#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:05:01 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179361 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/58/4325863.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_4325863
loop_
_publ_author_name
'Samit Majumder'
'Sohini Sarkar'
'Sujit Sasmal'
'E. Carolina Sañudo'
'Sasankasekhar Mohanta'
_publ_section_title
;
 Heterobridged Dinuclear, Tetranuclear, Dinuclear-Based 1-D, and
 Heptanuclear-Based 1-D Complexes of Copper(II) Derived from a
 Dinucleating Ligand: Syntheses, Structures, Magnetochemistry,
 Spectroscopy, and Catecholase Activity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7540
_journal_page_last               7554
_journal_paper_doi               10.1021/ic200409d
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C27 H25 Cu2 N7 O S3'
_chemical_formula_weight         686.80
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 91.7770(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4131(4)
_cell_length_b                   26.1746(8)
_cell_length_c                   8.7937(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2855.77(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'π and ω 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  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21254
_diffrn_reflns_theta_full        30.54
_diffrn_reflns_theta_max         30.54
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    1.744
_exptl_absorpt_correction_T_max  0.7923
_exptl_absorpt_correction_T_min  0.7002
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       Square
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.018(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         7262
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0307
_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)+(0.0000P)²+2.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0526
_reflns_number_gt                6170
_reflns_number_total             7262
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200409d_si_002_3.cif
_cod_data_source_block           3
_cod_database_code               4325863
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'
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
Cu1 Cu 0.47817(2) 0.109861(11) 0.45657(3) 0.01840(7) Uani 1 1 d .
Cu2 Cu 0.46445(2) 0.163145(11) 0.12204(3) 0.01783(7) Uani 1 1 d .
S3 S 0.30990(6) 0.11171(3) -0.33977(8) 0.02631(15) Uani 1 1 d .
S1 S 0.46528(6) 0.29044(3) 0.42305(11) 0.0407(2) Uani 1 1 d .
C1 C 0.30536(19) 0.08971(10) 0.2256(3) 0.0195(5) Uani 1 1 d .
C3 C 0.1361(2) 0.08182(11) 0.0798(3) 0.0266(6) Uani 1 1 d .
C10 C 0.2345(2) 0.16277(11) 0.0671(3) 0.0240(6) Uani 1 1 d .
C2 C 0.22678(19) 0.11045(10) 0.1225(3) 0.0207(5) Uani 1 1 d .
C11 C 0.5162(2) 0.00216(11) 0.5475(3) 0.0269(6) Uani 1 1 d .
C9 C 0.3648(2) 0.01550(11) 0.3857(3) 0.0212(6) Uani 1 1 d .
C24 C 0.6418(2) 0.23579(10) 0.0962(3) 0.0224(6) Uani 1 1 d .
C4 C 0.1198(2) 0.03250(11) 0.1304(4) 0.0290(6) Uani 1 1 d .
C5 C 0.1962(2) 0.01236(11) 0.2322(3) 0.0249(6) Uani 1 1 d .
C17 C 0.6343(2) 0.14520(10) 0.6911(3) 0.0202(5) Uani 1 1 d .
C13 C 0.6675(2) 0.06177(10) 0.6222(3) 0.0195(5) Uani 1 1 d .
C16 C 0.7201(2) 0.14565(12) 0.7942(3) 0.0258(6) Uani 1 1 d .
C12 C 0.6347(2) 0.01567(11) 0.5296(3) 0.0249(6) Uani 1 1 d .
C15 C 0.7808(2) 0.10156(11) 0.8126(3) 0.0270(6) Uani 1 1 d .
C21 C 0.5591(3) 0.29775(12) -0.1233(4) 0.0365(8) Uani 1 1 d .
C14 C 0.7540(2) 0.05964(11) 0.7251(3) 0.0241(6) Uani 1 1 d .
C6 C 0.2879(2) 0.04020(10) 0.2837(3) 0.0200(5) Uani 1 1 d .
