#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:48:41 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179264 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/84/4318429.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_4318429
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            'C49.6 H45.4 Cl2 N13.4 O8.8 Zn4'
_chemical_formula_weight         1302.38
_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           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 91.62(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.826(5)
_cell_length_b                   17.739(6)
_cell_length_c                   15.680(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.7
_cell_measurement_theta_min      5.3
_cell_volume                     3288(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_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0159
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4677
_diffrn_reflns_theta_max         60.02
_diffrn_reflns_theta_min         4.49
_diffrn_standards_decay_%        -3.2
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.866
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_meas      1.28
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             1322.4
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.985
_refine_ls_goodness_of_fit_obs   0.973
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         4504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_restrained_S_obs      0.973
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_obs          0.0511
_refine_ls_shift/esd_max         2.971
_refine_ls_shift/esd_mean        0.060
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0994P)²+5.9390P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1570
_refine_ls_wR_factor_obs         0.1440
_reflns_number_observed          3932
_reflns_number_total             4504
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0200904_2.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^)+(0.0994P)^2^+5.9390P] 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^)+(0.0994P)^2^+5.9390P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4318429
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Zn1 Zn 0.87488(5) 0.63253(3) 0.05335(3) 0.0434(2) Uani 1 d . .
Zn2 Zn 1.07166(5) 0.55138(3) -0.06420(3) 0.0406(2) Uani 1 d . .
O1 O 0.8804(3) 0.5936(2) 0.1701(2) 0.0555(8) Uani 1 d . .
Cl Cl 0.72871(13) 0.70740(8) 0.02815(12) 0.0855(5) Uani 1 d . .
O2 O 0.9059(5) 0.5433(3) -0.0162(4) 0.0443(12) Uani 1 d . .
O21 O 1.0180(3) 0.6885(2) 0.0496(2) 0.0524(8) Uani 1 d . .
N1 N 0.9932(3) 0.3816(2) 0.1705(2) 0.0456(9) Uani 1 d . .
N3 N 0.9234(3) 0.5230(2) 0.1725(2) 0.0438(8) Uani 1 d . .
N21 N 1.2537(3) 0.5717(2) -0.0680(2) 0.0481(9) Uani 1 d . .
N23 N 1.1018(3) 0.6474(2) 0.0154(2) 0.0444(8) Uani 1 d . .
N2 N 1.0755(6) 0.5699(4) 0.3424(4) 0.104(2) Uani 1 d . .
C1 C 1.0272(5) 0.3099(3) 0.1685(3) 0.0567(12) Uani 1 d . .
C2 C 1.0698(5) 0.2722(3) 0.2387(3) 0.0662(14) Uani 1 d . .
C3 C 1.0787(5) 0.3106(3) 0.3145(3) 0.0693(15) Uani 1 d . .
C4 C 1.0454(5) 0.3845(3) 0.3187(3) 0.0593(13) Uani 1 d . .
C5 C 1.0022(4) 0.4196(2) 0.2451(3) 0.0445(10) Uani 1 d . .
C6 C 0.9625(4) 0.4983(2) 0.2444(3) 0.0468(10) Uani 1 d . .
C7 C 0.9722(5) 0.5457(3) 0.3217(3) 0.0574(13) Uani 1 d . .
C8 C 0.8837(8) 0.5659(5) 0.3664(4) 0.095(2) Uani 1 d . .
C9 C 0.8985(12) 0.6157(5) 0.4379(5) 0.109(3) Uani 1 d . .
C10 C 1.0021(12) 0.6387(4) 0.4566(5) 0.107(3) Uani 1 d . .
C11 C 1.0891(11) 0.6184(5) 0.4091(6) 0.123(3) Uani 1 d . .
H11 H 1.1605(11) 0.6379(5) 0.4218(6) 3.267(731) Uiso 1 calc R .
N22 N 1.2863(5) 0.7932(3) 0.0487(4) 0.096(2) Uani 1 d . .
C21 C 1.3292(4) 0.5299(3) -0.1090(3) 0.0580(12) Uani 1 d . .
C22 C 1.4441(5) 0.5419(4) -0.1005(4) 0.071(2) Uani 1 d . .
C23 C 1.4842(5) 0.5971(4) -0.0482(4) 0.0712(15) Uani 1 d . .
C24 C 1.4075(4) 0.6404(3) -0.0041(4) 0.0649(14) Uani 1 d . .
C25 C 1.2919(4) 0.6266(2) -0.0148(3) 0.0496(11) Uani 1 d . .
C26 C 1.2047(4) 0.6699(3) 0.0286(3) 0.0492(11) Uani 1 d . .
C27 C 1.2336(4) 0.7353(3) 0.0850(4) 0.0662(14) Uani 1 d . .
C28 C 1.2071(6) 0.7339(5) 0.1697(4) 0.094(2) Uani 1 d . .
