#------------------------------------------------------------------------------
#$Date: 2021-04-16 11:46:56 +0300 (Fri, 16 Apr 2021) $
#$Revision: 264242 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/17/4311756.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_4311756
loop_
_publ_author_name
'Zhiliang Liu'
'Zhengliang Lü'
'Deqing Zhang'
'Zonghui Jiang'
'Licun Li'
'Caiming Liu'
'Daoben Zhu'
_publ_section_title
;
 New Types of Heterospin Complexes from trans-Oxamido-Bridged Copper(II)
 Binuclear Units and Nitronyl Nitroxide Radicals: Crystal Structure and
 Magnetic Characterization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6620
_journal_page_last               6627
_journal_paper_doi               10.1021/ic049247d
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C30 H36 Cl2 Cu2 N10 O14'
_chemical_formula_weight         958.66
_chemical_name_systematic
; 
 ? 
;
_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                 102.06(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.896(3)
_cell_length_b                   10.915(2)
_cell_length_c                   12.452(2)
_cell_measurement_reflns_used    13350
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.21
_cell_measurement_theta_min      1.40
_cell_volume                     1979.9(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku RAXIS RAPID IP'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0930
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7420
_diffrn_reflns_theta_full        27.21
_diffrn_reflns_theta_max         27.21
_diffrn_reflns_theta_min         1.40
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.284
_exptl_absorpt_correction_T_max  1.1748
_exptl_absorpt_correction_T_min  0.7337
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            darkblue
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0435
_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)+(0.0410P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                2056
_reflns_number_total             4319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049247dsi20040610_073414_2.cif
_cod_data_source_block           2(complex2)
_cod_depositor_comments
;

2021-04-13
Formula fixed to be consistent with given Z value
                 miguel
;
_cod_original_formula_sum            'C15 H18 Cl Cu N5 O7'
_cod_original_formula_weight         479.33
_cod_original_cell_volume        1979.9(6)
_cod_database_code               4311756
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
Cu1 Cu 0.42235(3) 0.01298(5) 0.16792(4) 0.04746(19) Uani 1 1 d . . .
Cl1 Cl 0.61655(9) -0.18376(12) 0.44873(10) 0.0633(4) Uani 1 1 d . . .
C1 C 0.2917(3) -0.0568(4) 0.3028(3) 0.0522(12) Uani 1 1 d . . .
H1A H 0.3414 -0.0439 0.3607 0.063 Uiso 1 1 calc R . .
C2 C 0.2085(3) -0.0836(4) 0.3274(3) 0.0490(11) Uani 1 1 d . . .
H2A H 0.2025 -0.0875 0.4002 0.059 Uiso 1 1 calc R . .
C3 C 0.1337(3) -0.1046(3) 0.2438(3) 0.0369(9) Uani 1 1 d . . .
C4 C 0.1483(3) -0.1013(4) 0.1377(3) 0.0478(11) Uani 1 1 d . . .
H4A H 0.1004 -0.1177 0.0785 0.057 Uiso 1 1 calc R . .
C5 C 0.2339(3) -0.0736(4) 0.1205(3) 0.0498(11) Uani 1 1 d . . .
H5A H 0.2425 -0.0725 0.0486 0.060 Uiso 1 1 calc R . .
C6 C 0.0422(3) -0.1185(3) 0.2666(3) 0.0381(10) Uani 1 1 d . . .
C7 C -0.0771(3) -0.1690(4) 0.3557(3) 0.0446(10) Uani 1 1 d . . .
C8 C -0.1154(3) -0.0864(4) 0.2573(3) 0.0436(10) Uani 1 1 d . . .
C9 C -0.1012(3) -0.1322(4) 0.4633(3) 0.0636(13) Uani 1 1 d . . .
H11A H -0.0749 -0.1898 0.5193 0.095 Uiso 1 1 calc R . .
H11B H -0.1667 -0.1315 0.4552 0.095 Uiso 1 1 calc R . .
