#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:49:54 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179209 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/40/4314000.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_4314000
loop_
_publ_author_name
'Srijit Das'
'Chen-Hsiung Hung'
'Sreebrata Goswami'
_publ_section_title
;
 Syntheses and Structures of Zwitterionic Indium(III) and Di-zinc
 Compounds of an Extended Nitrogenous Ligand. Examples of Unusually Long
 Wavelength Transitions in d10-Metal Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5153
_journal_page_last               5157
_journal_paper_doi               10.1021/ic030009c
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C32 H24 Cl2 N10 Zn2'
_chemical_formula_weight         750.26
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                   29.419(2)
_cell_length_b                   11.8121(8)
_cell_length_c                   17.7672(13)
_cell_measurement_temperature    293(2)
_cell_volume                     6174.1(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0657
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9574
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    1.769
_exptl_absorpt_correction_T_max  0.9486
_exptl_absorpt_correction_T_min  0.7250
_exptl_absorpt_correction_type   'Empirical Used SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cubic
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.71(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2872
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0749P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1193
_reflns_number_gt                2344
_reflns_number_total             2872
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030009c_2.cif
_cod_data_source_block           C32H24Cl2N10Zn2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        6174.0(8)
_cod_database_code               4314000
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'
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 0.480776(19) 0.82454(5) 0.12476(3) 0.02851(17) Uani 1 1 d . . .
Cl1 Cl 0.43382(5) 0.71055(13) 0.05735(9) 0.0393(4) Uani 1 1 d . . .
N1 N 0.51605(13) 0.6911(4) 0.1872(3) 0.0286(10) Uani 1 1 d . . .
N2 N 0.48830(14) 0.7877(4) 0.2950(3) 0.0288(10) Uani 1 1 d . . .
N3 N 0.47300(14) 0.8548(4) 0.2441(3) 0.0269(10) Uani 1 1 d . . .
N4 N 0.44615(15) 0.9792(4) 0.1312(3) 0.0326(10) Uani 1 1 d . . .
N5 N 0.53415(15) 0.8650(3) 0.0543(3) 0.0292(10) Uani 1 1 d . . .
C1 C 0.54030(18) 0.6063(5) 0.1565(4) 0.0358(13) Uani 1 1 d . . .
H1 H 0.5416 0.6002 0.1043 0.043 Uiso 1 1 calc R . .
C2 C 0.56324(19) 0.5283(5) 0.1997(4) 0.0407(15) Uani 1 1 d . . .
H2 H 0.5797 0.4701 0.1774 0.049 Uiso 1 1 calc R . .
C3 C 0.56129(19) 0.5387(5) 0.2775(4) 0.0425(16) Uani 1 1 d . . .
H3 H 0.5770 0.4880 0.3079 0.051 Uiso 1 1 calc R . .
C4 C 0.53618(19) 0.6235(5) 0.3093(4) 0.0372(13) Uani 1 1 d . . .
H4 H 0.5341 0.6302 0.3613 0.045 Uiso 1 1 calc R . .
C5 C 0.51368(17) 0.7004(5) 0.2620(4) 0.0300(12) Uani 1 1 d . . .
C6 C 0.44782(17) 0.9494(4) 0.2635(3) 0.0276(11) Uani 1 1 d . . .
C7 C 0.43711(18) 0.9827(5) 0.3382(3) 0.0323(12) Uani 1 1 d . . .
H7 H 0.4469 0.9394 0.3788 0.039 Uiso 1 1 calc R . .
C8 C 0.41245(19) 1.0784(5) 0.3498(4) 0.0366(14) Uani 1 1 d . . .
H8 H 0.4059 1.1022 0.3986 0.044 Uiso 1 1 calc R . .
C9 C 0.39674(18) 1.1417(5) 0.2874(4) 0.0342(13) Uani 1 1 d . . .
H9 H 0.3784 1.2045 0.2959 0.041 Uiso 1 1 calc R . .
C10 C 0.40762(17) 1.1138(4) 0.2151(3) 0.0289(12) Uani 1 1 d . . .
H10 H 0.3975 1.1584 0.1754 0.035 Uiso 1 1 calc R . .
C11 C 0.43462(16) 1.0159(4) 0.2006(3) 0.0262(11) Uani 1 1 d . . .
C12 C 0.43833(17) 1.0442(4) 0.0675(3) 0.0281(11) Uani 1 1 d . . .
C13 C 0.40531(18) 1.0133(5) 0.0155(4) 0.0340(13) Uani 1 1 d . . .
H13 H 0.3872 0.9502 0.0243 0.041 Uiso 1 1 calc R . .