H28 H 1.1691(6) 0.6934(5) 0.1934(4) 0.104(27) Uiso 1 calc R .
C29 C 1.2407(7) 0.7974(7) 0.2190(6) 0.131(4) Uani 1 d . .
H29 H 1.2280(7) 0.7977(7) 0.2773(6) 0.187(46) Uiso 1 calc R .
C30 C 1.2907(8) 0.8575(6) 0.1832(9) 0.131(4) Uani 1 d . .
C31 C 1.3129(9) 0.8524(5) 0.0989(9) 0.131(4) Uani 1 d . .
H31 H 1.3493(9) 0.8930(5) 0.0741(9) 0.339(126) Uiso 1 calc R .
OS O 0.2608(5) 0.0231(5) 0.6435(4) 0.112(3) Uani 0.70 d P .
NS N 0.3227(8) 0.0524(10) 0.7741(7) 0.153(6) Uani 0.70 d P .
C1S C 0.2714(14) 0.0242(9) 0.7090(13) 0.138(5) Uiso 0.70 d P .
C2S C 0.3341(20) 0.0401(12) 0.8622(16) 0.196(8) Uiso 0.70 d P .
C3S C 0.3660(24) 0.1267(15) 0.7553(17) 0.212(10) Uiso 0.70 d P .
OM1 O 0.4492(19) 0.1471(12) 0.1676(14) 0.170(7) Uiso 0.40 d P .
CM1 C 0.5179(29) 0.2044(19) 0.1271(20) 0.165(11) Uiso 0.40 d P .
OM2 O 0.4008(18) 0.0362(11) 0.1888(14) 0.123(6) Uiso 0.30 d P .
CM2 C 0.4026(31) 0.0342(19) 0.0877(25) 0.136(11) Uiso 0.30 d P .
H1 H 1.0178(39) 0.2867(26) 0.1162(31) 0.049(13) Uiso 1 d . .
H2 H 1.0934(48) 0.2216(35) 0.2378(35) 0.074(17) Uiso 1 d . .
H3 H 1.1122(49) 0.2849(32) 0.3636(37) 0.075(16) Uiso 1 d . .
H4 H 1.0475(43) 0.4136(29) 0.3712(33) 0.060(14) Uiso 1 d . .
H8 H 0.8146(43) 0.5493(26) 0.3429(32) 0.046(13) Uiso 1 d . .
H9 H 0.8038(111) 0.6351(63) 0.4330(74) 0.191(47) Uiso 1 d . .
H10 H 1.0069(87) 0.6683(54) 0.5020(68) 0.160(35) Uiso 1 d . .
HO2 H 0.8671(65) 0.5295(41) -0.0635(54) 0.101(24) Uiso 1 d . .
H21 H 1.2982(39) 0.4827(28) -0.1456(30) 0.052(12) Uiso 1 d . .
H22 H 1.4898(51) 0.5118(34) -0.1320(36) 0.072(17) Uiso 1 d . .
H23 H 1.5780(55) 0.6052(34) -0.0476(36) 0.084(18) Uiso 1 d . .
H24 H 1.4339(49) 0.6807(35) 0.0415(38) 0.081(17) Uiso 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 '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
O1 Zn1 O2 103.5(2) . . ?
O1 Zn1 O21 101.58(14) . . ?
O2 Zn1 O21 102.5(2) . . ?
O1 Zn1 Cl 112.67(11) . . ?
O2 Zn1 Cl 122.9(2) . . ?
O21 Zn1 Cl 111.20(11) . . ?
O2 Zn2 N23 105.6(2) 3_765 . ?
O2 Zn2 O2 80.6(2) 3_765 . ?
N23 Zn2 O2 89.3(2) . . ?
O2 Zn2 N3 88.7(2) 3_765 3_765 ?
N23 Zn2 N3 160.44(14) . 3_765 ?
O2 Zn2 N3 106.5(2) . 3_765 ?
O2 Zn2 N1 158.4(2) 3_765 3_765 ?
N23 Zn2 N1 93.52(13) . 3_765 ?
O2 Zn2 N1 90.0(2) . 3_765 ?
N3 Zn2 N1 75.35(13) 3_765 3_765 ?
O2 Zn2 N21 92.3(2) 3_765 . ?
N23 Zn2 N21 74.69(14) . . ?
O2 Zn2 N21 160.1(2) . . ?
N3 Zn2 N21 91.79(14) 3_765 . ?
N1 Zn2 N21 102.44(14) 3_765 . ?
N3 O1 Zn1 110.9(2) . . ?
Zn1 O2 Zn2 109.4(3) . 3_765 ?
Zn1 O2 Zn2 109.3(3) . . ?
Zn2 O2 Zn2 99.4(2) 3_765 . ?
N23 O21 Zn1 112.4(2) . . ?
C1 N1 C5 118.7(4) . . ?
