#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/19/7011940.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_7011940
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            'C24 H36 Cl2 Cu N4 O10'
_chemical_formula_weight         675.01
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 109.698(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3004(9)
_cell_length_b                   23.5227(17)
_cell_length_c                   9.6924(7)
_cell_measurement_reflns_used    6593
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.48
_cell_measurement_theta_min      2.37
_cell_volume                     2854.9(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 0.994
_diffrn_measured_fraction_theta_max 0.898
_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  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0861
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17498
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.77
_diffrn_reflns_theta_min         1.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.014
_exptl_absorpt_correction_T_max  0.720
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         6673
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0469
_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)+(0.0432P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.1017
_reflns_number_gt                4229
_reflns_number_total             6673
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b206076k.txt
_cod_data_source_block           jad05
_cod_original_cell_volume        2854.9(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7011940
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.29266(3) 0.253616(14) 0.22830(4) 0.01973(11) Uani 1 1 d . . .
O1 O 0.41762(15) 0.22460(8) 0.3700(2) 0.0245(5) Uani 1 1 d . . .
O2 O 0.18144(16) 0.28053(8) 0.0616(2) 0.0331(5) Uani 1 1 d . . .
N1 N 0.22262(17) 0.17760(9) 0.1985(2) 0.0183(5) Uani 1 1 d . . .
N2 N -0.04948(18) 0.11221(9) -0.1843(3) 0.0212(5) Uani 1 1 d . . .
H2 H -0.0782 0.1206 -0.1115 0.025 Uiso 1 1 calc R . .
N3 N 0.34862(18) 0.33221(9) 0.2808(2) 0.0188(5) Uani 1 1 d . . .
N4 N 0.62539(18) 0.37571(9) 0.6892(3) 0.0220(6) Uani 1 1 d . . .
H4 H 0.6369 0.3837 0.6018 0.026 Uiso 1 1 calc R . .
C1 C 0.4362(2) 0.17475(12) 0.4334(3) 0.0210(7) Uani 1 1 d . . .
C2 C 0.5327(2) 0.16605(12) 0.5505(3) 0.0253(7) Uani 1 1 d . . .
H2A H 0.5823 0.1964 0.5815 0.030 Uiso 1 1 calc R . .
C3 C 0.5559(2) 0.11434(12) 0.6205(3) 0.0270(7) Uani 1 1 d . . .
H3 H 0.6204 0.1099 0.7008 0.032 Uiso 1 1 calc R . .
C4 C 0.4863(2) 0.06814(13) 0.5755(3) 0.0280(7) Uani 1 1 d . . .
H4A H 0.5035 0.0324 0.6235 0.034 Uiso 1 1 calc R . .
C5 C 0.3930(2) 0.07532(12) 0.4611(3) 0.0265(7) Uani 1 1 d . . .
H5 H 0.3458 0.0440 0.4297 0.032 Uiso 1 1 calc R . .
C6 C 0.3649(2) 0.12810(12) 0.3880(3) 0.0216(7) Uani 1 1 d . . .
C7 C 0.2631(2) 0.13282(12) 0.2737(3) 0.0223(7) Uani 1 1 d . . .
H7 H 0.2208 0.0993 0.2510 0.027 Uiso 1 1 calc R . .
C8 C 0.1160(2) 0.17014(12) 0.0852(3) 0.0228(7) Uani 1 1 d . . .
H8A H 0.0711 0.2038 0.0839 0.027 Uiso 1 1 calc R . .
H8B H 0.0804 0.1363 0.1085 0.027 Uiso 1 1 calc R . .
C9 C 0.1282(2) 0.16266(12) -0.0645(3) 0.0226(7) Uani 1 1 d . . .
H9A H 0.1713 0.1946 -0.0811 0.027 Uiso 1 1 calc R . .
H9B H 0.1682 0.1271 -0.0638 0.027 Uiso 1 1 calc R . .
C10 C 0.0234(2) 0.16035(12) -0.1913(3) 0.0242(7) Uani 1 1 d . . .
H10A H -0.0149 0.1967 -0.1947 0.029 Uiso 1 1 calc R . .
H10B H 0.0393 0.1571 -0.2837 0.029 Uiso 1 1 calc R . .
C11 C 0.0065(2) 0.05658(11) -0.1480(4) 0.0320(8) Uani 1 1 d . . .
H11A H 0.0485 0.0501 -0.2124 0.048 Uiso 1 1 calc R . .
H11B H -0.0462 0.0261 -0.1621 0.048 Uiso 1 1 calc R . .
H11C H 0.0540 0.0569 -0.0457 0.048 Uiso 1 1 calc R . .
C12 C -0.1391(2) 0.10841(13) -0.3263(3) 0.0322(8) Uani 1 1 d . . .
