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#$Date: 2016-03-21 07:06:34 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178549 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/56/4065679.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_4065679
loop_
_publ_author_name
'Gutschank, Benjamin'
'Schulz, Stephan'
'Westphal, Ulrich'
'Bläser, Dieter'
'Boese, Roland'
_publ_contact_author
;
         Prof. Dr. Boese, Roland
         Fachbereich Chemie der
         Universität Duisburg-Essen
         Campus Essen Universitätsstr. 7
         D-45117 Essen, Germany
;
_publ_section_title
;
 Synthesis and X-ray Crystal Structures of Tetranuclear Zincamidinate
 Complexes
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2093
_journal_paper_doi               10.1021/om100065w
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C29 H56 N8 Cl4 Zn4, 3 C7 H8'
_chemical_formula_sum            'C49 H72 Cl4 N8 Zn4'
_chemical_formula_weight         1176.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   11.8438(6)
_cell_length_b                   11.8438(6)
_cell_length_c                   34.4247(19)
_cell_measurement_reflns_used    9846
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.31
_cell_volume                     4182.0(4)
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_collection       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_molecular_graphics    'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_refinement  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type
; 
 Bruker D8 KAPPA series II  with APEX II area detector system 
;
_diffrn_measurement_method
;
 Data collection strategy APEX 2 / COSMO
;
_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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            29037
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    1.931
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 BRUKER AXS SMART APEX 2 Vers. 3.0-2009
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1830
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.356
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.016(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         6257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0294
_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)+(0.0462P)²+0.6162P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0764
_reflns_number_gt                5898
_reflns_number_total             6257
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100065w_si_002.cif
_cod_data_source_block           comp_2
_cod_original_sg_symbol_H-M      P3(1)21
_cod_database_code               4065679
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'
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 0.98138(3) 0.02113(3) 0.211959(8) 0.01953(8) Uani 1 1 d .
Zn2 Zn 0.84616(3) 0.33080(3) 0.166874(8) 0.02158(8) Uani 1 1 d .
Cl1 Cl 0.94543(8) -0.13583(7) 0.25168(2) 0.03651(17) Uani 1 1 d .
Cl2 Cl 0.71004(8) 0.40272(8) 0.17105(2) 0.03972(18) Uani 1 1 d .
N1 N 0.9841(2) 0.1873(2) 0.23389(6) 0.0186(4) Uani 1 1 d .
N2 N 1.0028(2) 0.3905(2) 0.20759(6) 0.0199(4) Uani 1 1 d .
N3 N 0.7738(2) 0.1291(2) 0.16420(6) 0.0199(4) Uani 1 1 d .
N4 N 0.8635(2) -0.0200(2) 0.16096(6) 0.0180(4) Uani 1 1 d .
C1 C 0.9700(3) 0.1983(3) 0.27660(7) 0.0229(5) Uani 1 1 d .
H1 H 0.9883 0.2853 0.2823 0.027 Uiso 1 1 d R
C2 C 1.0689(3) 0.1741(3) 0.29797(8) 0.0364(7) Uani 1 1 d .
H2A H 1.0453 0.0826 0.2948 0.055 Uiso 1 1 d R
H2B H 1.0683 0.1933 0.3256 0.055 Uiso 1 1 d R
H2C H 1.1563 0.2307 0.2873 0.055 Uiso 1 1 d R
C3 C 0.8298(3) 0.1037(3) 0.28802(9) 0.0398(7) Uani 1 1 d .
H3A H 0.7716 0.1273 0.2745 0.060 Uiso 1 1 d R
H3B H 0.8193 0.1074 0.3162 0.060 Uiso 1 1 d R
H3C H 0.8078 0.0151 0.2806 0.060 Uiso 1 1 d R
C4 C 1.0163(3) 0.4660(3) 0.24389(7) 0.0266(6) Uani 1 1 d .
H4 H 0.9473 0.4090 0.2629 0.032 Uiso 1 1 d R
C5 C 0.9998(3) 0.5820(3) 0.23318(9) 0.0354(7) Uani 1 1 d .
H5A H 1.0698 0.6405 0.2155 0.053 Uiso 1 1 d R
H5B H 1.0025 0.6298 0.2567 0.053 Uiso 1 1 d R
H5C H 0.9153 0.5497 0.2203 0.053 Uiso 1 1 d R
C6 C 1.1496(3) 0.5134(3) 0.26158(8) 0.0311(6) Uani 1 1 d .
