligands
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3863
_journal_paper_doi               10.1021/om900291x
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C86 H98 N4 Zn2'
_chemical_formula_weight         1318.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.4886(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.2063(3)
_cell_length_b                   15.1241(3)
_cell_length_c                   15.2238(3)
_cell_measurement_reflns_used    9355
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.4252
_cell_measurement_theta_min      2.9207
_cell_volume                     3612.77(12)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S Sapphire'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_sigmaI/netI    0.0618
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33012
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         6356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0461
_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)+(0.0604P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1118
_reflns_number_gt                4484
_reflns_number_total             6356
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900291x_si_002.cif
_cod_data_source_block           fed46
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4069592
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Zn1 Zn 0.57167(2) -0.02984(2) 0.53616(2) 0.02512(12) Uani 1 1 d .
H1 H 0.5183(16) 0.0545(19) 0.5660(18) 0.030 Uiso 1 1 d .
N1 N 0.68501(14) -0.01159(15) 0.50998(16) 0.0217(5) Uani 1 1 d .
N2 N 0.62358(14) -0.13928(15) 0.60273(15) 0.0220(5) Uani 1 1 d .
C1 C 0.73163(17) -0.08284(19) 0.53605(18) 0.0210(6) Uani 1 1 d .
C2 C 0.81648(17) -0.1102(2) 0.52713(19) 0.0254(7) Uani 1 1 d .
C3 C 0.87630(18) -0.0760(2) 0.4869(2) 0.0329(8) Uani 1 1 d .
H3A H 0.8678 -0.0203 0.4570 0.039 Uiso 1 1 calc R
C4 C 0.95143(19) -0.1260(2) 0.4910(2) 0.0399(9) Uani 1 1 d .
H4A H 0.9931 -0.1030 0.4630 0.048 Uiso 1 1 calc R
C5 C 0.96594(19) -0.2063(2) 0.5338(2) 0.0395(9) Uani 1 1 d .
H5A H 1.0169 -0.2376 0.5346 0.047 Uiso 1 1 calc R
C6 C 0.90619(18) -0.2431(2) 0.5767(2) 0.0305(7) Uani 1 1 d .
C7 C 0.9123(2) -0.3230(2) 0.6259(2) 0.0396(9) Uani 1 1 d .
H7A H 0.9608 -0.3599 0.6313 0.048 Uiso 1 1 calc R
C8 C 0.8492(2) -0.3478(2) 0.6657(2) 0.0410(9) Uani 1 1 d .
H8A H 0.8557 -0.4011 0.6998 0.049 Uiso 1 1 calc R
C9 C 0.77458(19) -0.2973(2) 0.6582(2) 0.0343(8) Uani 1 1 d .
H9A H 0.7314 -0.3168 0.6858 0.041 Uiso 1 1 calc R
C10 C 0.76539(17) -0.21952(19) 0.61022(19) 0.0239(7) Uani 1 1 d .
C11 C 0.70012(17) -0.15005(19) 0.58590(18) 0.0212(6) Uani 1 1 d .
C12 C 0.83273(17) -0.1932(2) 0.57179(19) 0.0245(7) Uani 1 1 d .
C13 C 0.72302(16) 0.06546(19) 0.48076(19) 0.0213(6) Uani 1 1 d .
C14 C 0.78016(17) 0.11644(19) 0.5459(2) 0.0253(7) Uani 1 1 d .
C15 C 0.81458(18) 0.1916(2) 0.5165(2) 0.0299(7) Uani 1 1 d .
H15A H 0.8541 0.2266 0.5591 0.036 Uiso 1 1 calc R
C16 C 0.79225(19) 0.2163(2) 0.4265(2) 0.0335(8) Uani 1 1 d .
H16A H 0.8160 0.2682 0.4077 0.040 Uiso 1 1 calc R
C17 C 0.73555(18) 0.1658(2) 0.3636(2) 0.0285(7) Uani 1 1 d .
