#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:45:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179456 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/53/4335367.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_4335367
loop_
_publ_author_name
'Elzbieta Gumienna-Kontecka'
'Irina A. Golenya'
'Agnieszka Szebesczyk'
'Matti Haukka'
'Roland Krämer'
'Igor O. Fritsky'
_publ_contact_author             'Igor O.Fritsky'
_publ_contact_author_email       ifritsky@univ.kiev.ua
_publ_section_title
;
 Coordination Diversity in Mono- and Oligonuclear Copper(II) Complexes of
 Pyridine-2-Hydroxamic and Pyridine-2,6-Dihydroxamic Acids
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7633
_journal_page_last               7644
_journal_paper_doi               10.1021/ic4007229
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C27 H21 Cl2 Cu2 N7 O12, C3 H6 N O, H2 O'
_chemical_formula_sum            'C30 H29 Cl2 Cu2 N8 O14'
_chemical_formula_weight         923.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 107.710(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9500(10)
_cell_length_b                   13.8215(10)
_cell_length_c                   17.9208(14)
_cell_measurement_reflns_used    9506
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.00
_cell_volume                     3999.4(5)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Diamond v.3.1d (Brandenburg, 2006)'
_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 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0651
_diffrn_reflns_av_sigmaI/netI    0.0702
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12260
_diffrn_reflns_theta_full        25.11
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    1.269
_exptl_absorpt_correction_T_max  0.9323
_exptl_absorpt_correction_T_min  0.7827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       needle
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.312
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3486
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1191
_refine_ls_R_factor_gt           0.0797
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1315P)²+29.9931P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2222
_refine_ls_wR_factor_ref         0.2491
_reflns_number_gt                2337
_reflns_number_total             3486
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4007229_si_003.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4335367
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_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 0.59459(5) 0.04670(7) 0.51889(5) 0.0370(4) Uani 1 1 d . . .
Cl2 Cl 0.78280(12) -0.03723(15) 0.67969(11) 0.0457(5) Uani 1 1 d . . .
O1 O 0.5478(3) -0.0402(3) 0.5784(3) 0.0388(12) Uani 1 1 d . . .
O2 O 0.5676(3) 0.1477(4) 0.5826(3) 0.0398(12) Uani 1 1 d . . .
O5 O 0.7266(4) 0.0418(5) 0.6526(5) 0.076(2) Uani 1 1 d . . .
O6 O 0.8296(5) -0.0486(5) 0.6266(5) 0.089(3) Uani 1 1 d . . .
O7 O 0.7358(4) -0.1226(5) 0.6821(4) 0.0710(19) Uani 1 1 d . . .
O8 O 0.8335(5) -0.0213(6) 0.7551(5) 0.087(2) Uani 1 1 d . . .
O9 O 0.5000 -0.1090(5) 0.7500 0.0447(18) Uani 1 2 d S . .
N1 N 0.6400(3) 0.1361(5) 0.4557(3) 0.0359(14) Uani 1 1 d . . .
N2 N 0.6414(4) -0.0517(5) 0.4641(4) 0.0403(15) Uani 1 1 d . . .
N3 N 0.5389(4) 0.0137(4) 0.6399(3) 0.0352(13) Uani 1 1 d . . .
H3 H 0.5281 -0.0146 0.6797 0.042 Uiso 1 1 calc R . .
N4 N 0.5000 0.1152(6) 0.7500 0.0326(18) Uani 1 2 d S . .
C1 C 0.6366(4) 0.2314(6) 0.4561(4) 0.0401(17) Uani 1 1 d . . .
H1 H 0.6086 0.2617 0.4884 0.048 Uiso 1 1 calc R . .
C2 C 0.6714(5) 0.2891(7) 0.4122(4) 0.050(2) Uani 1 1 d . . .
H2 H 0.6681 0.3576 0.4144 0.060 Uiso 1 1 calc R . .
C3 C 0.7116(5) 0.2444(7) 0.3645(5) 0.050(2) Uani 1 1 d . . .