H12A H -0.1761 0.1451 -0.3481 0.048 Uiso 1 1 calc R . .
H12B H -0.1894 0.0789 -0.3198 0.048 Uiso 1 1 calc R . .
H12C H -0.1109 0.0987 -0.4046 0.048 Uiso 1 1 calc R . .
C13 C 0.1466(2) 0.33213(12) 0.0256(3) 0.0231(7) Uani 1 1 d . . .
C14 C 0.0527(2) 0.34017(13) -0.0966(3) 0.0251(7) Uani 1 1 d . . .
H14 H 0.0165 0.3080 -0.1497 0.030 Uiso 1 1 calc R . .
C15 C 0.0130(2) 0.39343(13) -0.1398(3) 0.0279(7) Uani 1 1 d . . .
H15 H -0.0494 0.3976 -0.2236 0.033 Uiso 1 1 calc R . .
C16 C 0.0623(3) 0.44152(13) -0.0632(3) 0.0323(8) Uani 1 1 d . . .
H16 H 0.0336 0.4783 -0.0927 0.039 Uiso 1 1 calc R . .
C17 C 0.1544(3) 0.43473(12) 0.0571(3) 0.0283(7) Uani 1 1 d . . .
H17 H 0.1886 0.4674 0.1101 0.034 Uiso 1 1 calc R . .
C18 C 0.1982(2) 0.38083(12) 0.1023(3) 0.0200(7) Uani 1 1 d . . .
C19 C 0.2980(2) 0.37771(12) 0.2207(3) 0.0219(7) Uani 1 1 d . . .
H19 H 0.3305 0.4129 0.2592 0.026 Uiso 1 1 calc R . .
C20 C 0.4536(2) 0.34112(12) 0.3970(3) 0.0228(7) Uani 1 1 d . . .
H20A H 0.4779 0.3806 0.3916 0.027 Uiso 1 1 calc R . .
H20B H 0.5069 0.3150 0.3809 0.027 Uiso 1 1 calc R . .
C21 C 0.4461(2) 0.33052(12) 0.5478(3) 0.0227(7) Uani 1 1 d . . .
H21A H 0.4037 0.2956 0.5445 0.027 Uiso 1 1 calc R . .
H21B H 0.4080 0.3627 0.5740 0.027 Uiso 1 1 calc R . .
C22 C 0.5550(2) 0.32384(11) 0.6655(3) 0.0225(7) Uani 1 1 d . . .
H22A H 0.5445 0.3141 0.7591 0.027 Uiso 1 1 calc R . .
H22B H 0.5925 0.2916 0.6387 0.027 Uiso 1 1 calc R . .
C23 C 0.5762(2) 0.42689(12) 0.7317(3) 0.0320(8) Uani 1 1 d . . .
H23A H 0.5583 0.4184 0.8197 0.048 Uiso 1 1 calc R . .
H23B H 0.5111 0.4373 0.6514 0.048 Uiso 1 1 calc R . .
H23C H 0.6269 0.4586 0.7519 0.048 Uiso 1 1 calc R . .
C24 C 0.7306(2) 0.36252(14) 0.8021(3) 0.0349(8) Uani 1 1 d . . .
H24A H 0.7780 0.3955 0.8150 0.052 Uiso 1 1 calc R . .
H24B H 0.7627 0.3297 0.7703 0.052 Uiso 1 1 calc R . .
H24C H 0.7204 0.3537 0.8953 0.052 Uiso 1 1 calc R . .
Cl1 Cl 0.80279(6) 0.29016(3) 0.46829(8) 0.02840(19) Uani 1 1 d . . .
O3 O 0.85474(18) 0.34409(9) 0.5175(2) 0.0417(6) Uani 1 1 d . . .
O4 O 0.7853(2) 0.28488(11) 0.3149(3) 0.0609(8) Uani 1 1 d . . .
O5 O 0.70515(19) 0.28787(13) 0.4931(3) 0.0713(9) Uani 1 1 d . . .
O6 O 0.8713(2) 0.24608(10) 0.5444(3) 0.0697(9) Uani 1 1 d . . .
Cl2 Cl 0.27347(6) -0.01369(3) 0.01245(8) 0.02595(18) Uani 1 1 d . . .
O7 O 0.20549(18) -0.02667(9) -0.1341(3) 0.0461(6) Uani 1 1 d . . .
O8 O 0.31182(19) 0.04308(9) 0.0161(3) 0.0524(7) Uani 1 1 d . . .
O9 O 0.36143(18) -0.05273(9) 0.0536(2) 0.0412(6) Uani 1 1 d . . .
O10 O 0.2165(2) -0.01816(11) 0.1120(3) 0.0581(8) 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'
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
O1 Cu O2 169.29(9) . . ?