H11C H -0.0773 -0.0519 0.4837 0.095 Uiso 1 1 calc R . .
C10 C -0.0977(3) -0.3041(4) 0.3339(4) 0.0642(13) Uani 1 1 d . . .
H12A H -0.0715 -0.3507 0.3982 0.096 Uiso 1 1 calc R . .
H12B H -0.0717 -0.3306 0.2734 0.096 Uiso 1 1 calc R . .
H12C H -0.1630 -0.3164 0.3162 0.096 Uiso 1 1 calc R . .
C11 C -0.1236(3) 0.0485(4) 0.2872(4) 0.0645(13) Uani 1 1 d . . .
H13A H -0.1481 0.0946 0.2220 0.097 Uiso 1 1 calc R . .
H13B H -0.0641 0.0797 0.3206 0.097 Uiso 1 1 calc R . .
H13C H -0.1639 0.0559 0.3378 0.097 Uiso 1 1 calc R . .
C12 C -0.2019(3) -0.1306(4) 0.1822(4) 0.0611(13) Uani 1 1 d . . .
H14A H -0.2209 -0.0721 0.1243 0.092 Uiso 1 1 calc R . .
H14B H -0.2494 -0.1398 0.2232 0.092 Uiso 1 1 calc R . .
H14C H -0.1905 -0.2082 0.1511 0.092 Uiso 1 1 calc R . .
C13 C 0.5590(3) 0.1681(4) 0.2972(3) 0.0574(12) Uani 1 1 d . . .
H15A H 0.6018 0.1781 0.3669 0.069 Uiso 1 1 calc R . .
H15B H 0.5363 0.2484 0.2713 0.069 Uiso 1 1 calc R . .
C14 C 0.6072(3) 0.1098(4) 0.2149(3) 0.0589(13) Uani 1 1 d . . .
H16A H 0.6396 0.1714 0.1817 0.071 Uiso 1 1 calc R . .
H16B H 0.6512 0.0494 0.2507 0.071 Uiso 1 1 calc R . .
C15 C 0.5427(3) 0.0297(4) 0.0321(3) 0.0470(11) Uani 1 1 d . . .
N5 N 0.0238(2) -0.1556(3) 0.3630(3) 0.0436(8) Uani 1 1 d . . .
N4 N -0.0368(2) -0.0915(3) 0.1974(3) 0.0442(9) Uani 1 1 d . . .
N3 N 0.3056(2) -0.0482(3) 0.2013(3) 0.0437(8) Uani 1 1 d . . .
N2 N 0.4813(2) 0.0894(3) 0.3121(2) 0.0510(9) Uani 1 1 d . . .
H2B H 0.4397 0.1348 0.3374 0.061 Uiso 1 1 calc R . .
H2C H 0.5017 0.0305 0.3616 0.061 Uiso 1 1 calc R . .
N1 N 0.5375(2) 0.0519(3) 0.1321(3) 0.0488(9) Uani 1 1 d . . .
O7 O 0.6318(3) -0.2330(4) 0.5544(3) 0.1357(19) Uani 1 1 d . . .
O6 O 0.6653(3) -0.0724(4) 0.4501(4) 0.1161(15) Uani 1 1 d . . .
O5 O 0.6463(2) -0.2693(3) 0.3781(3) 0.0880(11) Uani 1 1 d . . .
O4 O 0.5212(2) -0.1592(3) 0.4170(3) 0.0856(11) Uani 1 1 d . . .
O3 O 0.08235(18) -0.1898(3) 0.4480(2) 0.0596(9) Uani 1 1 d . . .
O2 O -0.04654(19) -0.0551(3) 0.0991(2) 0.0636(9) Uani 1 1 d . . .
O1 O 0.60909(18) 0.0521(3) -0.0151(2) 0.0532(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
N1 Cu1 N3 173.15(14) . . ?
N1 Cu1 O1 84.24(12) . 3_655 ?
N3 Cu1 O1 92.20(12) . 3_655 ?
N1 Cu1 N2 82.54(13) . . ?