H3A H 0.7371 0.2819 0.3339 0.061 Uiso 1 1 calc R . .
C4 C 0.7137(5) 0.1460(7) 0.3623(4) 0.048(2) Uani 1 1 d . . .
H4 H 0.7407 0.1146 0.3297 0.058 Uiso 1 1 calc R . .
C5 C 0.6760(4) 0.0907(6) 0.4080(4) 0.0420(18) Uani 1 1 d . . .
C6 C 0.6758(4) -0.0146(7) 0.4109(4) 0.0447(19) Uani 1 1 d . . .
C7 C 0.7056(5) -0.0762(7) 0.3648(5) 0.053(2) Uani 1 1 d . . .
H7 H 0.7297 -0.0501 0.3278 0.064 Uiso 1 1 calc R . .
C8 C 0.7006(5) -0.1726(8) 0.3722(5) 0.061(2) Uani 1 1 d . . .
H8 H 0.7199 -0.2141 0.3392 0.073 Uiso 1 1 calc R . .
C9 C 0.6674(5) -0.2122(7) 0.4276(5) 0.057(2) Uani 1 1 d . . .
H9 H 0.6648 -0.2802 0.4346 0.068 Uiso 1 1 calc R . .
C10 C 0.6383(5) -0.1463(7) 0.4721(5) 0.052(2) Uani 1 1 d . . .
H10 H 0.6150 -0.1710 0.5102 0.062 Uiso 1 1 calc R . .
C11 C 0.5469(4) 0.1069(5) 0.6381(4) 0.0356(16) Uani 1 1 d . . .
C12 C 0.5260(5) 0.1667(6) 0.6987(4) 0.0400(17) Uani 1 1 d . . .
C13 C 0.5304(5) 0.2663(6) 0.6981(5) 0.053(2) Uani 1 1 d . . .
H13 H 0.5535 0.2993 0.6632 0.063 Uiso 1 1 calc R . .
N5 N 0.4826(13) -0.2719(9) 0.7672(13) 0.067(7) Uani 0.50 1 d P . .
C14 C 0.5000 0.3164(9) 0.7500 0.059(3) Uani 1 2 d S . .
H14 H 0.5000 0.3851 0.7500 0.071 Uiso 1 2 calc SR . .
C15 C 0.5000 -0.1971(13) 0.7500 0.097(5) Uiso 1 2 d SD . .
C17 C 0.5000 -0.3672(10) 0.7500 0.093(5) Uani 1 2 d SD . .
C18 C 0.4269(12) -0.2726(13) 0.8172(11) 0.083(7) Uani 0.50 1 d PD . .
O10A O 0.5000 0.5000 0.5000 0.075(6) Uani 0.50 2 d SP A 1
O10B O 0.5051(14) 0.3908(19) 0.477(2) 0.079(9) Uani 0.25 1 d P B 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'
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'
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
O1 Cu1 O2 85.0(2) . .
O1 Cu1 N2 98.1(2) . .
O2 Cu1 N2 170.5(2) . .
O1 Cu1 N1 178.6(2) . .
O2 Cu1 N1 95.1(2) . .
N2 Cu1 N1 82.0(3) . .
O8 Cl2 O6 111.3(5) . .
O8 Cl2 O7 106.8(5) . .
O6 Cl2 O7 111.0(4) . .
O8 Cl2 O5 111.2(5) . .
O6 Cl2 O5 107.9(5) . .
O7 Cl2 O5 108.6(4) . .
N3 O1 Cu1 105.7(4) . .
C11 O2 Cu1 108.0(4) . .
C1 N1 C5 119.8(7) . .
C1 N1 Cu1 126.5(5) . .
C5 N1 Cu1 113.7(5) . .
C10 N2 C6 119.4(7) . .
C10 N2 Cu1 126.3(6) . .
C6 N2 Cu1 114.2(5) . .
C11 N3 O1 118.6(6) . .
C11 N3 H3 120.7 . .
O1 N3 H3 120.7 . .
C12 N4 C12 115.9(9) . 2_656
N1 C1 C2 123.4(7) . .