C19 C 0.3828(3) 0.25091(13) -0.1163(4) 0.0328(7) Uani 1 1 d .
C20 C 0.4982(2) 0.25829(10) -0.0637(3) 0.0251(6) Uani 1 1 d .
C23 C 0.7050(2) 0.27423(12) 0.0408(3) 0.0286(6) Uani 1 1 d .
C18 C 0.3078(2) 0.24318(12) 0.0153(4) 0.0317(7) Uani 1 1 d .
N1 N 0.44799(17) 0.03584(8) 0.4519(2) 0.0208(5) Uani 1 1 d .
N4 N 0.31827(17) 0.19115(8) 0.0756(3) 0.0222(5) Uani 1 1 d .
N3 N 0.54044(17) 0.22702(8) 0.0444(2) 0.0199(4) Uani 1 1 d .
N6 N 0.60009(17) 0.12938(8) 0.1911(3) 0.0232(5) Uani 1 1 d .
N2 N 0.60749(16) 0.10433(8) 0.6047(2) 0.0180(5) Uani 1 1 d .
O1 O 0.39143(14) 0.11621(7) 0.2667(2) 0.0204(4) Uani 1 1 d .
N5 N 0.4870(2) 0.18463(8) 0.4498(3) 0.0250(5) Uani 1 1 d .
C25 C 0.4783(2) 0.22893(10) 0.4387(3) 0.0229(6) Uani 1 1 d .
C7 C 0.0202(2) 0.00263(12) 0.0761(5) 0.0430(9) Uani 1 1 d .
H7A H -0.0388 0.0114 0.1409 0.052 Uiso 1 1 calc R
H7B H 0.0005 0.0139 -0.0261 0.052 Uiso 1 1 calc R
C8 C 0.0313(3) -0.05432(13) 0.0744(5) 0.0394(8) Uani 1 1 d .
C22 C 0.6629(3) 0.30549(12) -0.0721(4) 0.0401(8) Uani 1 1 d .
H22 H 0.7043 0.3314 -0.1128 0.048 Uiso 1 1 calc R
N7 N 0.44974(18) 0.11696(9) -0.0852(3) 0.0257(5) Uani 1 1 d .
H17 H 0.584(2) 0.1730(10) 0.679(3) 0.017(7) Uiso 1 1 d .
H9 H 0.3513(19) -0.0188(10) 0.404(3) 0.009(6) Uiso 1 1 d .
C27 C 0.3922(2) 0.11465(10) -0.1920(3) 0.0195(5) Uani 1 1 d .
C26 C 0.6873(2) 0.11515(10) 0.2172(3) 0.0211(5) Uani 1 1 d .
S2 S 0.80989(6) 0.09598(3) 0.25619(9) 0.03038(17) Uani 1 1 d .
H12B H 0.682(2) -0.0146(11) 0.556(3) 0.026(7) Uiso 1 1 d .
H24 H 0.668(2) 0.2152(10) 0.182(3) 0.019(7) Uiso 1 1 d .
H3 H 0.088(3) 0.0974(12) 0.013(4) 0.034(9) Uiso 1 1 d .
H11A H 0.501(2) -0.0347(11) 0.524(3) 0.020(7) Uiso 1 1 d .
H11B H 0.5003(18) 0.0088(9) 0.656(3) 0.009(6) Uiso 1 1 d .
H12A H 0.651(2) 0.0219(10) 0.413(3) 0.023(7) Uiso 1 1 d .
H14 H 0.793(3) 0.0272(13) 0.728(4) 0.043(10) Uiso 1 1 d .
H16 H 0.732(2) 0.1748(11) 0.849(3) 0.022(8) Uiso 1 1 d .
H15 H 0.835(2) 0.1012(10) 0.884(3) 0.014(7) Uiso 1 1 d .