H17A H 0.7205 0.1837 0.3019 0.034 Uiso 1 1 calc R
C18 C 0.70020(17) 0.08944(19) 0.38903(19) 0.0237(7) Uani 1 1 d .
C19 C 0.80219(19) 0.0937(2) 0.6471(2) 0.0335(8) Uani 1 1 d .
H19A H 0.7806 0.0327 0.6533 0.040 Uiso 1 1 calc R
C20 C 0.7560(3) 0.1566(3) 0.6965(3) 0.0675(13) Uani 1 1 d .
H20A H 0.6946 0.1546 0.6681 0.101 Uiso 1 1 calc R
H20B H 0.7771 0.2169 0.6931 0.101 Uiso 1 1 calc R
H20C H 0.7664 0.1387 0.7602 0.101 Uiso 1 1 calc R
C21 C 0.8973(2) 0.0937(4) 0.6892(3) 0.0794(16) Uani 1 1 d .
H21A H 0.9251 0.0518 0.6568 0.119 Uiso 1 1 calc R
H21B H 0.9083 0.0763 0.7531 0.119 Uiso 1 1 calc R
H21C H 0.9201 0.1532 0.6851 0.119 Uiso 1 1 calc R
C22 C 0.64154(18) 0.0312(2) 0.31961(19) 0.0267(7) Uani 1 1 d .
H22A H 0.6022 0.0009 0.3511 0.032 Uiso 1 1 calc R
C23 C 0.6922(2) -0.0402(2) 0.2862(2) 0.0460(9) Uani 1 1 d .
H23A H 0.7264 -0.0730 0.3382 0.069 Uiso 1 1 calc R
H23B H 0.7300 -0.0128 0.2528 0.069 Uiso 1 1 calc R
H23C H 0.6530 -0.0808 0.2461 0.069 Uiso 1 1 calc R
C24 C 0.5870(2) 0.0819(3) 0.2407(2) 0.0488(10) Uani 1 1 d .
H24A H 0.5541 0.1269 0.2634 0.073 Uiso 1 1 calc R
H24B H 0.5480 0.0410 0.2006 0.073 Uiso 1 1 calc R
H24C H 0.6236 0.1105 0.2067 0.073 Uiso 1 1 calc R
C25 C 0.59588(17) -0.19641(19) 0.66475(19) 0.0229(7) Uani 1 1 d .
C26 C 0.62900(18) -0.1846(2) 0.7590(2) 0.0301(7) Uani 1 1 d .
C27 C 0.5964(2) -0.2376(2) 0.8174(2) 0.0358(8) Uani 1 1 d .
H27A H 0.6187 -0.2316 0.8811 0.043 Uiso 1 1 calc R
C28 C 0.5332(2) -0.2979(2) 0.7854(2) 0.0390(8) Uani 1 1 d .
H28A H 0.5106 -0.3316 0.8266 0.047 Uiso 1 1 calc R
C29 C 0.5023(2) -0.3096(2) 0.6932(2) 0.0351(8) Uani 1 1 d .
H29A H 0.4585 -0.3518 0.6715 0.042 Uiso 1 1 calc R
C30 C 0.53407(18) -0.26065(19) 0.6312(2) 0.0259(7) Uani 1 1 d .
C31 C 0.6958(2) -0.1141(2) 0.7962(2) 0.0399(9) Uani 1 1 d .
H31A H 0.7283 -0.1036 0.7493 0.048 Uiso 1 1 calc R
C32 C 0.7604(2) -0.1448(3) 0.8835(3) 0.0648(12) Uani 1 1 d .
H32A H 0.8024 -0.0980 0.9049 0.097 Uiso 1 1 calc R
H32B H 0.7895 -0.1983 0.8707 0.097 Uiso 1 1 calc R
H32C H 0.7303 -0.1577 0.9304 0.097 Uiso 1 1 calc R
C33 C 0.6538(2) -0.0279(2) 0.8100(3) 0.0522(10) Uani 1 1 d .
