#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/19/7011941.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_7011941
loop_
_publ_author_name
'Saha, Manas Kumar'
'Dey, Dilip Kumar'
'Samanta, Brajagopal'
'Edwards, Andrew J.'
'Clegg, William'
'Mitra, Samiran'
_publ_section_title
;
 Synthesis, structure and magnetic properties of a mononuclear Cu(ii)
 complex with a NNO donor Schiff base ligand and its oxalato- and
 oxamidato-bridged dinuclear complexes
;
_journal_issue                   3
_journal_name_full               'Dalton Transactions'
_journal_page_first              488
_journal_paper_doi               10.1039/b206076k
_journal_year                    2003
_chemical_formula_sum            'C28 H36 Cu2 N6 O6 S2'
_chemical_formula_weight         743.83
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.720(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3820(8)
_cell_length_b                   13.6689(11)
_cell_length_c                   12.2240(10)
_cell_measurement_reflns_used    7030
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.61
_cell_measurement_theta_min      2.25
_cell_volume                     1545.1(2)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_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  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9342
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.63
_diffrn_reflns_theta_min         2.25
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.564
_exptl_absorpt_correction_T_max  0.802
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3633
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0251
_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)+(0.0358P)²+0.5514P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0688
_reflns_number_gt                3079
_reflns_number_total             3633
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b206076k.txt
_cod_data_source_block           jad06
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7011941
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_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
Cu Cu 0.23615(2) 0.497583(13) 0.383333(15) 0.01492(7) Uani 1 1 d . . .
S S 0.22275(6) 0.40500(4) -0.00958(4) 0.03382(13) Uani 1 1 d . . .
O1 O 0.08923(12) 0.40812(8) 0.41058(10) 0.0196(2) Uani 1 1 d . . .
O2 O 0.37402(12) 0.40597(8) 0.47669(9) 0.0184(2) Uani 1 1 d . . .
O3 O 0.59252(12) 0.40964(8) 0.58362(9) 0.0175(2) Uani 1 1 d . . .
N1 N 0.10365(14) 0.60213(9) 0.32206(11) 0.0161(3) Uani 1 1 d . . .
N2 N 0.23628(18) 0.71232(11) 0.00359(12) 0.0278(3) Uani 1 1 d . . .
H2N H 0.2597 0.7782 0.0133 0.033 Uiso 1 1 calc R . .
N3 N 0.27207(16) 0.44482(10) 0.21876(12) 0.0233(3) Uani 1 1 d . . .
C1 C -0.04987(17) 0.41826(12) 0.37559(13) 0.0172(3) Uani 1 1 d . . .
C2 C -0.14556(18) 0.34295(12) 0.39716(13) 0.0212(3) Uani 1 1 d . . .
H2 H -0.1075 0.2874 0.4389 0.025 Uiso 1 1 calc R . .
C3 C -0.29068(19) 0.34832(13) 0.35945(14) 0.0239(4) Uani 1 1 d . . .
H3 H -0.3509 0.2961 0.3751 0.029 Uiso 1 1 calc R . .
C4 C -0.35336(19) 0.42836(13) 0.29851(14) 0.0249(4) Uani 1 1 d . . .
H4 H -0.4542 0.4302 0.2707 0.030 Uiso 1 1 calc R . .
C5 C -0.26463(19) 0.50438(13) 0.27996(15) 0.0231(4) Uani 1 1 d . . .
H5 H -0.3061 0.5603 0.2407 0.028 Uiso 1 1 calc R . .
C6 C -0.11368(18) 0.50200(11) 0.31745(14) 0.0188(3) Uani 1 1 d . . .
C7 C -0.03407(18) 0.58905(12) 0.29903(13) 0.0183(3) Uani 1 1 d . . .
H7 H -0.0896 0.6428 0.2662 0.022 Uiso 1 1 calc R . .
C8 C 0.16040(18) 0.69993(11) 0.30220(13) 0.0183(3) Uani 1 1 d . . .
H8A H 0.2200 0.7238 0.3717 0.022 Uiso 1 1 calc R . .
H8B H 0.0783 0.7457 0.2824 0.022 Uiso 1 1 calc R . .
C9 C 0.25164(18) 0.70092(12) 0.20997(13) 0.0185(3) Uani 1 1 d . . .
H9A H 0.2995 0.7654 0.2089 0.022 Uiso 1 1 calc R . .
H9B H 0.3280 0.6504 0.2255 0.022 Uiso 1 1 calc R . .