H6A H 1.1694 0.4424 0.2616 0.047 Uiso 1 1 d R
H6B H 1.1497 0.5418 0.2883 0.047 Uiso 1 1 d R
H6C H 1.2157 0.5868 0.2464 0.047 Uiso 1 1 d R
C7 C 0.6316(2) 0.0379(3) 0.16435(7) 0.0229(5) Uani 1 1 d .
H7 H 0.6159 -0.0486 0.1593 0.027 Uiso 1 1 d R
C8 C 0.5648(3) 0.0723(3) 0.13261(8) 0.0333(6) Uani 1 1 d .
H8A H 0.5783 0.1596 0.1379 0.050 Uiso 1 1 d R
H8B H 0.4711 0.0090 0.1324 0.050 Uiso 1 1 d R
H8C H 0.6025 0.0722 0.1073 0.050 Uiso 1 1 d R
C9 C 0.5789(3) 0.0388(4) 0.20456(9) 0.0391(8) Uani 1 1 d .
H9A H 0.6239 0.0158 0.2242 0.059 Uiso 1 1 d R
H9B H 0.4851 -0.0241 0.2055 0.059 Uiso 1 1 d R
H9C H 0.5938 0.1266 0.2098 0.059 Uiso 1 1 d R
C10 C 0.7479(3) -0.1497(3) 0.15307(8) 0.0258(6) Uani 1 1 d .
H10 H 0.6799 -0.1654 0.1712 0.031 Uiso 1 1 d R
C11 C 0.7878(3) -0.2532(2) 0.15855(9) 0.0335(6) Uani 1 1 d .
H11A H 0.8650 -0.2305 0.1426 0.050 Uiso 1 1 d R
H11B H 0.7160 -0.3384 0.1505 0.050 Uiso 1 1 d R
H11C H 0.8082 -0.2569 0.1860 0.050 Uiso 1 1 d R
C12 C 0.6987(3) -0.1558(3) 0.11190(8) 0.0316(6) Uani 1 1 d .
H12A H 0.6838 -0.0826 0.1075 0.047 Uiso 1 1 d R
H12B H 0.6168 -0.2382 0.1083 0.047 Uiso 1 1 d R
H12C H 0.7638 -0.1511 0.0934 0.047 Uiso 1 1 d R
C13 C 1.0000 0.2191(3) 0.1667 0.0146(6) Uani 1 2 d S
C14 C 0.9945(2) 0.2719(2) 0.20781(6) 0.0164(5) Uani 1 1 d .
C15 C 0.8618(2) 0.0939(2) 0.16380(6) 0.0164(5) Uani 1 1 d .
C21 C 1.1429(4) 0.5710(4) 0.37549(8) 0.0406(8) Uani 1 1 d .
C22 C 1.0629(4) 0.6108(4) 0.35799(9) 0.0464(9) Uani 1 1 d .
H22 H 1.0988 0.7013 0.3515 0.056 Uiso 1 1 d R
C23 C 0.9355(4) 0.5222(4) 0.34903(10) 0.0524(10) Uani 1 1 d .
H23 H 0.8816 0.5518 0.3371 0.063 Uiso 1 1 d R
C24 C 0.8842(4) 0.3918(4) 0.35700(11) 0.0564(10) Uani 1 1 d .
H24 H 0.7949 0.3300 0.3510 0.068 Uiso 1 1 d R
C25 C 0.9647(5) 0.3524(4) 0.37473(11) 0.0537(10) Uani 1 1 d .
H25 H 0.9313 0.2628 0.3805 0.064 Uiso 1 1 d R
C26 C 1.0896(4) 0.4397(4) 0.38386(10) 0.0443(8) Uani 1 1 d .
H26 H 1.1432 0.4101 0.3960 0.053 Uiso 1 1 d R
C27 C 1.2805(4) 0.6664(4) 0.38617(11) 0.0557(10) Uani 1 1 d .
