#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/19/7011942.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_7011942
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            'C26 H34 Cu2 N4 O6'
_chemical_formula_weight         625.65
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            4
_cell_length_a                   10.2160(10)
_cell_length_b                   10.9109(10)
_cell_length_c                   23.883(2)
_cell_measurement_reflns_used    8636
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      2.62
_cell_volume                     2662.1(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.940
_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  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            19991
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.65
_diffrn_reflns_theta_min         1.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.646
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.214
_refine_diff_density_min         -1.229
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         3217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0521
_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)+(0.0527P)²+6.2811P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1231
_reflns_number_gt                2312
_reflns_number_total             3217
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b206076k.txt
_cod_data_source_block           jad04
_cod_database_code               7011942
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
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 0.56064(4) 0.36028(4) 0.410185(19) 0.02432(15) Uani 1 1 d . . .
O1 O 0.5629(3) 0.3525(2) 0.50056(10) 0.0287(6) Uani 1 1 d . . .
C1 C 0.5252(3) 0.4501(3) 0.52105(15) 0.0234(7) Uani 1 1 d . . .
O2 O 0.5223(2) 0.4781(2) 0.57231(10) 0.0268(6) Uani 1 1 d . . .
O3 O 0.6444(2) 0.4370(2) 0.34746(10) 0.0210(5) Uani 1 1 d . . .
C2 C 0.7594(3) 0.4085(3) 0.32718(13) 0.0196(7) Uani 1 1 d . . .
C3 C 0.8185(4) 0.4870(3) 0.28716(13) 0.0234(7) Uani 1 1 d . . .
H3 H 0.7726 0.5579 0.2751 0.028 Uiso 1 1 calc R . .
C4 C 0.9408(4) 0.4630(3) 0.26528(15) 0.0282(8) Uani 1 1 d . . .
H4 H 0.9775 0.5171 0.2384 0.034 Uiso 1 1 calc R . .
C5 C 1.0113(4) 0.3598(4) 0.28236(15) 0.0298(8) Uani 1 1 d . . .
H5 H 1.0966 0.3449 0.2681 0.036 Uiso 1 1 calc R . .
C6 C 0.9554(3) 0.2799(3) 0.32019(15) 0.0258(8) Uani 1 1 d . . .
H6 H 1.0024 0.2089 0.3313 0.031 Uiso 1 1 calc R . .
C7 C 0.8300(3) 0.3016(3) 0.34268(13) 0.0186(7) Uani 1 1 d . . .
C8 C 0.7786(3) 0.2100(3) 0.37971(13) 0.0196(7) Uani 1 1 d . . .
H8 H 0.8300 0.1382 0.3848 0.023 Uiso 1 1 calc R . .
N1 N 0.6693(3) 0.2156(2) 0.40677(12) 0.0207(6) Uani 1 1 d . . .
C9 C 0.6309(3) 0.1096(3) 0.44099(15) 0.0233(7) Uani 1 1 d . . .
H9A H 0.6256 0.1348 0.4807 0.028 Uiso 1 1 calc R . .
H9B H 0.6989 0.0452 0.4379 0.028 Uiso 1 1 calc R . .
C10 C 0.4992(3) 0.0568(3) 0.42275(14) 0.0230(7) Uani 1 1 d . . .
H10A H 0.5038 0.0370 0.3823 0.028 Uiso 1 1 calc R . .
H10B H 0.4843 -0.0209 0.4432 0.028 Uiso 1 1 calc R . .
C11 C 0.3831(3) 0.1404(3) 0.43252(15) 0.0229(7) Uani 1 1 d . . .
H11A H 0.3018 0.0935 0.4254 0.028 Uiso 1 1 calc R . .
H11B H 0.3825 0.1654 0.4724 0.028 Uiso 1 1 calc R . .
N2 N 0.3817(3) 0.2523(3) 0.39725(12) 0.0211(6) Uani 1 1 d . . .
C12 C 0.2655(4) 0.3246(3) 0.41235(17) 0.0307(8) Uani 1 1 d . . .
H12A H 0.1867 0.2746 0.4072 0.046 Uiso 1 1 calc R . .
H12B H 0.2603 0.3972 0.3883 0.046 Uiso 1 1 calc R . .
H12C H 0.2719 0.3503 0.4516 0.046 Uiso 1 1 calc R . .
C13 C 0.3712(4) 0.2186(3) 0.33764(15) 0.0313(9) Uani 1 1 d . . .
H13A H 0.2956 0.1646 0.3323 0.047 Uiso 1 1 calc R . .
H13B H 0.4511 0.1760 0.3259 0.047 Uiso 1 1 calc R . .
H13C H 0.3600 0.2929 0.3151 0.047 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
O1 Cu O2 80.22(10) . 5_666 ?
O1 Cu O3 142.47(10) . . ?
O1 Cu N1 90.23(10) . . ?
O1 Cu N2 97.37(10) . . ?
O2 Cu O3 88.14(10) 5_666 . ?
O2 Cu N1 166.54(11) 5_666 . ?
O2 Cu N2 98.62(10) 5_666 . ?
O3 Cu N1 93.85(10) . . ?
O3 Cu N2 119.71(10) . . ?
N1 Cu N2 91.96(11) . . ?
Cu O1 C1 111.1(2) . . ?
O1 C1 C1 116.6(4) . 5_666 ?
O1 C1 O2 127.0(3) . . ?
C1 C1 O2 116.4(4) 5_666 . ?
Cu O2 C1 115.2(2) 5_666 . ?
Cu O3 C2 125.9(2) . . ?
O3 C2 C3 119.3(3) . . ?
O3 C2 C7 123.7(3) . . ?
C3 C2 C7 117.0(3) . . ?
C2 C3 C4 121.8(3) . . ?
C3 C4 C5 120.6(3) . . ?
C4 C5 C6 119.2(3) . . ?
C5 C6 C7 121.3(3) . . ?
C2 C7 C6 120.0(3) . . ?
C2 C7 C8 123.2(3) . . ?
C6 C7 C8 116.8(3) . . ?
C7 C8 N1 126.3(3) . . ?
Cu N1 C8 123.8(2) . . ?
Cu N1 C9 117.8(2) . . ?
C8 N1 C9 118.1(3) . . ?
N1 C9 C10 111.9(3) . . ?
C9 C10 C11 114.8(3) . . ?
C10 C11 N2 114.6(3) . . ?
Cu N2 C11 110.7(2) . . ?
Cu N2 C12 110.5(2) . . ?
Cu N2 C13 109.2(2) . . ?
C11 N2 C12 108.1(3) . . ?
C11 N2 C13 110.1(3) . . ?
C12 N2 C13 108.2(3) . . ?
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 2.160(3) . ?
Cu O2 2.001(2) 5_666 ?
Cu O3 1.917(2) . ?
Cu N1 1.932(3) . ?
Cu N2 2.197(3) . ?
O1 C1 1.233(4) . ?
C1 C1 1.569(7) 5_666 ?
C1 O2 1.262(4) . ?
O2 Cu 2.001(2) 5_666 ?
O3 C2 1.308(4) . ?
C2 C3 1.418(5) . ?
C2 C7 1.421(5) . ?
C3 C4 1.380(5) . ?
C4 C5 1.397(5) . ?
C5 C6 1.379(5) . ?
C6 C7 1.410(5) . ?
C7 C8 1.435(4) . ?
C8 N1 1.292(4) . ?
N1 C9 1.470(4) . ?
C9 C10 1.527(5) . ?
C10 C11 1.515(5) . ?
C11 N2 1.483(4) . ?
N2 C12 1.470(4) . ?
N2 C13 1.474(4) . ?
