#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:48:41 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179264 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/84/4318428.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_4318428
loop_
_publ_author_name
'Maria Alexiou'
'Catherine Dendrinou-Samara'
'Catherine P. Raptopoulou'
'Aris Terzis'
'Dimitris P. Kessissoglou'
_publ_section_title
;
 From Monomer Zinc-Oxamato Complexes to Tetranuclear Inverse 12-Membered
 and Octanuclear 12-Membered Metallacrowns
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4732
_journal_page_last               4738
_journal_paper_doi               10.1021/ic0200904
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C11 H9 Cl2 N3 O Zn'
_chemical_formula_weight         335.48
_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
_cell_angle_alpha                88.55(3)
_cell_angle_beta                 82.75(4)
_cell_angle_gamma                89.78(4)
_cell_formula_units_Z            4
_cell_length_a                   7.295(9)
_cell_length_b                   12.71(1)
_cell_length_c                   14.20(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.7
_cell_measurement_theta_min      5.3
_cell_volume                     1306(2)
_computing_cell_refinement
'Program LEAST (UCLA Crystallographic package, C.E.Strouse 1994)'
_computing_data_collection
'Program COLLECT (UCLA Crystallographic package, C.E.Strouse 1994)'
_computing_data_reduction
'Program REDUCE (UCLA Crystallographic package, C.E.Strouse 1994)'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'Crystal Logic Dual Goniometer'
_diffrn_measurement_method       'theta-2theta 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  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0555
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3155
_diffrn_reflns_theta_max         21.50
_diffrn_reflns_theta_min         1.45
_diffrn_standards_decay_%        -2.9
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.280
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_meas      1.68
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.221
_refine_diff_density_min         -1.630
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.106
_refine_ls_goodness_of_fit_obs   1.144
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         3002
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_restrained_S_obs      1.144
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_obs          0.0986
_refine_ls_shift/esd_max         0.009
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1831P)²+8.3361P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2808
_refine_ls_wR_factor_obs         0.2621
_reflns_number_observed          2483
_reflns_number_total             3002
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0200904_1.cif
_cod_data_source_block           shel93
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1831P)^2^+8.3361P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1831P)^2^+8.3361P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1305(3)
_cod_database_code               4318428
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Zn1 Zn 0.2437(2) 0.14264(12) 0.28470(10) 0.0492(6) Uani 1 d . .
Cl1 Cl 0.1101(5) 0.0383(3) 0.1907(2) 0.0632(10) Uani 1 d . .
Cl2 Cl 0.5147(5) 0.2100(4) 0.2292(3) 0.0821(13) Uani 1 d . .
N1 N 0.2497(13) 0.0679(8) 0.4138(8) 0.049(3) Uani 1 d . .
N3 N 0.0690(14) 0.2569(8) 0.3439(7) 0.048(3) Uani 1 d . .
C1 C 0.2578(18) -0.0357(13) 0.4207(12) 0.064(4) Uani 1 d . .
H1 H 0.2618(18) -0.0752(13) 0.3662(12) 0.071(23) Uiso 1 calc R .
C2 C 0.2607(19) -0.0877(13) 0.5100(15) 0.077(5) Uani 1 d . .
H2 H 0.2674(19) -0.1607(13) 0.5139(15) 0.071(23) Uiso 1 calc R .
C3 C 0.2536(20) -0.0300(15) 0.5906(12) 0.073(4) Uani 1 d . .
H3 H 0.2530(20) -0.0626(15) 0.6500(12) 0.071(23) Uiso 1 calc R .
C4 C 0.2475(19) 0.0750(14) 0.5809(11) 0.067(4) Uani 1 d . .
H4 H 0.2419(19) 0.1156(14) 0.6348(11) 0.071(23) Uiso 1 calc R .
C5 C 0.2492(15) 0.1250(11) 0.4926(9) 0.049(3) Uani 1 d . .
C6 C 0.2327(17) 0.2403(12) 0.4807(10) 0.059(4) Uani 1 d . .
N2 N 0.3399(20) 0.3369(20) 0.5213(9) 0.127(9) Uani 1 d . .
O1 O 0.4341(27) 0.2763(10) 0.5576(11) 0.131(7) Uani 1 d . .
C7 C 0.0938(17) 0.2894(10) 0.4319(9) 0.048(3) Uani 1 d . .
C8 C -0.0292(22) 0.3664(11) 0.4765(11) 0.066(4) Uani 1 d . .