H5 H 0.196(2) -0.0188(13) 0.277(4) 0.036(9) Uiso 1 1 d .
H10 H 0.173(2) 0.1760(10) 0.029(3) 0.017(7) Uiso 1 1 d .
H18A H 0.230(3) 0.2469(11) -0.027(3) 0.036(9) Uiso 1 1 d .
H18B H 0.320(2) 0.2663(11) 0.097(3) 0.018(7) Uiso 1 1 d .
H23 H 0.775(2) 0.2800(11) 0.083(3) 0.029(8) Uiso 1 1 d .
H21 H 0.530(2) 0.3146(11) -0.192(4) 0.025(8) Uiso 1 1 d .
H19B H 0.385(2) 0.2196(12) -0.182(3) 0.031(8) Uiso 1 1 d .
H19A H 0.361(2) 0.2792(12) -0.173(3) 0.033(8) Uiso 1 1 d .
H8A H 0.038(3) -0.0657(14) 0.194(4) 0.057(11) Uiso 1 1 d .
H8B H -0.029(3) -0.0718(13) 0.044(4) 0.051(10) Uiso 1 1 d .
H8C H 0.090(3) -0.0616(15) 0.002(5) 0.068(12) Uiso 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'
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'
O O 0.0106 0.0060 '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
N5 Cu1 O1 85.38(9) . .
N5 Cu1 N1 171.80(10) . .
O1 Cu1 N1 88.09(8) . .
N5 Cu1 N2 92.68(9) . .
O1 Cu1 N2 161.36(7) . .
N1 Cu1 N2 95.09(9) . .
N5 Cu1 S3 92.62(8) . 1_556
O1 Cu1 S3 98.19(5) . 1_556
N1 Cu1 S3 83.41(6) . 1_556
N2 Cu1 S3 100.42(6) . 1_556
N5 Cu1 Cu2 63.02(7) . .
O1 Cu1 Cu2 35.33(5) . .
N1 Cu1 Cu2 113.40(6) . .
N2 Cu1 Cu2 128.71(6) . .
S3 Cu1 Cu2 123.553(18) 1_556 .
N5 Cu1 Cu2 78.57(7) . 1_556
O1 Cu1 Cu2 140.76(5) . 1_556
N1 Cu1 Cu2 103.68(6) . 1_556
N2 Cu1 Cu2 56.06(6) . 1_556
S3 Cu1 Cu2 47.850(15) 1_556 1_556
Cu2 Cu1 Cu2 140.941(11) . 1_556
N6 Cu2 N4 171.77(9) . .
N6 Cu2 O1 85.91(8) . .
N4 Cu2 O1 85.91(8) . .
N6 Cu2 N3 94.05(9) . .
N4 Cu2 N3 93.29(9) . .
O1 Cu2 N3 159.05(8) . .
N6 Cu2 N7 93.28(9) . .
N4 Cu2 N7 88.88(9) . .
O1 Cu2 N7 99.33(8) . .
N3 Cu2 N7 101.58(8) . .
N6 Cu2 Cu1 60.75(7) . .
N4 Cu2 Cu1 111.44(7) . .
O1 Cu2 Cu1 34.53(5) . .
N3 Cu2 Cu1 129.75(6) . .
N7 Cu2 Cu1 121.09(6) . .
C27 S3 Cu1 92.83(9) . 1_554
O1 C1 C6 121.1(2) . .
O1 C1 C2 120.7(2) . .
C6 C1 C2 118.2(2) . .
C4 C3 C2 122.7(3) . .
N4 C10 C2 126.0(3) . .
C3 C2 C1 120.0(3) . .
C3 C2 C10 118.4(2) . .
C1 C2 C10 121.4(2) . .
N1 C11 C12 110.0(2) . .
N1 C9 C6 127.1(3) . .
N3 C24 C23 122.9(3) . .
C3 C4 C5 117.2(3) . .
C3 C4 C7 120.2(3) . .
