#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/51/4305178.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_4305178
loop_
_publ_author_name
'Yurii S. Moroz'
'Kinga Kulon'
'Matti Haukka'
'Elżbieta Gumienna-Kontecka'
'Henryk Kozłowski'
'Franc Meyer'
'Igor O. Fritsky'
_publ_contact_author             'Igor O.Fritsky'
_publ_contact_author_email       ifritsky@univ.kiev.ua
_publ_section_title
;
Synthesis and Structure of [2 x 2] Molecular Grid Copper(II) and
Nickel(II) Complexes with a New Polydentate Oxime-Containing Schiff Base
Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5656
_journal_page_last               5665
_journal_paper_doi               10.1021/ic702375h
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C44 H48 Cu4 N16 O16, 2(H2 O)'
_chemical_formula_sum            'C11 H13 Cu N4 O4.5'
_chemical_formula_weight         336.79
_chemical_name_systematic
; 
 ?
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :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                   15.4644(10)
_cell_length_b                   15.4644(10)
_cell_length_c                   11.4200(4)
_cell_measurement_reflns_used    16074
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     2731.1(3)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            25942
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.44
_exptl_absorpt_coefficient_mu    1.623
_exptl_absorpt_correction_T_max  0.8771
_exptl_absorpt_correction_T_min  0.7076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Xprep in Shelxtl v.6.14-1 (Sheldrick, 2005)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0436
_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)+(0.0332P)²+3.9982P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.1034
_reflns_number_gt                2196
_reflns_number_total             3116
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702375h-file003.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_original_formula_sum        'C11 H13 Cu N4 O4.50'
_cod_database_code               4305178
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'y, -x-1/2, -z-1/2'
'x-1/2, y-1/2, -z'
'-y-1/2, x, -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_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
Cu1 Cu 0.10130(2) 0.36523(2) 0.24091(3) 0.02488(13) Uani 1 1 d . . .
O1 O 0.12419(14) 0.24182(14) 0.18872(18) 0.0277(5) Uani 1 1 d . . .
O2 O 0.01359(15) 0.33912(18) 0.4715(2) 0.0428(6) Uani 1 1 d . . .
O3 O -0.04185(16) 0.33697(17) 0.1922(2) 0.0408(6) Uani 1 1 d . . .
O4 O -0.11777(18) 0.3186(3) 0.3539(3) 0.0691(10) Uani 1 1 d . . .
HO4 H -0.0692 0.3056 0.3869 0.104 Uiso 1 1 d R . .
O5 O -0.2500 0.2500 0.5080(3) 0.0519(10) Uani 1 2 d S . .
H5O H -0.2892 0.2398 0.4418 0.078 Uiso 1 1 d R . .
N1 N 0.09462(17) 0.49776(17) 0.2290(2) 0.0296(6) Uani 1 1 d . . .
N2 N 0.11924(17) 0.38042(18) 0.0745(2) 0.0295(6) Uani 1 1 d . . .
N3 N 0.13295(18) 0.30912(18) 0.0064(2) 0.0309(6) Uani 1 1 d . . .
N4 N 0.09097(17) 0.34995(18) 0.4143(2) 0.0307(6) Uani 1 1 d . . .
C1 C 0.0868(2) 0.5559(2) 0.3135(3) 0.0376(8) Uani 1 1 d . . .
H1 H 0.0820 0.5366 0.3922 0.045 Uiso 1 1 calc R . .
C2 C 0.0856(3) 0.6444(2) 0.2907(4) 0.0491(10) Uani 1 1 d . . .
H2 H 0.0821 0.6847 0.3532 0.059 Uiso 1 1 calc R . .
C3 C 0.0894(3) 0.6723(3) 0.1775(3) 0.0502(11) Uani 1 1 d . . .
H3 H 0.0870 0.7324 0.1606 0.060 Uiso 1 1 calc R . .
C4 C 0.0969(3) 0.6128(2) 0.0872(3) 0.0410(9) Uani 1 1 d . . .
H4 H 0.0987 0.6310 0.0078 0.049 Uiso 1 1 calc R . .
C5 C 0.1016(2) 0.5266(2) 0.1162(3) 0.0315(7) Uani 1 1 d . . .
C6 C 0.1160(2) 0.4573(2) 0.0292(3) 0.0299(7) Uani 1 1 d . . .
C7 C 0.1267(2) 0.4761(2) -0.0982(3) 0.0372(8) Uani 1 1 d . . .
H7A H 0.1843 0.5004 -0.1121 0.056 Uiso 1 1 calc R . .
H7B H 0.0827 0.5178 -0.1231 0.056 Uiso 1 1 calc R . .
H7C H 0.1202 0.4225 -0.1431 0.056 Uiso 1 1 calc R . .
C8 C 0.1338(2) 0.2411(2) 0.0764(3) 0.0284(7) Uani 1 1 d . . .
C9 C 0.1568(2) 0.3531(2) 0.4824(3) 0.0308(7) Uani 1 1 d . . .
