#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:34:00 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179796 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/92/7009263.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_7009263
loop_
_publ_author_name
'He Cheng'
'Duan Chun-ying'
'Fang Chen-jie'
'Liu Yong-jiang'
'Meng Qing-jin'
_publ_section_title
;
 Self-assembled macrocyclic tetranuclear molecular square [Ni(HL)]44+
 and molecular rectangle
 [Cu2Cl2L]2{H2L = bis[phenyl(2-pyridyl)methanone]
 thiocarbazone}
;
_journal_issue                   7
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1207
_journal_page_last               1212
_journal_paper_doi               10.1039/a909604c
_journal_year                    2000
_chemical_formula_sum            'C25 H18 Cl2 Cu2 N6 S'
_chemical_formula_weight         632.49
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.43(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.142(3)
_cell_length_b                   10.625(2)
_cell_length_c                   19.535(6)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.47
_cell_measurement_theta_min      5.13
_cell_volume                     2520.1(11)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω 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  0.0995
_diffrn_reflns_av_sigmaI/netI    0.1836
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            3559
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.97
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.010
_exptl_crystal_colour            dark-blue
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.028
_refine_ls_goodness_of_fit_obs   1.222
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         2734
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.043
_refine_ls_restrained_S_obs      1.173
_refine_ls_R_factor_all          0.1850
_refine_ls_R_factor_obs          0.0728
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0261P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1519
_refine_ls_wR_factor_obs         0.1129
_reflns_number_observed          1600
_reflns_number_total             3365
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a909604c.txt
_cod_data_source_block           compound_3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+0.0000P] 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^)+(0.0261P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_database_code               7009263
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Cu1 Cu 0.12928(8) -0.18678(10) 0.43144(5) 0.0392(3) Uani 1 d . .
Cu2 Cu -0.18660(8) 0.03563(10) 0.41830(5) 0.0400(3) Uani 1 d . .
Cl1 Cl 0.0893(2) -0.2518(2) 0.53630(11) 0.0524(7) Uani 1 d . .
Cl2 Cl -0.2380(2) -0.0225(2) 0.52414(10) 0.0435(6) Uani 1 d . .
S1 S -0.0323(2) -0.0866(2) 0.40962(10) 0.0447(7) Uani 1 d . .
N1 N 0.2615(5) -0.2980(5) 0.4201(3) 0.034(2) Uani 1 d . .
C1 C 0.3016(7) -0.3842(8) 0.4589(5) 0.051(3) Uani 1 d . .
H1A H 0.2676(7) -0.3970(8) 0.5008(5) 0.062 Uiso 1 calc R .
C2 C 0.3913(7) -0.4600(8) 0.4437(5) 0.061(3) Uani 1 d . .
H2A H 0.4179(7) -0.5205(8) 0.4739(5) 0.073 Uiso 1 calc R .
C3 C 0.4380(7) -0.4392(7) 0.3808(5) 0.057(3) Uani 1 d . .
H3A H 0.4973(7) -0.4883(7) 0.3671(5) 0.069 Uiso 1 calc R .
C4 C 0.3987(7) -0.3478(7) 0.3381(4) 0.047(3) Uani 1 d . .
H4A H 0.4338(7) -0.3325(7) 0.2967(4) 0.056 Uiso 1 calc R .
C5 C 0.3087(6) -0.2786(7) 0.3554(4) 0.038(2) Uani 1 d . .
C6 C 0.2539(6) -0.1875(7) 0.3134(3) 0.031(2) Uani 1 d . .
C7 C 0.3034(7) -0.1459(7) 0.2483(4) 0.041(3) Uani 1 d . .
C8 C 0.3111(7) -0.2243(8) 0.1909(4) 0.053(3) Uani 1 d . .
H8A H 0.2823(7) -0.3052(8) 0.1929(4) 0.063 Uiso 1 calc R .
C9 C 0.3597(7) -0.1849(10) 0.1323(4) 0.071(3) Uani 1 d . .
H9A H 0.3640(7) -0.2392(10) 0.0951(4) 0.085 Uiso 1 calc R .