H33A H 0.6145 -0.0098 0.7528 0.078 Uiso 1 1 calc R
H33B H 0.6976 0.0177 0.8296 0.078 Uiso 1 1 calc R
H33C H 0.6222 -0.0356 0.8565 0.078 Uiso 1 1 calc R
C34 C 0.50462(19) -0.2806(2) 0.5309(2) 0.0310(7) Uani 1 1 d .
H34A H 0.5340 -0.2382 0.4984 0.037 Uiso 1 1 calc R
C35 C 0.4099(2) -0.2681(3) 0.4942(3) 0.0660(13) Uani 1 1 d .
H35A H 0.3942 -0.2078 0.5071 0.099 Uiso 1 1 calc R
H35B H 0.3793 -0.3105 0.5231 0.099 Uiso 1 1 calc R
H35C H 0.3946 -0.2779 0.4284 0.099 Uiso 1 1 calc R
C36 C 0.5314(3) -0.3736(2) 0.5115(3) 0.0557(11) Uani 1 1 d .
H36A H 0.5930 -0.3802 0.5357 0.084 Uiso 1 1 calc R
H36B H 0.5166 -0.3838 0.4458 0.084 Uiso 1 1 calc R
H36C H 0.5016 -0.4168 0.5405 0.084 Uiso 1 1 calc R
C37 C 0.1501(4) -0.0787(3) 0.8984(4) 0.0798(16) Uani 1 1 d .
C38 C 0.1197(4) -0.1019(3) 0.8113(3) 0.0716(13) Uani 1 1 d .
H38A H 0.1591 -0.1033 0.7745 0.086 Uiso 1 1 calc R
C39 C 0.0386(5) -0.1234(4) 0.7713(5) 0.128(3) Uani 1 1 d .
H39A H 0.0224 -0.1388 0.7089 0.154 Uiso 1 1 calc R
C40 C -0.0190(5) -0.1227(4) 0.8209(5) 0.127(3) Uani 1 1 d .
H40A H -0.0767 -0.1384 0.7945 0.153 Uiso 1 1 calc R
C41 C 0.0077(4) -0.0983(4) 0.9136(5) 0.102(2) Uani 1 1 d .
H41A H -0.0337 -0.0966 0.9481 0.122 Uiso 1 1 calc R
C42 C 0.0882(4) -0.0775(3) 0.9549(4) 0.0814(16) Uani 1 1 d .
H42 H 0.1048 -0.0626 1.0175 0.098 Uiso 1 1 calc R
C43 C 0.2316(4) -0.0561(4) 0.9457(4) 0.120(2) Uani 1 1 d .
H43A H 0.2695 -0.0572 0.9046 0.181 Uiso 1 1 calc R
H43B H 0.2520 -0.0984 0.9951 0.181 Uiso 1 1 calc R
H43C H 0.2311 0.0035 0.9710 0.181 Uiso 1 1 calc R
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'
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_3
N1 Zn1 N2 85.67(9) .
N1 Zn1 Zn1 131.97(7) 3_656
N2 Zn1 Zn1 138.65(7) 3_656
C1 N1 C13 119.8(2) .
C1 N1 Zn1 108.29(18) .
C13 N1 Zn1 131.35(18) .
C11 N2 C25 120.7(2) .
C11 N2 Zn1 107.13(18) .
C25 N2 Zn1 131.90(18) .
N1 C1 C11 119.0(2) .
N1 C1 C2 132.8(3) .
C11 C1 C2 108.2(2) .
C3 C2 C12 118.7(3) .
C3 C2 C1 135.6(3) .
C12 C2 C1 105.6(2) .
C2 C3 C4 118.2(3) .
C5 C4 C3 122.4(3) .
C4 C5 C6 120.9(3) .
C12 C6 C5 115.9(3) .
C12 C6 C7 115.9(3) .
C5 C6 C7 128.1(3) .
C8 C7 C6 120.6(3) .
C7 C8 C9 122.5(3) .
C10 C9 C8 119.0(3) .
C9 C10 C12 117.9(3) .
C9 C10 C11 136.2(3) .
C12 C10 C11 105.9(2) .