H8 H -0.0173(22) 0.3874(11) 0.5377(11) 0.049(17) Uiso 1 calc R .
C9 C -0.1635(22) 0.4085(12) 0.4293(11) 0.066(4) Uani 1 d . .
H9 H -0.2403(22) 0.4607(12) 0.4571(11) 0.049(17) Uiso 1 calc R .
C10 C -0.1866(23) 0.3742(12) 0.3397(11) 0.070(4) Uani 1 d . .
H10 H -0.2794(23) 0.4016(12) 0.3070(11) 0.049(17) Uiso 1 calc R .
C11 C -0.0655(19) 0.2969(12) 0.3002(11) 0.063(4) Uani 1 d . .
H11 H -0.0806(19) 0.2726(12) 0.2404(11) 0.049(17) Uiso 1 calc R .
Zn2 Zn 0.2446(2) -0.36108(12) 0.22025(10) 0.0493(6) Uani 1 d . .
Cl3 Cl 0.3888(5) -0.4581(3) 0.3200(3) 0.0638(10) Uani 1 d . .
Cl4 Cl -0.0346(6) -0.3037(4) 0.2693(3) 0.0848(13) Uani 1 d . .
N11 N 0.2482(13) -0.4391(8) 0.0951(7) 0.045(2) Uani 1 d . .
N13 N 0.4108(14) -0.2459(9) 0.1536(8) 0.052(3) Uani 1 d . .
C21 C 0.2490(18) -0.5470(11) 0.0948(12) 0.063(4) Uani 1 d . .
H21 H 0.2545(18) -0.5841(11) 0.1517(12) 0.066(22) Uiso 1 calc R .
C22 C 0.2420(21) -0.6016(14) 0.0140(14) 0.075(5) Uani 1 d . .
H22 H 0.2374(21) -0.6747(14) 0.0160(14) 0.066(22) Uiso 1 calc R .
C23 C 0.2419(20) -0.5470(16) -0.0695(15) 0.088(6) Uani 1 d . .
H23 H 0.2383(20) -0.5829(16) -0.1255(15) 0.066(22) Uiso 1 calc R .
C24 C 0.2472(18) -0.4378(13) -0.0715(11) 0.066(4) Uani 1 d . .
H24 H 0.2511(18) -0.3995(13) -0.1284(11) 0.066(22) Uiso 1 calc R .
C25 C 0.2463(17) -0.3878(12) 0.0136(11) 0.058(4) Uani 1 d . .
C26 C 0.2533(16) -0.2704(11) 0.0167(9) 0.050(3) Uani 1 d . .
N12 N 0.1216(23) -0.2315(10) -0.0376(11) 0.094(6) Uani 1 d . .
O11 O 0.1350(16) -0.1283(11) -0.0364(9) 0.095(4) Uani 1 d . .
C27 C 0.3909(17) -0.2151(9) 0.0636(9) 0.045(3) Uani 1 d . .
C28 C 0.5064(18) -0.1422(10) 0.0163(9) 0.049(3) Uani 1 d . .
H28 H 0.4895(18) -0.1220(10) -0.0454(9) 0.085(25) Uiso 1 calc R .
C29 C 0.6468(19) -0.0979(10) 0.0571(10) 0.055(3) Uani 1 d . .
H29 H 0.7267(19) -0.0495(10) 0.0234(10) 0.085(25) Uiso 1 calc R .
C30 C 0.6667(20) -0.1266(11) 0.1488(11) 0.066(4) Uani 1 d . .
H30 H 0.7585(20) -0.0967(11) 0.1794(11) 0.085(25) Uiso 1 calc R .
C31 C 0.5453(21) -0.2025(11) 0.1960(10) 0.062(4) Uani 1 d . .
H31 H 0.5588(21) -0.2230(11) 0.2581(10) 0.085(25) Uiso 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'
O O 0.0106 0.0060 '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
_geom_angle_publ_flag
N1 Zn1 N3 91.8(4) . . ?
N1 Zn1 Cl2 111.7(3) . . ?
N3 Zn1 Cl2 110.8(3) . . ?
N1 Zn1 Cl1 109.1(3) . . ?
N3 Zn1 Cl1 112.9(3) . . ?
Cl2 Zn1 Cl1 117.6(2) . . ?
C1 N1 C5 119.4(12) . . ?
C1 N1 Zn1 120.8(10) . . ?
