#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:51:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179211 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/41/4314156.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_4314156
loop_
_publ_author_name
'Ke-liang Pang'
'Dong Guo'
'Chun-ying Duan'
'Hong Mo'
'Qing-jin Meng'
_publ_contact_author_address
;
Coordination Chemistry Institute
The State Key Laboratory of Coordinaiton Chemistry
Nanjing University , Nanjing 210093
P. R. China
;
_publ_contact_author_email       duancy@nju.edu.cn
_publ_contact_author_fax         '00 86 25 331 4502'
_publ_contact_author_name        'Dr. Duan Chun-ying'
_publ_contact_author_phone       '00 86 25 359 7006'
_publ_section_title
;
 Generation of an Equilibrating Collection of Crystalline Solids from a
 Dynamic Combinational Library
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5453
_journal_page_last               5455
_journal_paper_doi               10.1021/ic034176o
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C12 H13 Cu N O4 S'
_chemical_formula_weight         330.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 93.673(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.175(7)
_cell_length_b                   7.431(4)
_cell_length_c                   14.542(16)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      9.81
_cell_measurement_theta_min      5.19
_cell_volume                     2499(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2θ/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  0.1384
_diffrn_reflns_av_sigmaI/netI    0.1297
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5133
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        11.70_
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.923
_exptl_absorpt_correction_T_max  0.5002
_exptl_absorpt_correction_T_min  0.4295
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.153
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0689
_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)+(0.0689P)²+12.8504P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1739
_refine_ls_wR_factor_ref         0.1906
_reflns_number_gt                1633
_reflns_number_total             2212
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034176osi20030417_050415_2.cif
_cod_data_source_block           compound_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4314156
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'
'-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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.73450(3) 0.79258(13) 0.59643(5) 0.0353(3) Uani 1 1 d . . .
S1 S 0.55805(8) 0.8144(4) 0.68679(14) 0.0656(8) Uani 1 1 d . . .
O1 O 0.69942(16) 0.6893(6) 0.4804(3) 0.0311(10) Uani 1 1 d . . .
O2 O 0.75432(18) 0.9412(7) 0.7075(3) 0.0413(12) Uani 1 1 d . . .
O3 O 0.7212(2) 1.0251(8) 0.8416(3) 0.0489(14) Uani 1 1 d . . .
N1 N 0.6630(2) 0.7676(8) 0.6525(4) 0.0350(13) Uani 1 1 d . . .
C1 C 0.6434(3) 0.6860(9) 0.4553(4) 0.0322(15) Uani 1 1 d . . .
C2 C 0.6252(3) 0.6393(11) 0.3658(5) 0.0429(17) Uani 1 1 d . . .
H2A H 0.6529 0.6137 0.3242 0.051 Uiso 1 1 calc R . .
C3 C 0.5685(3) 0.6297(13) 0.3368(5) 0.055(2) Uani 1 1 d . . .
H3A H 0.5582 0.5954 0.2765 0.066 Uiso 1 1 calc R . .
C4 C 0.5265(3) 0.6696(16) 0.3949(6) 0.073(3) Uani 1 1 d . . .
H4A H 0.4878 0.6668 0.3739 0.088 Uiso 1 1 calc R . .
C5 C 0.5419(3) 0.7140(14) 0.4845(5) 0.062(3) Uani 1 1 d . . .
H5A H 0.5130 0.7385 0.5244 0.074 Uiso 1 1 calc R . .
C6 C 0.6008(3) 0.7237(11) 0.5182(5) 0.0383(16) Uani 1 1 d . . .
C7 C 0.6132(3) 0.7661(10) 0.6139(5) 0.0358(16) Uani 1 1 d . . .
C8 C 0.6097(3) 0.8800(15) 0.7784(5) 0.059(2) Uani 1 1 d . . .
H8A H 0.6108 1.0100 0.7848 0.070 Uiso 1 1 calc R . .
H8B H 0.5998 0.8278 0.8365 0.070 Uiso 1 1 calc R . .
C9 C 0.6675(3) 0.8096(10) 0.7512(4) 0.0369(16) Uani 1 1 d . . .
H9A H 0.6762 0.6982 0.7854 0.044 Uiso 1 1 calc R . .
C10 C 0.7182(3) 0.9384(10) 0.7681(4) 0.0339(15) Uani 1 1 d . . .
O4 O 0.6904(5) 1.0733(12) 0.5176(6) 0.130(4) Uani 1 1 d . . .
H4B H 0.6971 1.0661 0.4630 0.156 Uiso 1 1 d R . .
C11 C 0.6682(9) 1.2343(18) 0.5340(11) 0.132(7) Uani 1 1 d . . .
H11A H 0.6990 1.3209 0.5270 0.158 Uiso 1 1 calc R . .
H11B H 0.6392 1.2575 0.4844 0.158 Uiso 1 1 calc R . .
C12 C 0.6450(8) 1.275(2) 0.6092(13) 0.132(6) Uani 1 1 d . . .
H12A H 0.6409 1.4035 0.6131 0.198 Uiso 1 1 calc R . .