C1 N1 Zn2 127.1(3) . 3_765 ?
C5 N1 Zn2 114.1(3) . 3_765 ?
C6 N3 O1 117.8(3) . . ?
C6 N3 Zn2 117.8(3) . 3_765 ?
O1 N3 Zn2 124.4(2) . 3_765 ?
C21 N21 C25 118.7(4) . . ?
C21 N21 Zn2 126.3(3) . . ?
C25 N21 Zn2 114.5(3) . . ?
C26 N23 O21 117.8(4) . . ?
C26 N23 Zn2 118.8(3) . . ?
O21 N23 Zn2 123.3(3) . . ?
C7 N2 C11 118.7(8) . . ?
N1 C1 C2 123.3(5) . . ?
C3 C2 C1 118.1(5) . . ?
C4 C3 C2 120.1(5) . . ?
C3 C4 C5 119.1(5) . . ?
N1 C5 C4 120.7(4) . . ?
N1 C5 C6 116.7(4) . . ?
C4 C5 C6 122.6(4) . . ?
N3 C6 C5 115.9(4) . . ?
N3 C6 C7 123.0(4) . . ?
C5 C6 C7 121.1(4) . . ?
N2 C7 C8 121.3(6) . . ?
N2 C7 C6 115.8(5) . . ?
C8 C7 C6 122.9(6) . . ?
C7 C8 C9 120.0(9) . . ?
C10 C9 C8 117.2(9) . . ?
C11 C10 C9 121.1(8) . . ?
C10 C11 N2 121.6(10) . . ?
C27 N22 C31 117.0(8) . . ?
N21 C21 C22 122.5(5) . . ?
C23 C22 C21 119.8(6) . . ?
C22 C23 C24 118.7(5) . . ?
C23 C24 C25 119.6(5) . . ?
N21 C25 C24 120.7(5) . . ?
N21 C25 C26 115.8(4) . . ?
C24 C25 C26 123.5(4) . . ?
N23 C26 C25 115.8(4) . . ?
N23 C26 C27 122.3(4) . . ?
C25 C26 C27 122.0(4) . . ?
N22 C27 C28 123.2(6) . . ?
N22 C27 C26 116.5(5) . . ?
C28 C27 C26 120.3(6) . . ?
C27 C28 C29 116.4(9) . . ?
C30 C29 C28 121.4(9) . . ?
C29 C30 C31 116.8(9) . . ?
N22 C31 C30 125.1(11) . . ?
C1S NS C2S 139.3(19) . . ?
C1S NS C3S 111.0(17) . . ?
C2S NS C3S 108.5(17) . . ?
OS C1S NS 147.8(19) . . ?
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 O1 1.956(3) . ?
Zn1 O2 1.963(5) . ?
Zn1 O21 1.964(3) . ?
Zn1 Cl 2.207(2) . ?
Zn2 O2 2.112(6) 3_765 ?
Zn2 N23 2.135(4) . ?
Zn2 O2 2.124(7) . ?
Zn2 N3 2.153(3) 3_765 ?
Zn2 N1 2.170(4) 3_765 ?
Zn2 N21 2.185(4) . ?
O1 N3 1.351(5) . ?
O2 Zn2 2.112(6) 3_765 ?
O21 N23 1.353(5) . ?
N1 C1 1.334(6) . ?
N1 C5 1.351(5) . ?
N1 Zn2 2.170(4) 3_765 ?
N3 C6 1.285(5) . ?
N3 Zn2 2.152(3) 3_765 ?
N21 C21 1.339(6) . ?
N21 C25 1.352(6) . ?
N23 C26 1.293(6) . ?
N2 C7 1.325(8) . ?
N2 C11 1.360(9) . ?
C1 C2 1.373(7) . ?
C2 C3 1.371(8) . ?
C3 C4 1.370(7) . ?
C4 C5 1.396(6) . ?
C5 C6 1.473(6) . ?
C6 C7 1.477(6) . ?
C7 C8 1.325(10) . ?
C8 C9 1.434(11) . ?
C9 C10 1.317(14) . ?
C10 C11 1.337(14) . ?
N22 C27 1.337(8) . ?
N22 C31 1.345(10) . ?
C21 C22 1.378(8) . ?
C22 C23 1.354(8) . ?
C23 C24 1.389(8) . ?
C24 C25 1.395(7) . ?
C25 C26 1.468(7) . ?
C26 C27 1.492(6) . ?
C27 C28 1.374(9) . ?
C28 C29 1.417(11) . ?
C29 C30 1.349(15) . ?
C30 C31 1.36(2) . ?
OS C1S 1.03(2) . ?
NS C1S 1.27(2) . ?
NS C2S 1.40(2) . ?
NS C3S 1.45(2) . ?
OM1 CM1 1.46(3) . ?
OM2 CM2 1.59(4) . ?