C5 N1 Zn1 119.8(9) . . ?
C11 N3 C7 120.2(11) . . ?
C11 N3 Zn1 122.2(8) . . ?
C7 N3 Zn1 117.5(8) . . ?
N1 C1 C2 120.9(15) . . ?
C3 C2 C1 119.8(15) . . ?
C4 C3 C2 117.7(16) . . ?
C3 C4 C5 121.9(15) . . ?
N1 C5 C4 120.2(13) . . ?
N1 C5 C6 116.8(12) . . ?
C4 C5 C6 122.8(13) . . ?
C7 C6 C5 123.0(10) . . ?
C7 C6 N2 104.6(12) . . ?
C5 C6 N2 132.2(12) . . ?
O1 N2 C6 89.8(20) . . ?
N3 C7 C8 119.0(12) . . ?
N3 C7 C6 119.4(11) . . ?
C8 C7 C6 121.3(12) . . ?
C9 C8 C7 119.7(14) . . ?
C8 C9 C10 120.3(14) . . ?
C9 C10 C11 117.7(15) . . ?
N3 C11 C10 123.0(14) . . ?
N13 Zn2 N11 90.8(4) . . ?
N13 Zn2 Cl4 112.4(3) . . ?
N11 Zn2 Cl4 110.8(3) . . ?
N13 Zn2 Cl3 112.0(3) . . ?
N11 Zn2 Cl3 109.0(3) . . ?
Cl4 Zn2 Cl3 118.3(2) . . ?
C25 N11 C21 118.1(12) . . ?
C25 N11 Zn2 121.4(9) . . ?
C21 N11 Zn2 120.5(9) . . ?
C31 N13 C27 118.9(11) . . ?
C31 N13 Zn2 121.2(9) . . ?
C27 N13 Zn2 119.8(8) . . ?
C22 C21 N11 122.2(16) . . ?
C23 C22 C21 118.6(16) . . ?
C22 C23 C24 120.2(15) . . ?
C25 C24 C23 117.9(17) . . ?
N11 C25 C24 122.9(14) . . ?
N11 C25 C26 116.3(11) . . ?
C24 C25 C26 120.8(15) . . ?
N12 C26 C27 130.3(13) . . ?
N12 C26 C25 107.1(11) . . ?
C27 C26 C25 122.4(10) . . ?
O11 N12 C26 105.9(15) . . ?
N13 C27 C28 120.7(12) . . ?
N13 C27 C26 117.3(11) . . ?
C28 C27 C26 121.7(11) . . ?
C27 C28 C29 121.7(12) . . ?
C28 C29 C30 118.3(12) . . ?
C29 C30 C31 118.6(13) . . ?
N13 C31 C30 121.6(14) . . ?
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 N1 2.048(11) . ?
Zn1 N3 2.053(10) . ?
Zn1 Cl2 2.201(4) . ?
Zn1 Cl1 2.219(4) . ?
N1 C1 1.32(2) . ?
N1 C5 1.35(2) . ?
N3 C11 1.32(2) . ?
N3 C7 1.36(2) . ?
C1 C2 1.42(2) . ?
C2 C3 1.37(2) . ?
C3 C4 1.34(2) . ?
C4 C5 1.39(2) . ?
C5 C6 1.48(2) . ?
C6 C7 1.43(2) . ?
C6 N2 1.61(3) . ?
N2 O1 1.18(2) . ?
C7 C8 1.43(2) . ?
C8 C9 1.36(2) . ?
C9 C10 1.38(2) . ?
C10 C11 1.40(2) . ?
Zn2 N13 2.041(11) . ?
Zn2 N11 2.053(10) . ?
Zn2 Cl4 2.196(5) . ?
Zn2 Cl3 2.216(4) . ?
N11 C25 1.31(2) . ?
N11 C21 1.37(2) . ?
N13 C31 1.34(2) . ?
N13 C27 1.35(2) . ?
C21 C22 1.36(2) . ?
C22 C23 1.36(3) . ?
C23 C24 1.39(2) . ?
C24 C25 1.38(2) . ?
C25 C26 1.49(2) . ?
C26 N12 1.39(2) . ?
C26 C27 1.46(2) . ?
N12 O11 1.32(2) . ?
C27 C28 1.36(2) . ?
C28 C29 1.37(2) . ?
C29 C30 1.37(2) . ?
C30 C31 1.41(2) . ?