C10 C 0.16038(18) 0.68150(12) 0.09683(13) 0.0211(3) Uani 1 1 d . . .
H10A H 0.1378 0.6108 0.0897 0.025 Uiso 1 1 calc R . .
H10B H 0.0679 0.7175 0.0911 0.025 Uiso 1 1 calc R . .
C11 C 0.3727(2) 0.65737(15) 0.00152(17) 0.0340(4) Uani 1 1 d . . .
H11A H 0.3506 0.5878 -0.0112 0.051 Uiso 1 1 calc R . .
H11B H 0.4373 0.6655 0.0728 0.051 Uiso 1 1 calc R . .
H11C H 0.4199 0.6827 -0.0583 0.051 Uiso 1 1 calc R . .
C12 C 0.1361(3) 0.70179(17) -0.10465(16) 0.0440(6) Uani 1 1 d . . .
H12A H 0.1853 0.7231 -0.1651 0.066 Uiso 1 1 calc R . .
H12B H 0.0500 0.7422 -0.1039 0.066 Uiso 1 1 calc R . .
H12C H 0.1073 0.6331 -0.1159 0.066 Uiso 1 1 calc R . .
C13 C 0.25068(17) 0.42777(11) 0.12403(14) 0.0197(3) Uani 1 1 d . . .
C14 C 0.49083(16) 0.44662(11) 0.51774(12) 0.0152(3) Uani 1 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 0.0033 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'
S S 0.1246 0.1234 '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
O1 Cu O2 85.21(5) . . ?
O1 Cu O3 158.81(5) . 3_666 ?
O1 Cu N1 95.94(5) . . ?
O1 Cu N3 100.05(5) . . ?
O2 Cu O3 82.21(4) . 3_666 ?
O2 Cu N1 167.79(5) . . ?
O2 Cu N3 97.51(5) . . ?
O3 Cu N1 92.89(5) 3_666 . ?
O3 Cu N3 98.46(5) 3_666 . ?
N1 Cu N3 94.26(5) . . ?
Cu O1 C1 125.64(10) . . ?
Cu O2 C14 112.68(10) . . ?
Cu O3 C14 111.62(10) 3_666 . ?
Cu N1 C7 122.09(11) . . ?
Cu N1 C8 120.08(10) . . ?
C7 N1 C8 117.83(13) . . ?
C10 N2 C11 112.99(14) . . ?
C10 N2 C12 109.68(16) . . ?
C11 N2 C12 110.51(15) . . ?
Cu N3 C13 160.14(13) . . ?
O1 C1 C2 119.27(14) . . ?
O1 C1 C6 124.00(14) . . ?
C2 C1 C6 116.72(15) . . ?
C1 C2 C3 121.66(16) . . ?
C2 C3 C4 121.94(16) . . ?
C3 C4 C5 117.92(16) . . ?
C4 C5 C6 122.07(16) . . ?
C1 C6 C5 119.59(15) . . ?
C1 C6 C7 123.74(15) . . ?
C5 C6 C7 116.57(15) . . ?
N1 C7 C6 127.39(15) . . ?
N1 C8 C9 113.13(12) . . ?
C8 C9 C10 111.72(13) . . ?
N2 C10 C9 111.99(14) . . ?
S C13 N3 179.06(17) . . ?
O2 C14 O3 126.86(14) . . ?
O2 C14 C14 116.00(16) . 3_666 ?
O3 C14 C14 117.15(17) . 3_666 ?
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
Cu O1 1.9134(11) . ?
Cu O2 2.0113(11) . ?
Cu O3 2.0338(11) 3_666 ?
Cu N1 1.9580(13) . ?
Cu N3 2.2158(14) . ?
S C13 1.6397(18) . ?
O1 C1 1.3103(19) . ?
O2 C14 1.2553(19) . ?
O3 Cu 2.0337(11) 3_666 ?
O3 C14 1.2469(19) . ?
N1 C7 1.288(2) . ?
N1 C8 1.4743(19) . ?
N2 C10 1.503(2) . ?
N2 C11 1.488(2) . ?
N2 C12 1.495(2) . ?
N3 C13 1.165(2) . ?
C1 C2 1.419(2) . ?
C1 C6 1.425(2) . ?
C2 C3 1.364(2) . ?
C3 C4 1.396(3) . ?
C4 C5 1.374(3) . ?
C5 C6 1.413(2) . ?
C6 C7 1.443(2) . ?
C8 C9 1.526(2) . ?
C9 C10 1.522(2) . ?
C14 C14 1.540(3) 3_666 ?
