#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/37/7103722.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_7103722
loop_
_publ_author_name
'Daofeng Sun'
'Rong Cao'
'Wenhua Bi'
'Daqiang Yuan'
'Qian Shi'
'Xing Li'
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/b302692b
_journal_year                    2003
_chemical_formula_moiety         '[Cu4(OH)2(SIPA)2(bipy)22H2O]n'
_chemical_formula_sum            'C9 H7 Cu N O4.5 S0.5'
_chemical_formula_weight         280.73
_chemical_name_systematic
;
?
;
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_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            8
_cell_length_a                   10.9368(10)
_cell_length_b                   16.2104(16)
_cell_length_c                   10.7803(10)
_cell_measurement_reflns_used    44
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.25
_cell_volume                     1911.2(3)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens XPREP'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0740
_diffrn_reflns_av_sigmaI/netI    0.0614
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5971
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.394
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  .8180
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'deep blue'
_exptl_crystal_density_diffrn    1.951
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .35
_exptl_crystal_size_min          .10
_refine_diff_density_max         1.022
_refine_diff_density_min         -1.072
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         1802
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_gt           0.0574
_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)+(0.0204P)²+16.0791P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1300
_reflns_number_gt                1111
_reflns_number_total             1802
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b302692b.txt
_cod_data_source_block           (1)
_cod_original_sg_symbol_H-M      Pnnm
_cod_original_formula_sum        'C9 H7 Cu N O4.50 S0.50'
_cod_database_code               7103722
#BEGIN Tags that were not found in dictionaries:
_refine_ls_r_factor_ref          0.1202
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-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
S S 0.2746(3) -0.09350(17) 0.0000 0.0401(8) Uani 1 2 d S . .
Cu1 Cu 0.49380(15) -0.31834(6) 0.5000 0.0261(3) Uani 1 2 d S . .
Cu2 Cu 0.5000 -0.5000 0.36457(10) 0.0325(4) Uani 1 2 d S . .
O1 O 0.1974(13) -0.0918(7) -0.0987(7) 0.195(7) Uani 1 1 d . . .
O2 O 0.3548(11) -0.0404(6) -0.0785(12) 0.050(3) Uani 0.50 1 d P . .
O3 O 0.4561(6) -0.3058(3) 0.3242(4) 0.0446(17) Uani 1 1 d . . .
O4 O 0.4414(5) -0.4296(3) 0.2332(4) 0.0388(14) Uani 1 1 d . . .
O5 O 0.4337(7) -0.4320(4) 0.5000 0.0255(16) Uani 1 2 d S . .
N1 N 0.5623(8) -0.2015(5) 0.5000 0.027(2) Uani 1 2 d S . .
N2 N 0.7942(9) 0.2085(6) 0.5000 0.043(3) Uani 1 2 d S . .
C1 C 0.4377(7) -0.3529(4) 0.2331(7) 0.0302(18) Uani 1 1 d . . .
C2 C 0.4125(7) -0.3116(4) 0.1115(6) 0.0245(17) Uani 1 1 d . . .
C3 C 0.3711(7) -0.2304(4) 0.1101(7) 0.0276(18) Uani 1 1 d . . .
H3 H 0.368(7) -0.204(4) 0.181(7) 0.04(2) Uiso 1 1 d . . .
C4 C 0.3478(10) -0.1904(5) 0.0000 0.023(2) Uani 1 2 d S . .
C5 C 0.4279(10) -0.3534(6) 0.0000 0.023(2) Uani 1 2 d S . .
H5 H 0.452(10) -0.409(7) 0.0000 0.05(3) Uiso 1 2 d S . .
C11 C 0.5855(9) -0.1609(5) 0.3951(8) 0.044(2) Uani 1 1 d . . .
H11 H 0.576(8) -0.186(5) 0.323(8) 0.05(3) Uiso 1 1 d . . .
C12 C 0.6314(9) -0.0819(5) 0.3923(8) 0.043(2) Uani 1 1 d . . .
H12 H 0.638(7) -0.056(4) 0.319(7) 0.04(2) Uiso 1 1 d . . .
C13 C 0.6557(11) -0.0384(6) 0.5000 0.031(3) Uani 1 2 d S . .
C14 C 0.7067(10) 0.0457(6) 0.5000 0.029(3) Uani 1 2 d S . .
C15 C 0.7319(9) 0.0867(5) 0.6091(8) 0.043(2) Uani 1 1 d . . .
H15 H 0.720(8) 0.061(5) 0.679(8) 0.05(3) Uiso 1 1 d . . .
C16 C 0.7745(9) 0.1670(5) 0.6035(9) 0.051(3) Uani 1 1 d . . .
H16 H 0.804(7) 0.195(5) 0.672(7) 0.04(2) Uiso 1 1 d . . .
O01 O 0.2034(11) -0.3794(6) 0.4491(12) 0.063(4) Uani 0.50 1 d P . .