C5 C4 C7 122.5(3) . .
C4 C5 C6 122.6(3) . .
N2 C17 C16 123.4(3) . .
N2 C13 C14 121.6(2) . .
N2 C13 C12 117.5(2) . .
C14 C13 C12 120.9(2) . .
C17 C16 C15 118.5(3) . .
C13 C12 C11 112.1(2) . .
C14 C15 C16 118.6(3) . .
C22 C21 C20 120.2(3) . .
C15 C14 C13 120.2(3) . .
C1 C6 C5 119.2(2) . .
C1 C6 C9 122.1(2) . .
C5 C6 C9 118.6(2) . .
C20 C19 C18 112.5(3) . .
N3 C20 C21 120.8(3) . .
N3 C20 C19 119.0(2) . .
C21 C20 C19 120.2(3) . .
C24 C23 C22 118.8(3) . .
N4 C18 C19 110.4(3) . .
C9 N1 C11 116.8(2) . .
C9 N1 Cu1 124.44(19) . .
C11 N1 Cu1 118.15(17) . .
C10 N4 C18 117.1(2) . .
C10 N4 Cu2 122.24(19) . .
C18 N4 Cu2 119.17(17) . .
C24 N3 C20 118.3(2) . .
C24 N3 Cu2 117.55(18) . .
C20 N3 Cu2 123.90(17) . .
C26 N6 Cu2 169.3(2) . .
C13 N2 C17 117.8(2) . .
C13 N2 Cu1 123.59(17) . .
C17 N2 Cu1 118.61(17) . .
C1 O1 Cu1 127.45(16) . .
C1 O1 Cu2 121.88(16) . .
Cu1 O1 Cu2 110.13(8) . .
C25 N5 Cu1 171.1(2) . .
N5 C25 S1 179.5(3) . .
C8 C7 C4 116.1(3) . .
C21 C22 C23 118.9(3) . .
C27 N7 Cu2 137.2(2) . .
N7 C27 S3 179.0(3) . .
N6 C26 S2 178.9(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N5 1.961(2) .
Cu1 O1 1.9654(18) .
Cu1 N1 1.974(2) .
Cu1 N2 2.041(2) .
Cu1 S3 2.7936(8) 1_556
Cu1 Cu2 3.2553(4) .
Cu1 Cu2 6.0234(5) 1_556
Cu2 N6 1.980(2) .
Cu2 N4 1.988(2) .
Cu2 O1 2.0052(17) .
Cu2 N3 2.047(2) .
Cu2 N7 2.190(2) .
S3 C27 1.630(3) .
S3 Cu1 2.7936(8) 1_554
S1 C25 1.624(3) .
C1 O1 1.315(3) .
C1 C6 1.412(4) .
C1 C2 1.419(3) .
C3 C4 1.382(4) .
C3 C2 1.394(4) .
C10 N4 1.278(3) .
C10 C2 1.458(4) .
C11 N1 1.468(3) .
C11 C12 1.526(4) .
C9 N1 1.285(3) .
C9 C6 1.442(4) .
C24 N3 1.345(3) .
C24 C23 1.374(4) .
C4 C5 1.388(4) .
C4 C7 1.526(4) .
C5 C6 1.415(4) .
C17 N2 1.348(3) .
C17 C16 1.377(4) .
C13 N2 1.346(3) .
C13 C14 1.383(4) .
C13 C12 1.505(4) .
C16 C15 1.385(4) .
C15 C14 1.375(4) .
C21 C22 1.366(4) .
C21 C20 1.392(4) .
C19 C20 1.504(4) .
C19 C18 1.521(5) .
C20 N3 1.348(3) .
C23 C22 1.378(4) .
C18 N4 1.466(4) .
N6 C26 1.161(3) .
N5 C25 1.168(3) .
C7 C8 1.497(5) .
N7 C27 1.163(3) .
C26 S2 1.629(3) .