C10 C 0.4029(7) -0.0648(9) 0.1275(5) 0.071(3) Uani 1 d . .
H10A H 0.4336(7) -0.0362(9) 0.0869(5) 0.085 Uiso 1 calc R .
C11 C 0.3992(7) 0.0116(8) 0.1846(5) 0.065(3) Uani 1 d . .
H11A H 0.4322(7) 0.0905(8) 0.1833(5) 0.078 Uiso 1 calc R .
C12 C 0.3480(7) -0.0266(8) 0.2425(5) 0.057(3) Uani 1 d . .
H12A H 0.3429(7) 0.0287(8) 0.2792(5) 0.068 Uiso 1 calc R .
N2 N 0.1625(5) -0.1429(6) 0.3371(3) 0.035(2) Uani 1 d . .
N3 N 0.1019(5) -0.0610(6) 0.2989(3) 0.033(2) Uani 1 d . .
C13 C 0.0073(6) -0.0307(7) 0.3272(3) 0.027(2) Uani 1 d . .
N4 N -0.0598(5) 0.0432(6) 0.2895(3) 0.039(2) Uani 1 d . .
N5 N -0.1554(5) 0.0727(6) 0.3226(3) 0.037(2) Uani 1 d . .
N6 N -0.3302(5) 0.1217(6) 0.3926(3) 0.044(2) Uani 1 d . .
C14 C -0.4205(6) 0.1385(8) 0.4296(4) 0.048(3) Uani 1 d . .
H14A H -0.4225(6) 0.1068(8) 0.4740(4) 0.058 Uiso 1 calc R .
C15 C -0.5119(7) 0.2018(8) 0.4040(4) 0.054(3) Uani 1 d . .
H15A H -0.5741(7) 0.2121(8) 0.4309(4) 0.065 Uiso 1 calc R .
C16 C -0.5097(7) 0.2494(8) 0.3380(4) 0.049(3) Uani 1 d . .
H16A H -0.5698(7) 0.2929(8) 0.3202(4) 0.058 Uiso 1 calc R .
C17 C -0.4171(6) 0.2311(7) 0.2998(4) 0.043(3) Uani 1 d . .
H17A H -0.4121(6) 0.2648(7) 0.2560(4) 0.051 Uiso 1 calc R .
C18 C -0.3313(7) 0.1621(7) 0.3270(4) 0.035(2) Uani 1 d . .
C19 C -0.2313(7) 0.1315(8) 0.2897(4) 0.046(3) Uani 1 d . .
C20 C -0.2244(5) 0.1589(6) 0.2149(3) 0.064(3) Uani 1 d D .
C21 C -0.1640(8) 0.2568(8) 0.1870(3) 0.083(3) Uani 0.791(8) d PDU 1
H21A H -0.1250(8) 0.3110(8) 0.2157(3) 0.099 Uiso 0.791(8) calc PR 1
C22 C -0.1612(8) 0.2743(8) 0.1166(3) 0.084(3) Uani 0.791(8) d PDU 1
H22A H -0.1179(8) 0.3374(8) 0.0977(3) 0.101 Uiso 0.791(8) calc PR 1
C23 C -0.2241(7) 0.1965(8) 0.0747(4) 0.083(3) Uani 0.791(8) d PDU 1
H23A H -0.2236(7) 0.2103(8) 0.0277(4) 0.099 Uiso 0.791(8) calc PR 1
C24 C -0.2879(8) 0.0986(9) 0.1002(3) 0.077(3) Uani 0.791(8) d PDU 1
H24A H -0.3299(8) 0.0478(9) 0.0714(3) 0.092 Uiso 0.791(8) calc PR 1
C25 C -0.2863(8) 0.0798(9) 0.1711(3) 0.071(4) Uani 0.791(8) d PDU 1
H25A H -0.3267(8) 0.0140(9) 0.1897(3) 0.085 Uiso 0.791(8) calc PR 1
C21' C -0.1469(10) 0.2565(12) 0.2135(5) 0.085(6) Uani 0.209(8) d PDU 2