O1 Cu N1 92.00(9) . . ?
O1 Cu N3 89.33(9) . . ?
O2 Cu N1 89.07(9) . . ?
O2 Cu N3 91.42(9) . . ?
N1 Cu N3 170.23(9) . . ?
Cu O1 C1 130.20(18) . . ?
Cu O2 C13 130.12(19) . . ?
Cu N1 C7 124.43(19) . . ?
Cu N1 C8 119.83(17) . . ?
C7 N1 C8 115.7(2) . . ?
C10 N2 C11 113.1(2) . . ?
C10 N2 C12 109.3(2) . . ?
C11 N2 C12 110.3(2) . . ?
Cu N3 C19 124.02(19) . . ?
Cu N3 C20 119.98(18) . . ?
C19 N3 C20 116.0(2) . . ?
C22 N4 C23 112.8(2) . . ?
C22 N4 C24 109.0(2) . . ?
C23 N4 C24 110.8(2) . . ?
O1 C1 C2 119.0(3) . . ?
O1 C1 C6 123.1(3) . . ?
C2 C1 C6 117.9(3) . . ?
C1 C2 C3 121.1(3) . . ?
C2 C3 C4 121.2(3) . . ?
C3 C4 C5 118.7(3) . . ?
C4 C5 C6 121.9(3) . . ?
C1 C6 C5 119.1(3) . . ?
C1 C6 C7 122.5(3) . . ?
C5 C6 C7 118.4(3) . . ?
N1 C7 C6 127.1(3) . . ?
N1 C8 C9 109.7(2) . . ?
C8 C9 C10 114.3(2) . . ?
N2 C10 C9 114.8(2) . . ?
O2 C13 C14 118.9(3) . . ?
O2 C13 C18 123.2(3) . . ?
C14 C13 C18 117.9(3) . . ?
C13 C14 C15 121.3(3) . . ?
C14 C15 C16 121.1(3) . . ?
C15 C16 C17 118.7(3) . . ?
C16 C17 C18 121.6(3) . . ?
C13 C18 C17 119.4(3) . . ?
C13 C18 C19 122.3(3) . . ?
C17 C18 C19 118.1(3) . . ?
N3 C19 C18 127.1(3) . . ?
N3 C20 C21 111.0(2) . . ?
C20 C21 C22 112.6(2) . . ?
N4 C22 C21 114.6(2) . . ?
O3 Cl1 O4 108.14(14) . . ?
O3 Cl1 O5 110.16(16) . . ?
O3 Cl1 O6 108.62(16) . . ?
O4 Cl1 O5 109.88(18) . . ?
O4 Cl1 O6 109.23(18) . . ?
O5 Cl1 O6 110.76(17) . . ?
O7 Cl2 O8 108.94(15) . . ?
O7 Cl2 O9 108.77(13) . . ?
O7 Cl2 O10 110.77(16) . . ?
O8 Cl2 O9 109.96(14) . . ?
O8 Cl2 O10 108.74(16) . . ?
O9 Cl2 O10 109.65(14) . . ?
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 1.8908(19) . ?
Cu O2 1.895(2) . ?
Cu N1 1.992(2) . ?
Cu N3 1.994(2) . ?
O1 C1 1.309(3) . ?
O2 C13 1.304(3) . ?
N1 C7 1.291(3) . ?
N1 C8 1.482(3) . ?
N2 C10 1.507(3) . ?
N2 C11 1.488(3) . ?
N2 C12 1.490(3) . ?
N3 C19 1.294(3) . ?
N3 C20 1.484(3) . ?
N4 C22 1.508(3) . ?
N4 C23 1.493(3) . ?
N4 C24 1.490(3) . ?
C1 C2 1.412(4) . ?
C1 C6 1.420(4) . ?
C2 C3 1.376(4) . ?
C3 C4 1.399(4) . ?
C4 C5 1.367(4) . ?
C5 C6 1.416(4) . ?
C6 C7 1.436(4) . ?
C8 C9 1.524(4) . ?
C9 C10 1.517(4) . ?
C13 C14 1.414(4) . ?
C13 C18 1.412(4) . ?
C14 C15 1.369(4) . ?
C15 C16 1.390(4) . ?
C16 C17 1.386(4) . ?
C17 C18 1.403(4) . ?
C18 C19 1.434(4) . ?
C20 C21 1.518(4) . ?
C21 C22 1.520(4) . ?
Cl1 O3 1.447(2) . ?
Cl1 O4 1.431(2) . ?
Cl1 O5 1.399(2) . ?
Cl1 O6 1.413(2) . ?
Cl2 O7 1.436(2) . ?
Cl2 O8 1.426(2) . ?
Cl2 O9 1.434(2) . ?
Cl2 O10 1.418(2) . ?