H27A H 1.2878 0.6811 0.4143 0.084 Uiso 1 1 d R
H27B H 1.3072 0.7490 0.3727 0.084 Uiso 1 1 d R
H27C H 1.3371 0.6322 0.3782 0.084 Uiso 1 1 d R
C31 C 0.4027(6) 1.0419(6) 0.35178(17) 0.0352(13) Uiso 0.50 1 d P
C32 C 0.2833(5) 1.0000 0.3333 0.0549(13) Uiso 1 2 d S
C33 C 0.2525(10) 0.9107(10) 0.2993(3) 0.070(2) Uiso 0.50 1 d P
C34 C 0.3189(6) 0.8749(6) 0.28387(18) 0.0359(13) Uiso 0.50 1 d P
C35 C 0.4603(9) 0.9295(9) 0.3064(3) 0.063(2) Uiso 0.50 1 d P
C36 C 0.4853(5) 1.0000 0.3333 0.0559(14) Uiso 1 2 d S
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'
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
N1 Zn1 N4 97.48(8) . 6_765
N1 Zn1 N4 102.20(8) . .
N4 Zn1 N4 83.47(8) 6_765 .
N1 Zn1 Cl1 118.82(6) . .
N4 Zn1 Cl1 127.71(6) 6_765 .
N4 Zn1 Cl1 119.65(6) . .
N1 Zn1 C15 70.86(8) . .
N4 Zn1 C15 83.29(7) 6_765 .
N4 Zn1 C15 31.68(8) . .
Cl1 Zn1 C15 141.40(6) . .
N1 Zn1 Zn1 110.88(5) . 6_765
N4 Zn1 Zn1 42.75(6) 6_765 6_765
N4 Zn1 Zn1 41.85(5) . 6_765
Cl1 Zn1 Zn1 130.21(2) . 6_765
C15 Zn1 Zn1 54.74(5) . 6_765
N3 Zn2 N2 97.63(8) . 6_765
N3 Zn2 N2 101.41(8) . .
N2 Zn2 N2 82.98(8) 6_765 .
N3 Zn2 Cl2 119.24(6) . .
N2 Zn2 Cl2 126.58(6) 6_765 .
N2 Zn2 Cl2 121.14(6) . .
N3 Zn2 Zn2 110.72(6) . 6_765
N2 Zn2 Zn2 42.52(6) 6_765 6_765
N2 Zn2 Zn2 41.70(5) . 6_765
Cl2 Zn2 Zn2 130.02(2) . 6_765
C14 N1 C1 125.6(2) . .
C14 N1 Zn1 115.16(16) . .
C1 N1 Zn1 119.18(15) . .
C14 N2 C4 122.9(2) . .
C14 N2 Zn2 98.87(14) . 6_765
C4 N2 Zn2 115.81(17) . 6_765
C14 N2 Zn2 93.40(14) . .
C4 N2 Zn2 123.96(17) . .
Zn2 N2 Zn2 95.78(8) 6_765 .
C15 N3 C7 124.6(2) . .
C15 N3 Zn2 115.37(17) . .
C7 N3 Zn2 120.03(16) . .
C15 N4 C10 125.1(2) . .
C15 N4 Zn1 98.99(14) . 6_765
C10 N4 Zn1 115.32(16) . 6_765
C15 N4 Zn1 92.68(14) . .
C10 N4 Zn1 122.98(16) . .
Zn1 N4 Zn1 95.40(8) 6_765 .
N1 C1 C3 108.6(2) . .
N1 C1 C2 109.2(2) . .
C3 C1 C2 113.3(2) . .
N2 C4 C6 109.7(2) . .
N2 C4 C5 108.2(2) . .
C6 C4 C5 110.0(2) . .
N3 C7 C8 110.9(2) . .
N3 C7 C9 108.6(2) . .
C8 C7 C9 112.4(2) . .
N4 C10 C12 110.7(2) . .
N4 C10 C11 108.2(2) . .
C12 C10 C11 109.9(2) . .
C14 C13 C14 130.2(3) 6_765 .
C14 C13 C15 101.70(11) 6_765 6_765
C14 C13 C15 98.85(12) . 6_765
C14 C13 C15 98.85(12) 6_765 .
C14 C13 C15 101.71(11) . .
C15 C13 C15 129.9(3) 6_765 .
N1 C14 N2 136.8(2) . .
N1 C14 C13 108.8(2) . .
N2 C14 C13 114.4(2) . .
N3 C15 N4 136.8(2) . .
N3 C15 C13 108.7(2) . .
N4 C15 C13 114.5(2) . .
N3 C15 Zn1 139.27(16) . .
N4 C15 Zn1 55.64(12) . .
C13 C15 Zn1 77.79(13) . .
C26 C21 C22 117.8(4) . .
C26 C21 C27 120.7(3) . .
C22 C21 C27 121.5(4) . .