H21B H -0.1244(10) 0.2871(12) 0.2560(5) 0.103 Uiso 0.209(8) calc PR 2
C22' C -0.0988(10) 0.3141(18) 0.1566(4) 0.087(4) Uani 0.209(8) d PDU 2
H22B H -0.0364(10) 0.3647(18) 0.1582(4) 0.104 Uiso 0.209(8) calc PR 2
C23' C -0.1582(9) 0.2846(15) 0.0971(6) 0.085(4) Uani 0.209(8) d PDU 2
H23B H -0.1354(9) 0.3256(15) 0.0576(6) 0.102 Uiso 0.209(8) calc PR 2
C24' C -0.2470(12) 0.2023(15) 0.0888(5) 0.082(4) Uani 0.209(8) d PDU 2
H24B H -0.2849(12) 0.1899(15) 0.0479(5) 0.098 Uiso 0.209(8) calc PR 2
C25' C -0.2713(14) 0.1411(19) 0.1502(4) 0.081(4) Uani 0.209(8) d PDU 2
H25B H -0.3262(14) 0.0802(19) 0.1476(4) 0.097 Uiso 0.209(8) calc PR 2
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'
S S 0.1246 0.1234 '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'
Cu Cu 0.3201 1.2651 '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
N2 Cu1 N1 82.2(3) . . ?
N2 Cu1 Cl1 175.6(2) . . ?
N1 Cu1 Cl1 95.7(2) . . ?
N2 Cu1 S1 84.0(2) . . ?
N1 Cu1 S1 161.2(2) . . ?
Cl1 Cu1 S1 97.16(9) . . ?
N2 Cu1 Cl2 90.2(2) . 3_556 ?
N1 Cu1 Cl2 97.4(2) . 3_556 ?
Cl1 Cu1 Cl2 93.96(8) . 3_556 ?
S1 Cu1 Cl2 95.34(8) . 3_556 ?
N5 Cu2 N6 81.1(2) . . ?
N5 Cu2 Cl2 173.3(2) . . ?
N6 Cu2 Cl2 96.2(2) . . ?
N5 Cu2 S1 83.0(2) . . ?
N6 Cu2 S1 160.2(2) . . ?
Cl2 Cu2 S1 98.35(9) . . ?
N5 Cu2 Cl1 93.1(2) . 3_556 ?
N6 Cu2 Cl1 94.0(2) . 3_556 ?
Cl2 Cu2 Cl1 93.14(8) . 3_556 ?
S1 Cu2 Cl1 98.58(8) . 3_556 ?
Cu1 Cl1 Cu2 86.59(8) . 3_556 ?
Cu2 Cl2 Cu1 86.08(8) . 3_556 ?
C13 S1 Cu1 95.0(3) . . ?
C13 S1 Cu2 96.0(3) . . ?
Cu1 S1 Cu2 163.71(11) . . ?
C1 N1 C5 118.7(7) . . ?
C1 N1 Cu1 130.9(6) . . ?
C5 N1 Cu1 110.2(5) . . ?
N1 C1 C2 125.6(8) . . ?
C3 C2 C1 115.3(8) . . ?
C4 C3 C2 121.1(8) . . ?
C5 C4 C3 120.7(8) . . ?
C4 C5 N1 118.5(7) . . ?
C4 C5 C6 126.4(7) . . ?
N1 C5 C6 115.1(6) . . ?
N2 C6 C5 116.0(6) . . ?
N2 C6 C7 123.6(7) . . ?
C5 C6 C7 120.4(7) . . ?
C12 C7 C8 116.8(7) . . ?
C12 C7 C6 120.4(7) . . ?
C8 C7 C6 122.8(7) . . ?
C9 C8 C7 121.6(8) . . ?
C8 C9 C10 120.6(9) . . ?
C11 C10 C9 118.2(8) . . ?
C12 C11 C10 121.0(9) . . ?
C11 C12 C7 121.6(8) . . ?
C6 N2 N3 120.0(6) . . ?
C6 N2 Cu1 115.8(5) . . ?
N3 N2 Cu1 123.9(5) . . ?
C13 N3 N2 113.4(6) . . ?
N3 C13 N4 116.1(6) . . ?