C10 C 0.1509(3) 0.3471(3) 0.6127(3) 0.0482(10) Uani 1 1 d . . .
H10A H 0.1068 0.3874 0.6412 0.072 Uiso 1 1 calc R . .
H10B H 0.2069 0.3619 0.6473 0.072 Uiso 1 1 calc R . .
H10C H 0.1351 0.2880 0.6351 0.072 Uiso 1 1 calc R . .
C11 C -0.1075(2) 0.3174(3) 0.2446(3) 0.0402(8) Uani 1 1 d . . .
H11 H -0.1555 0.2995 0.1987 0.048 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'
O O 0.0106 0.0060 '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 N4 176.33(11) . . y
N2 Cu1 O1 78.51(10) . . y
N4 Cu1 O1 101.15(10) . . y
N2 Cu1 N1 79.69(11) . . y
N4 Cu1 N1 100.33(11) . . y
O1 Cu1 N1 157.81(10) . . y
N2 Cu1 O1 101.37(9) . 6_566 y
N4 Cu1 O1 74.96(9) . 6_566 y
O1 Cu1 O1 90.26(11) . 6_566 y
N1 Cu1 O1 89.99(9) . 6_566 y
N2 Cu1 O3 85.67(10) . . y
N4 Cu1 O3 97.96(10) . . y
O1 Cu1 O3 85.36(9) . . y
N1 Cu1 O3 97.11(10) . . y
O1 Cu1 O3 170.83(8) 6_566 . y
N2 Cu1 Cu1 83.81(8) . 6_566 ?
N4 Cu1 Cu1 92.53(8) . 6_566 ?
O1 Cu1 Cu1 87.71(6) . 6_566 ?
N1 Cu1 Cu1 85.87(7) . 6_566 ?
O1 Cu1 Cu1 17.59(5) 6_566 6_566 ?
O3 Cu1 Cu1 168.38(6) . 6_566 ?
C8 O1 Cu1 108.7(2) . . ?
C8 O1 Cu1 109.09(19) . 8_656 ?
Cu1 O1 Cu1 142.20(10) . 8_656 ?
C11 O3 Cu1 136.4(2) . . ?
C11 O4 HO4 108.6 . . ?
C1 N1 C5 118.2(3) . . ?
C1 N1 Cu1 129.2(2) . . ?
C5 N1 Cu1 112.6(2) . . ?
C6 N2 N3 121.3(3) . . ?
C6 N2 Cu1 119.8(2) . . ?
N3 N2 Cu1 118.9(2) . . ?
C8 N3 N2 107.5(3) . . ?
C9 N4 O2 114.1(3) . . ?
C9 N4 Cu1 122.2(2) . . ?
O2 N4 Cu1 123.7(2) . . ?
N1 C1 C2 122.1(3) . . ?
N1 C1 H1 118.9 . . ?
C2 C1 H1 118.9 . . ?
C3 C2 C1 119.2(4) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 119.8(4) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 117.9(3) . . ?
C5 C4 H4 121.0 . . ?
C3 C4 H4 121.0 . . ?
N1 C5 C4 122.6(3) . . ?
N1 C5 C6 114.1(3) . . ?
C4 C5 C6 123.3(3) . . ?
N2 C6 C5 113.8(3) . . ?
N2 C6 C7 124.2(3) . . ?
C5 C6 C7 122.0(3) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O1 C8 N3 126.3(3) . . ?
O1 C8 C9 118.3(3) . 8_656 ?
N3 C8 C9 115.3(3) . 8_656 ?
N4 C9 C8 115.4(3) . 6_566 ?
N4 C9 C10 123.6(3) . . ?
C8 C9 C10 121.0(3) 6_566 . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O3 C11 O4 126.1(4) . . ?
O3 C11 H11 117.0 . . ?
O4 C11 H11 117.0 . . ?
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 1.935(3) . y
Cu1 N4 2.001(3) . y
Cu1 O1 2.030(2) . y
Cu1 N1 2.057(3) . y
Cu1 O1 2.323(2) 6_566 y
Cu1 O3 2.324(2) . y
Cu1 Cu1 4.1195(6) 6_566 y
O1 C8 1.291(4) . y
O1 Cu1 2.323(2) 8_656 n
O2 N4 1.374(3) . y
O3 C11 1.217(4) . y
O4 C11 1.259(4) . y
O4 HO4 0.8647 . ?
O5 H5O 0.9817 . ?
N1 C1 1.325(4) . y
N1 C5 1.367(4) . y
N2 C6 1.297(4) . y
N2 N3 1.366(4) . y
N3 C8 1.322(4) . y
N4 C9 1.282(4) . y
C1 C2 1.392(5) . n
C1 H1 0.9500 . ?
C2 C3 1.364(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.387(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.375(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.478(5) . ?
C6 C7 1.494(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.479(4) 8_656 ?
C9 C8 1.479(5) 6_566 ?
C9 C10 1.494(5) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11 0.9500 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 HO4 O2 0.86 1.69 2.456(4) 147.0 .
O5 H5O O4 0.98 1.97 2.899(4) 156.3 3_455