N2 C11 C1 119.0(2) .
N2 C11 C10 133.0(3) .
C1 C11 C10 108.1(2) .
C6 C12 C10 124.1(3) .
C6 C12 C2 123.9(3) .
C10 C12 C2 112.1(2) .
C18 C13 C14 121.6(3) .
C18 C13 N1 119.4(2) .
C14 C13 N1 118.9(3) .
C15 C14 C13 117.9(3) .
C15 C14 C19 119.8(3) .
C13 C14 C19 122.2(3) .
C16 C15 C14 121.0(3) .
C15 C16 C17 120.3(3) .
C16 C17 C18 121.1(3) .
C17 C18 C13 118.0(3) .
C17 C18 C22 121.4(3) .
C13 C18 C22 120.6(3) .
C21 C19 C20 111.4(3) .
C21 C19 C14 112.5(3) .
C20 C19 C14 109.8(3) .
C24 C22 C18 113.6(3) .
C24 C22 C23 110.6(3) .
C18 C22 C23 110.5(2) .
C30 C25 C26 121.0(3) .
C30 C25 N2 119.5(2) .
C26 C25 N2 119.4(3) .
C27 C26 C25 117.8(3) .
C27 C26 C31 120.8(3) .
C25 C26 C31 121.3(3) .
C28 C27 C26 121.7(3) .
C27 C28 C29 119.8(3) .
C28 C29 C30 121.3(3) .
C29 C30 C25 118.3(3) .
C29 C30 C34 120.1(3) .
C25 C30 C34 121.6(3) .
C33 C31 C26 110.6(3) .
C33 C31 C32 111.8(3) .
C26 C31 C32 112.0(3) .
C35 C34 C30 112.6(3) .
C35 C34 C36 110.9(3) .
C30 C34 C36 110.3(3) .
C38 C37 C43 130.5(6) .
C38 C37 C42 116.4(5) .
C43 C37 C42 113.2(6) .
C37 C38 C39 126.1(6) .
C40 C39 C38 118.9(7) .
C39 C40 C41 118.7(8) .
C42 C41 C40 123.3(6) .
C41 C42 C37 116.7(6) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N1 1.994(2) .
Zn1 N2 2.012(2) .
Zn1 Zn1 2.4785(6) 3_656
N1 C1 1.319(4) .
N1 C13 1.440(4) .
N2 C11 1.338(3) .
N2 C25 1.432(3) .
C1 C11 1.437(4) .
C1 C2 1.474(4) .
C2 C3 1.371(4) .
C2 C12 1.420(4) .
C3 C4 1.422(4) .
C4 C5 1.370(5) .
C5 C6 1.411(4) .
C6 C12 1.395(4) .
C6 C7 1.412(4) .
C7 C8 1.366(5) .
C8 C9 1.410(4) .
C9 C10 1.372(4) .
C10 C12 1.418(4) .
C10 C11 1.471(4) .
C13 C18 1.400(4) .
C13 C14 1.406(4) .
C14 C15 1.389(4) .
C14 C19 1.530(4) .
C15 C16 1.377(4) .
C16 C17 1.379(4) .
C17 C18 1.387(4) .
C18 C22 1.515(4) .
C19 C21 1.515(5) .
C19 C20 1.521(5) .
C22 C24 1.510(4) .
C22 C23 1.519(4) .
C25 C30 1.397(4) .
C25 C26 1.412(4) .
C26 C27 1.395(4) .
C26 C31 1.524(4) .
C27 C28 1.367(5) .
C28 C29 1.379(4) .
C29 C30 1.395(4) .
C30 C34 1.513(4) .
C31 C33 1.510(5) .
C31 C32 1.544(5) .
C34 C35 1.509(4) .
C34 C36 1.523(4) .
C37 C38 1.340(6) .
C37 C43 1.380(7) .
C37 C42 1.477(7) .
C38 C39 1.342(7) .
C39 C40 1.340(9) .
C40 C41 1.418(8) .
C41 C42 1.336(7) .