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 S O1 103.1(11) . 6 ?
O1 S O2 143.0(8) . 6 ?
O1 S O2 84.8(8) 6 6 ?
O1 S O2 84.8(8) . . ?
O1 S O2 143.0(8) 6 . ?
O2 S O2 69.1(10) 6 . ?
O1 S C4 107.5(4) . . ?
O1 S C4 107.5(4) 6 . ?
O2 S C4 104.3(5) 6 . ?
O2 S C4 104.3(5) . . ?
O5 Cu1 O3 91.56(15) . . ?
O5 Cu1 O3 91.56(15) . 6_556 ?
O3 Cu1 O3 152.7(4) . 6_556 ?
O5 Cu1 N1 178.0(4) . . ?
O3 Cu1 N1 88.91(16) . . ?
O3 Cu1 N1 88.91(16) 6_556 . ?
O4 Cu2 O4 85.5(3) . 2_645 ?
O4 Cu2 O5 95.23(19) . . ?
O4 Cu2 O5 177.2(3) 2_645 . ?
O4 Cu2 O5 177.2(3) . 5_646 ?
O4 Cu2 O5 95.23(19) 2_645 5_646 ?
O5 Cu2 O5 84.2(3) . 5_646 ?
O4 Cu2 Cu2 137.26(15) . 5_646 ?
O4 Cu2 Cu2 137.26(15) 2_645 5_646 ?
O5 Cu2 Cu2 42.10(14) . 5_646 ?
O5 Cu2 Cu2 42.10(14) 5_646 5_646 ?
S O2 O2 55.4(5) . 6 ?
C1 O3 Cu1 136.7(5) . . ?
C1 O4 Cu2 127.1(5) . . ?
Cu1 O5 Cu2 113.8(3) . . ?
Cu1 O5 Cu2 113.8(3) . 5_646 ?
Cu2 O5 Cu2 95.8(3) . 5_646 ?
C11 N1 C11 116.0(9) 6_556 . ?
C11 N1 Cu1 122.0(5) 6_556 . ?
C11 N1 Cu1 122.0(5) . . ?
C16 N2 C16 115.3(11) 6_556 . ?
O4 C1 O3 126.9(7) . . ?
O4 C1 C2 117.0(6) . . ?
O3 C1 C2 116.1(6) . . ?
C5 C2 C3 119.4(7) . . ?
C5 C2 C1 121.1(6) . . ?
C3 C2 C1 119.5(6) . . ?
C4 C3 C2 121.0(7) . . ?
C3 C4 C3 119.1(9) 6 . ?
C3 C4 S 120.3(4) 6 . ?
C3 C4 S 120.3(4) . . ?
C2 C5 C2 119.7(9) 6 . ?
N1 C11 C12 123.3(8) . . ?
C11 C12 C13 121.8(8) . . ?
C12 C13 C12 113.9(10) . 6_556 ?
C12 C13 C14 123.0(5) . . ?
C12 C13 C14 123.0(5) 6_556 . ?
C15 C14 C15 117.1(10) . 6_556 ?
C15 C14 C13 121.5(5) . . ?
C15 C14 C13 121.5(5) 6_556 . ?
C14 C15 C16 119.0(9) . . ?
N2 C16 C15 124.8(9) . . ?
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
S O1 1.359(9) . ?
S O1 1.359(9) 6 ?
S O2 1.492(11) 6 ?
S O2 1.492(11) . ?
S C4 1.762(9) . ?
Cu1 O5 1.956(6) . ?
Cu1 O3 1.950(5) . ?
Cu1 O3 1.950(5) 6_556 ?
Cu1 N1 2.036(8) . ?
Cu2 O4 1.929(5) . ?
Cu2 O4 1.929(5) 2_645 ?
Cu2 O5 1.968(4) . ?
Cu2 O5 1.968(4) 5_646 ?
Cu2 Cu2 2.920(2) 5_646 ?
O2 O2 1.69(3) 6 ?
O3 C1 1.260(8) . ?
O4 C1 1.243(8) . ?
O5 Cu2 1.968(4) 5_646 ?
N1 C11 1.333(9) 6_556 ?
N1 C11 1.333(9) . ?
N2 C16 1.321(10) 6_556 ?
N2 C16 1.321(10) . ?
C1 C2 1.497(9) . ?
C2 C5 1.391(8) . ?
C2 C3 1.391(9) . ?
C3 C4 1.377(8) . ?
C4 C3 1.377(8) 6 ?
C5 C2 1.391(8) 6 ?
C11 C12 1.375(11) . ?
C12 C13 1.385(10) . ?
C13 C12 1.385(10) 6_556 ?
C13 C14 1.472(13) . ?
C14 C15 1.379(10) . ?
C14 C15 1.379(10) 6_556 ?
C15 C16 1.384(11) . ?
O01 O01 1.10(3) 6_556 ?