N3 C13 S1 122.5(6) . . ?
N4 C13 S1 121.4(5) . . ?
C13 N4 N5 112.7(6) . . ?
C19 N5 N4 118.8(6) . . ?
C19 N5 Cu2 115.8(5) . . ?
N4 N5 Cu2 125.3(5) . . ?
C14 N6 C18 118.1(7) . . ?
C14 N6 Cu2 129.5(5) . . ?
C18 N6 Cu2 112.3(5) . . ?
N6 C14 C15 121.9(8) . . ?
C16 C15 C14 119.5(8) . . ?
C17 C16 C15 118.5(8) . . ?
C16 C17 C18 119.1(8) . . ?
N6 C18 C17 122.5(7) . . ?
N6 C18 C19 113.6(7) . . ?
C17 C18 C19 123.8(7) . . ?
N5 C19 C18 117.1(7) . . ?
N5 C19 C20 122.8(7) . . ?
C18 C19 C20 119.9(7) . . ?
C25' C20 C21' 110.6(9) . . ?
C21 C20 C25 119.2(6) . . ?
C21 C20 C19 124.4(6) . . ?
C25' C20 C19 146.6(8) . . ?
C21' C20 C19 101.9(6) . . ?
C25 C20 C19 116.4(6) . . ?
C20 C21 C22 120.4(7) . . ?
C23 C22 C21 119.1(8) . . ?
C22 C23 C24 122.7(7) . . ?
C23 C24 C25 117.2(8) . . ?
C24 C25 C20 121.3(7) . . ?
C22' C21' C20 128.5(10) . . ?
C23' C22' C21' 110.3(10) . . ?
C24' C23' C22' 129.0(11) . . ?
C23' C24' C25' 111.1(11) . . ?
C20 C25' C24' 128.8(11) . . ?
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
Cu1 N2 1.947(6) . ?
Cu1 N1 2.007(6) . ?
Cu1 Cl1 2.219(2) . ?
Cu1 S1 2.270(2) . ?
Cu1 Cl2 2.724(2) 3_556 ?
Cu2 N5 1.950(6) . ?
Cu2 N6 2.029(6) . ?
Cu2 Cl2 2.250(2) . ?
Cu2 S1 2.286(2) . ?
Cu2 Cl1 2.729(3) 3_556 ?
Cl1 Cu2 2.729(3) 3_556 ?
Cl2 Cu1 2.724(2) 3_556 ?
S1 C13 1.786(7) . ?
N1 C1 1.282(10) . ?
N1 C5 1.406(9) . ?
C1 C2 1.389(11) . ?
C2 C3 1.375(12) . ?
C3 C4 1.364(11) . ?
C4 C5 1.363(10) . ?
C5 C6 1.430(10) . ?
C6 N2 1.295(9) . ?
C6 C7 1.478(10) . ?
C7 C12 1.383(11) . ?
C7 C8 1.400(10) . ?
C8 C9 1.357(10) . ?
C9 C10 1.384(13) . ?
C10 C11 1.380(12) . ?
C11 C12 1.357(11) . ?
N2 N3 1.359(8) . ?
N3 C13 1.318(9) . ?
C13 N4 1.347(9) . ?
N4 N5 1.369(8) . ?
N5 C19 1.282(10) . ?
N6 C14 1.329(9) . ?
N6 C18 1.352(9) . ?
C14 C15 1.387(11) . ?
C15 C16 1.384(11) . ?
C16 C17 1.369(11) . ?
C17 C18 1.377(10) . ?
C18 C19 1.458(11) . ?
C19 C20 1.491(9) . ?
C20 C21 1.387(7) . ?
C20 C25' 1.396(8) . ?
C20 C21' 1.401(9) . ?
C20 C25 1.413(7) . ?
C21 C22 1.390(7) . ?
C22 C23 1.388(8) . ?
C23 C24 1.391(8) . ?
C24 C25 1.398(7) . ?
C21' C22' 1.400(9) . ?
C22' C23' 1.398(9) . ?
C23' C24' 1.397(9) . ?
C24' C25' 1.397(9) . ?