H12B H 0.6692 1.2331 0.6608 0.198 Uiso 1 1 calc R . .
H12C H 0.6077 1.2196 0.6098 0.198 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'
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
N1 Cu1 O1 170.50(19) . 7_666 ?
N1 Cu1 O1 90.3(2) . . ?
O1 Cu1 O1 80.43(18) 7_666 . ?
N1 Cu1 O2 82.4(2) . . ?
O1 Cu1 O2 106.10(18) 7_666 . ?
O1 Cu1 O2 165.79(19) . . ?
N1 Cu1 O3 97.0(2) . 4_646 ?
O1 Cu1 O3 86.55(18) 7_666 4_646 ?
O1 Cu1 O3 98.17(19) . 4_646 ?
O2 Cu1 O3 94.8(2) . 4_646 ?
N1 Cu1 Cu1 130.23(17) . 7_666 ?
O1 Cu1 Cu1 40.49(12) 7_666 7_666 ?
O1 Cu1 Cu1 39.95(12) . 7_666 ?
O2 Cu1 Cu1 144.97(14) . 7_666 ?
O3 Cu1 Cu1 93.12(13) 4_646 7_666 ?
C7 S1 C8 91.6(3) . . ?
C1 O1 Cu1 129.2(4) . 7_666 ?
C1 O1 Cu1 125.7(4) . . ?
Cu1 O1 Cu1 99.57(18) 7_666 . ?
C10 O2 Cu1 115.6(4) . . ?
C10 O3 Cu1 138.9(4) . 4_656 ?
C7 N1 C9 116.5(5) . . ?
C7 N1 Cu1 127.8(5) . . ?
C9 N1 Cu1 112.9(4) . . ?
O1 C1 C2 119.8(6) . . ?
O1 C1 C6 121.9(6) . . ?
C2 C1 C6 118.3(6) . . ?
C3 C2 C1 122.4(6) . . ?
C3 C2 H2A 118.8 . . ?
C1 C2 H2A 118.8 . . ?
C2 C3 C4 120.8(7) . . ?
C2 C3 H3A 119.6 . . ?
C4 C3 H3A 119.6 . . ?
C3 C4 C5 119.4(7) . . ?
C3 C4 H4A 120.3 . . ?
C5 C4 H4A 120.3 . . ?
C4 C5 C6 121.6(7) . . ?
C4 C5 H5A 119.2 . . ?
C6 C5 H5A 119.2 . . ?
C1 C6 C5 117.5(6) . . ?
C1 C6 C7 124.4(6) . . ?
C5 C6 C7 118.1(6) . . ?
N1 C7 C6 123.8(6) . . ?
N1 C7 S1 114.6(5) . . ?
C6 C7 S1 121.6(5) . . ?
C9 C8 S1 105.7(5) . . ?
C9 C8 H8A 110.6 . . ?
S1 C8 H8A 110.6 . . ?
C9 C8 H8B 110.6 . . ?
S1 C8 H8B 110.6 . . ?
H8A C8 H8B 108.7 . . ?
N1 C9 C8 108.8(5) . . ?
N1 C9 C10 107.3(5) . . ?
C8 C9 C10 115.3(6) . . ?
N1 C9 H9A 108.4 . . ?
C8 C9 H9A 108.4 . . ?
C10 C9 H9A 108.4 . . ?
O3 C10 O2 126.3(6) . . ?
O3 C10 C9 117.6(5) . . ?
O2 C10 C9 116.1(6) . . ?
C11 O4 H4B 109.4 . . ?
C12 C11 O4 123.6(15) . . ?
C12 C11 H11A 106.4 . . ?
O4 C11 H11A 106.4 . . ?
C12 C11 H11B 106.4 . . ?
O4 C11 H11B 106.4 . . ?
H11A C11 H11B 106.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
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 1.902(5) . ?
Cu1 O1 1.958(4) 7_666 ?
Cu1 O1 1.980(4) . ?
Cu1 O2 1.986(5) . ?
Cu1 O3 2.388(5) 4_646 ?
Cu1 Cu1 3.007(3) 7_666 ?
S1 C7 1.749(6) . ?
S1 C8 1.801(8) . ?
O1 C1 1.327(7) . ?
O1 Cu1 1.958(4) 7_666 ?
O2 C10 1.254(7) . ?
O3 C10 1.245(8) . ?
O3 Cu1 2.388(5) 4_656 ?
N1 C7 1.251(8) . ?
N1 C9 1.467(8) . ?
C1 C2 1.386(9) . ?
C1 C6 1.415(9) . ?
C2 C3 1.356(9) . ?
C2 H2A 0.9300 . ?
C3 C4 1.362(11) . ?
C3 H3A 0.9300 . ?
C4 C5 1.368(11) . ?
C4 H4A 0.9300 . ?
C5 C6 1.424(9) . ?
C5 H5A 0.9300 . ?
C6 C7 1.438(9) . ?
C8 C9 1.513(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.524(9) . ?
C9 H9A 0.9800 . ?
O4 C11 1.330(14) . ?
O4 H4B 0.8201 . ?
C11 C12 1.284(19) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