N1 C1 H1 118.3 . .
C2 C1 H1 118.3 . .
C1 C2 C3 118.1(8) . .
C1 C2 H2 120.9 . .
C3 C2 H2 120.9 . .
C4 C3 C2 118.9(8) . .
C4 C3 H3A 120.5 . .
C2 C3 H3A 120.5 . .
C3 C4 C5 120.4(8) . .
C3 C4 H4 119.8 . .
C5 C4 H4 119.8 . .
N1 C5 C4 119.3(8) . .
N1 C5 C6 115.8(7) . .
C4 C5 C6 124.8(7) . .
N2 C6 C7 119.9(8) . .
N2 C6 C5 114.2(7) . .
C7 C6 C5 126.0(8) . .
C8 C7 C6 120.4(9) . .
C8 C7 H7 119.8 . .
C6 C7 H7 119.8 . .
C7 C8 C9 120.7(8) . .
C7 C8 H8 119.7 . .
C9 C8 H8 119.7 . .
C8 C9 C10 116.1(9) . .
C8 C9 H9 122.0 . .
C10 C9 H9 122.0 . .
N2 C10 C9 123.5(8) . .
N2 C10 H10 118.2 . .
C9 C10 H10 118.2 . .
O2 C11 N3 120.8(6) . .
O2 C11 C12 120.2(6) . .
N3 C11 C12 118.9(6) . .
N4 C12 C13 124.4(7) . .
N4 C12 C11 114.0(7) . .
C13 C12 C11 121.6(7) . .
C14 C13 C12 117.7(8) . .
C14 C13 H13 121.1 . .
C12 C13 H13 121.1 . .
N5 N5 C15 64.8(9) 2_656 .
N5 N5 C17 69.7(7) 2_656 .
C15 N5 C17 134.5(15) . .
N5 N5 C18 178(4) 2_656 .
C15 N5 C18 115.6(15) . .
C17 N5 C18 109.9(12) . .
C13 C14 C13 119.7(12) 2_656 .
C13 C14 H14 120.2 2_656 .
C13 C14 H14 120.2 . .
N5 C15 N5 50.4(19) 2_656 .
N5 C15 O9 154.8(10) 2_656 .
N5 C15 O9 154.8(10) . .
N5 C17 N5 40.5(14) . 2_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.929(5) .
Cu1 O2 1.944(5) .
Cu1 N2 1.980(6) .
Cu1 N1 1.983(6) .
Cl2 O8 1.380(8) .
Cl2 O6 1.421(7) .
Cl2 O7 1.432(7) .
Cl2 O5 1.433(7) .
O1 N3 1.376(7) .
O2 C11 1.282(8) .
O9 C15 1.218(19) .
N1 C1 1.319(10) .
N1 C5 1.347(9) .
N2 C10 1.318(11) .
N2 C6 1.359(10) .
N3 C11 1.296(9) .
N3 H3 0.8800 .
N4 C12 1.339(8) .
N4 C12 1.339(8) 2_656
C1 C2 1.372(11) .
C1 H1 0.9500 .
C2 C3 1.390(12) .
C2 H2 0.9500 .
C3 C4 1.360(13) .
C3 H3A 0.9500 .
C4 C5 1.407(11) .
C4 H4 0.9500 .
C5 C6 1.457(13) .
C6 C7 1.384(11) .
C7 C8 1.344(14) .
C7 H7 0.9500 .
C8 C9 1.394(13) .
C8 H8 0.9500 .
C9 C10 1.396(12) .
C9 H9 0.9500 .
C10 H10 0.9500 .
C11 C12 1.490(10) .
C12 C13 1.379(11) .
C13 C14 1.378(10) .
C13 H13 0.9500 .
N5 N5 0.97(3) 2_656
N5 C15 1.142(19) .
N5 C17 1.404(18) .
N5 C18 1.49(2) .
C14 C13 1.378(10) 2_656
C14 H14 0.9500 .
C15 N5 1.142(19) 2_656
C17 N5 1.404(18) 2_656