N3 Cu1 N2 101.01(13) . . ?
O1 Cu1 N2 166.76(11) 3_655 . ?
O7 Cl1 O6 109.8(3) . . ?
O7 Cl1 O5 108.7(2) . . ?
O6 Cl1 O5 110.3(2) . . ?
O7 Cl1 O4 107.0(2) . . ?
O6 Cl1 O4 108.8(2) . . ?
O5 Cl1 O4 112.1(2) . . ?
N3 C1 C2 123.8(4) . . ?
C1 C2 C3 119.6(3) . . ?
C2 C3 C4 117.0(3) . . ?
C2 C3 C6 120.8(3) . . ?
C4 C3 C6 121.9(4) . . ?
C5 C4 C3 119.5(4) . . ?
N3 C5 C4 123.5(4) . . ?
N4 C6 N5 108.9(3) . . ?
N4 C6 C3 125.7(3) . . ?
N5 C6 C3 125.3(3) . . ?
N5 C7 C9 110.0(3) . . ?
N5 C7 C10 105.6(3) . . ?
C9 C7 C10 109.9(3) . . ?
N5 C7 C8 101.1(3) . . ?
C9 C7 C8 115.8(4) . . ?
C10 C7 C8 113.6(3) . . ?
C12 C8 N4 109.4(3) . . ?
C12 C8 C11 111.0(3) . . ?
N4 C8 C11 105.4(3) . . ?
C12 C8 C7 115.8(3) . . ?
N4 C8 C7 100.1(3) . . ?
C11 C8 C7 114.0(3) . . ?
N2 C13 C14 109.6(3) . . ?
N1 C14 C13 107.2(3) . . ?
O1 C15 N1 128.3(4) . . ?
O1 C15 C15 119.4(4) . 3_655 ?
N1 C15 C15 112.3(4) . 3_655 ?
O3 N5 C6 126.4(3) . . ?
O3 N5 C7 121.7(3) . . ?
C6 N5 C7 111.4(3) . . ?
O2 N4 C6 126.8(3) . . ?
O2 N4 C8 121.3(3) . . ?
C6 N4 C8 110.9(3) . . ?
C1 N3 C5 116.4(3) . . ?
C1 N3 Cu1 122.7(3) . . ?
C5 N3 Cu1 120.7(3) . . ?
C13 N2 Cu1 109.6(2) . . ?
C15 N1 C14 126.3(3) . . ?
C15 N1 Cu1 115.1(3) . . ?
C14 N1 Cu1 118.5(2) . . ?
C15 O1 Cu1 108.8(2) . 3_655 ?
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 N1 1.908(3) . ?
Cu1 N3 1.986(3) . ?
Cu1 O1 1.994(3) 3_655 ?
Cu1 N2 2.008(3) . ?
Cl1 O7 1.396(4) . ?
Cl1 O6 1.415(4) . ?
Cl1 O5 1.415(3) . ?
Cl1 O4 1.419(3) . ?
C1 N3 1.327(5) . ?
C1 C2 1.369(5) . ?
C2 C3 1.375(5) . ?
C3 C4 1.384(5) . ?
C3 C6 1.457(5) . ?
C4 C5 1.369(5) . ?
C5 N3 1.335(5) . ?
C6 N4 1.339(4) . ?
C6 N5 1.348(4) . ?
C7 N5 1.494(5) . ?
C7 C9 1.512(5) . ?
C7 C10 1.519(5) . ?
C7 C8 1.533(5) . ?
C8 C12 1.504(5) . ?
C8 N4 1.515(5) . ?
C8 C11 1.530(5) . ?
C13 N2 1.484(5) . ?
C13 C14 1.509(5) . ?
C14 N1 1.446(5) . ?
C15 O1 1.274(4) . ?
C15 N1 1.287(5) . ?
C15 C15 1.502(8) 3_655 ?
N5 O3 1.279(4) . ?
N4 O2 1.266(4) . ?
O1 Cu1 1.994(3) 3_655 ?