C14 C 0.39946(18) 1.0762(5) -0.0491(4) 0.0349(13) Uani 1 1 d . . .
H14 H 0.3772 1.0562 -0.0837 0.042 Uiso 1 1 calc R . .
C15 C 0.53951(19) 0.8057(5) -0.0095(3) 0.0311(12) Uani 1 1 d . . .
H15 H 0.5200 0.7454 -0.0189 0.037 Uiso 1 1 calc R . .
C16 C 0.57304(18) 0.8305(5) -0.0621(4) 0.0328(12) Uani 1 1 d . . .
H16 H 0.5769 0.7859 -0.1047 0.039 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'
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'
Cl Cl 0.1484 0.1585 '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
N5 Zn1 N4 101.59(17) . . ?
N5 Zn1 N3 129.57(18) . . ?
N4 Zn1 N3 75.60(19) . . ?
N5 Zn1 N1 96.50(17) . . ?
N4 Zn1 N1 146.2(2) . . ?
N3 Zn1 N1 70.87(17) . . ?
N5 Zn1 Cl1 106.26(14) . . ?
N4 Zn1 Cl1 104.48(14) . . ?
N3 Zn1 Cl1 123.43(12) . . ?
N1 Zn1 Cl1 97.40(12) . . ?
C5 N1 C1 119.5(5) . . ?
C5 N1 Zn1 114.9(3) . . ?
C1 N1 Zn1 125.6(4) . . ?
N3 N2 C5 110.2(5) . . ?
N2 N3 C6 120.7(5) . . ?
N2 N3 Zn1 123.5(4) . . ?
C6 N3 Zn1 115.7(4) . . ?
C11 N4 C12 121.7(4) . . ?
C11 N4 Zn1 116.8(4) . . ?
C12 N4 Zn1 121.3(4) . . ?
C15 N5 C12 119.0(5) . 2_675 ?
C15 N5 Zn1 118.8(4) . . ?
C12 N5 Zn1 122.0(4) 2_675 . ?
N1 C1 C2 122.1(6) . . ?
C1 C2 C3 118.4(6) . . ?
C4 C3 C2 119.9(6) . . ?
C3 C4 C5 118.8(6) . . ?
N1 C5 N2 120.4(5) . . ?
N1 C5 C4 121.2(5) . . ?
N2 C5 C4 118.4(6) . . ?
N3 C6 C11 113.4(5) . . ?
N3 C6 C7 125.1(5) . . ?
C11 C6 C7 121.5(5) . . ?
C8 C7 C6 119.4(5) . . ?
C7 C8 C9 119.6(5) . . ?
C10 C9 C8 122.3(5) . . ?
C9 C10 C11 119.8(6) . . ?
N4 C11 C6 118.2(5) . . ?
N4 C11 C10 124.4(5) . . ?
C6 C11 C10 117.3(5) . . ?
N5 C12 N4 118.5(5) 2_675 . ?
N5 C12 C13 120.5(5) 2_675 . ?
N4 C12 C13 120.9(5) . . ?
C14 C13 C12 119.9(5) . . ?
C13 C14 C16 119.6(6) . 2_675 ?
N5 C15 C16 122.7(5) . . ?
C14 C16 C15 118.0(6) 2_675 . ?
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 N5 2.064(5) . ?
Zn1 N4 2.095(4) . ?
Zn1 N3 2.163(5) . ?
Zn1 N1 2.189(4) . ?
Zn1 Cl1 2.2706(16) . ?
N1 C5 1.335(8) . ?
N1 C1 1.345(7) . ?
N2 N3 1.284(7) . ?
N2 C5 1.402(7) . ?
N3 C6 1.385(7) . ?
N4 C11 1.351(7) . ?
N4 C12 1.387(7) . ?
N5 C15 1.342(7) . ?
N5 C12 1.364(7) 2_675 ?
C1 C2 1.376(9) . ?
C2 C3 1.388(10) . ?
C3 C4 1.367(9) . ?
C4 C5 1.403(8) . ?
C6 C11 1.420(8) . ?
C6 C7 1.419(8) . ?
C7 C8 1.359(8) . ?
C8 C9 1.416(9) . ?
C9 C10 1.364(8) . ?
C10 C11 1.426(7) . ?
C12 N5 1.364(7) 2_675 ?
C12 C13 1.389(8) . ?
C13 C14 1.377(9) . ?
C14 C16 1.387(8) 2_675 ?
C15 C16 1.390(8) . ?
C16 C14 1.387(8) 2_675 ?