C23 C22 C21 120.9(4) . .
C24 C23 C22 120.8(4) . .
C23 C24 C25 118.1(4) . .
C26 C25 C24 121.1(4) . .
C25 C26 C21 121.3(3) . .
C33 C31 C34 54.1(6) 5_675 5_675
C33 C31 C32 69.1(6) 5_675 .
C34 C31 C32 123.1(6) 5_675 .
C33 C31 C35 127.1(8) 5_675 5_675
C34 C31 C35 73.2(6) 5_675 5_675
C32 C31 C35 163.1(6) . 5_675
C33 C31 C36 174.1(7) 5_675 .
C34 C31 C36 122.0(5) 5_675 .
C32 C31 C36 114.6(5) . .
C35 C31 C36 48.8(4) 5_675 .
C33 C31 C31 125.5(5) 5_675 5_675
C34 C31 C31 175.5(8) 5_675 5_675
C32 C31 C31 56.7(3) . 5_675
C35 C31 C31 106.7(4) 5_675 5_675
C36 C31 C31 58.0(3) . 5_675
C31 C32 C31 66.7(6) 5_675 .
C31 C32 C33 50.4(5) 5_675 .
C31 C32 C33 117.0(6) . .
C31 C32 C33 117.0(6) 5_675 5_675
C31 C32 C33 50.4(5) . 5_675
C33 C32 C33 167.4(9) . 5_675
C34 C33 C31 68.6(7) . 5_675
C34 C33 C32 129.1(9) . .
C31 C33 C32 60.5(6) 5_675 .
C33 C34 C31 57.4(6) . 5_675
C33 C34 C35 111.9(7) . .
C31 C34 C35 54.6(5) 5_675 .
C36 C35 C31 67.2(6) . 5_675
C36 C35 C34 119.4(8) . .
C31 C35 C34 52.2(5) 5_675 .
C35 C36 C35 168.2(11) . 5_675
C35 C36 C31 63.9(5) . 5_675
C35 C36 C31 127.8(7) 5_675 5_675
C35 C36 C31 127.8(7) . .
C35 C36 C31 63.9(5) 5_675 .
C31 C36 C31 64.0(6) 5_675 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N1 2.093(2) .
Zn1 N4 2.105(2) 6_765
Zn1 N4 2.142(2) .
Zn1 Cl1 2.1714(7) .
Zn1 C15 2.592(2) .
Zn1 Zn1 3.1416(6) 6_765
Zn2 N3 2.098(2) .
Zn2 N2 2.110(2) 6_765
Zn2 N2 2.144(2) .
Zn2 Cl2 2.1723(7) .
Zn2 Zn2 3.1559(6) 6_765
N1 C14 1.305(3) .
N1 C1 1.493(3) .
N2 C14 1.358(3) .
N2 C4 1.498(3) .
N2 Zn2 2.110(2) 6_765
N3 C15 1.302(3) .
N3 C7 1.477(3) .
N4 C15 1.363(3) .
N4 C10 1.484(3) .
N4 Zn1 2.105(2) 6_765
C1 C3 1.519(4) .
C1 C2 1.527(4) .
C4 C6 1.514(4) .
C4 C5 1.527(4) .
C7 C8 1.520(4) .
C7 C9 1.521(4) .
C10 C12 1.520(4) .
C10 C11 1.530(4) .
C13 C14 1.563(3) 6_765
C13 C14 1.563(3) .
C13 C15 1.569(3) 6_765
C13 C15 1.569(3) .
C21 C26 1.385(5) .
C21 C22 1.389(5) .
C21 C27 1.492(5) .
C22 C23 1.375(6) .
C23 C24 1.375(6) .
C24 C25 1.395(6) .
C25 C26 1.352(5) .
C31 C33 1.236(11) 5_675
C31 C34 1.366(9) 5_675
C31 C32 1.395(8) .
C31 C35 1.410(11) 5_675
C31 C36 1.447(8) .
C31 C31 1.534(12) 5_675
C32 C31 1.395(8) 5_675
C32 C33 1.498(10) .
C32 C33 1.498(10) 5_675
C33 C34 1.188(11) .
C33 C31 1.236(11) 5_675
C34 C31 1.366(9) 5_675
C34 C35 1.655(11) .
C35 C36 1.181(9) .
C35 C31 1.410(11) 5_675
C36 C35 1.181(9) 5_675
C36 C31 1.447(8) 5_675
