#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:44:30 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180353 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/22/7202251.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_7202251
loop_
_publ_author_name
'He, Haiyan'
'Dai, Fangna'
'Xie, Aiping'
'Tong, Xin'
'Sun, Daofeng'
_publ_section_title
;
 Three novel 3D metal--organic frameworks with a 1D ladder, tube or
 chain as assembly units
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1429
_journal_paper_doi               10.1039/b808373h
_journal_volume                  10
_journal_year                    2008
_chemical_formula_sum            'C38 H26 Cu4 N4 O18 S'
_chemical_formula_weight         1112.85
_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                 126.7420(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   33.5656(8)
_cell_length_b                   6.6676(2)
_cell_length_c                   21.2236(5)
_cell_measurement_reflns_used    3264
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.65
_cell_measurement_theta_min      2.50
_cell_volume                     3806.26(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_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  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12823
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    2.351
_exptl_absorpt_correction_T_max  0.8915
_exptl_absorpt_correction_T_min  0.7989
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.295
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         2738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0606
_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)+(0.1023P)²+23.1305P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1718
_reflns_number_gt                2108
_reflns_number_total             2738
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b808373h.txt
_cod_data_source_block           080418c
_cod_original_cell_volume        3806.26(17)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7202251
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
S S 1.0000 0.9738(4) 0.7500 0.0271(7) Uani 1 2 d S . .
Cu1 Cu 0.89735(3) 0.65965(14) 0.64687(5) 0.0232(3) Uani 1 1 d . . .
Cu2 Cu 1.00132(3) 0.51301(14) 0.81957(5) 0.0200(3) Uani 1 1 d . . .
O1 O 0.8841(2) 0.6532(9) 0.7244(3) 0.0351(16) Uani 1 1 d . . .
O2 O 0.95322(19) 0.5546(10) 0.8394(3) 0.0358(16) Uani 1 1 d . . .
O3 O 0.95108(19) 0.5176(8) 1.0688(3) 0.0267(14) Uani 1 1 d . . .
O4 O 0.87856(19) 0.4384(9) 1.0458(3) 0.0288(14) Uani 1 1 d . . .
O5 O 0.7224(2) 0.5927(12) 0.7855(3) 0.0512(19) Uani 1 1 d . . .
O6 O 0.7249(2) 0.5857(10) 0.6827(3) 0.0358(15) Uani 1 1 d . . .
O7 O 0.95150(17) 0.4680(7) 0.7054(3) 0.0162(12) Uani 1 1 d . . .
O8 O 0.9664(2) 0.8439(8) 0.6805(3) 0.0375(15) Uani 1 1 d . . .
O9 O 0.9707(3) 1.0966(9) 0.7647(4) 0.0454(17) Uani 1 1 d . . .
C1 C 0.8793(3) 0.5857(12) 0.8282(4) 0.0193(17) Uani 1 1 d . . .
C2 C 0.9046(3) 0.5530(11) 0.9090(4) 0.0181(17) Uani 1 1 d . . .
H2 H 0.9391 0.5430 0.9422 0.022 Uiso 1 1 calc R . .
C3 C 0.8776(3) 0.5356(11) 0.9389(4) 0.0203(18) Uani 1 1 d . . .
C4 C 0.8261(3) 0.5542(12) 0.8890(4) 0.0218(18) Uani 1 1 d . . .
H4 H 0.8083 0.5464 0.9095 0.026 Uiso 1 1 calc R . .
C5 C 0.8015(3) 0.5836(12) 0.8101(4) 0.0230(18) Uani 1 1 d . . .
C6 C 0.8278(3) 0.6004(12) 0.7796(4) 0.0232(18) Uani 1 1 d . . .
H6 H 0.8110 0.6219 0.7260 0.028 Uiso 1 1 calc R . .
C7 C 0.9087(3) 0.6000(12) 0.7958(4) 0.0259(19) Uani 1 1 d . . .
C8 C 0.9045(3) 0.4976(11) 1.0246(4) 0.0182(18) Uani 1 1 d . . .
C9 C 0.7452(3) 0.5902(13) 0.7582(5) 0.032(2) Uani 1 1 d . . .
C10 C 0.8433(4) 1.0244(15) 0.6325(5) 0.056(3) Uani 1 1 d . . .
H10 H 0.8678 1.0280 0.6865 0.067 Uiso 1 1 calc R . .
C11 C 0.8077(4) 1.1693(16) 0.5994(5) 0.063(4) Uani 1 1 d . . .
H11 H 0.8086 1.2680 0.6312 0.075 Uiso 1 1 calc R . .
C12 C 0.7699(3) 1.1729(13) 0.5190(5) 0.035(2) Uani 1 1 d . . .
C13 C 0.7721(4) 1.0225(16) 0.4761(5) 0.058(3) Uani 1 1 d . . .
H13 H 0.7486 1.0189 0.4217 0.070 Uiso 1 1 calc R . .
C14 C 0.8083(4) 0.8799(16) 0.5131(5) 0.052(3) Uani 1 1 d . . .
H14 H 0.8076 0.7788 0.4823 0.062 Uiso 1 1 calc R . .
C15 C 0.8905(3) 0.0709(14) 0.8605(5) 0.037(2) Uani 1 1 d . . .
H15 H 0.8697 0.0959 0.8067 0.045 Uiso 1 1 calc R . .
C16 C 0.9415(3) 0.0508(14) 0.8976(5) 0.039(2) Uani 1 1 d . . .
H16 H 0.9543 0.0626 0.8693 0.047 Uiso 1 1 calc R . .
C17 C 0.9727(3) 0.0125(11) 0.9785(4) 0.0225(18) Uani 1 1 d . . .
C18 C 0.9510(3) 0.0026(13) 1.0171(5) 0.032(2) Uani 1 1 d . . .
H18 H 0.9708 -0.0165 1.0713 0.039 Uiso 1 1 calc R . .
C19 C 0.9003(3) 0.0207(13) 0.9758(5) 0.036(2) Uani 1 1 d . . .
H19 H 0.8864 0.0080 1.0027 0.044 Uiso 1 1 calc R . .
N1 N 0.8448(3) 0.8747(11) 0.5906(4) 0.0342(18) Uani 1 1 d . . .
N2 N 0.8702(2) 0.0559(11) 0.8984(4) 0.0333(17) 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'
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
O9 S O9 111.2(5) 2_756 . ?
O9 S O8 109.0(3) 2_756 . ?
O9 S O8 109.4(4) . . ?
O9 S O8 109.4(4) 2_756 2_756 ?
O9 S O8 109.0(3) . 2_756 ?
O8 S O8 108.7(5) . 2_756 ?
O7 Cu1 O1 92.6(2) . . ?
O7 Cu1 O4 92.6(2) . 6_565 ?
O1 Cu1 O4 146.7(3) . 6_565 ?
O7 Cu1 N1 175.8(3) . . ?
O1 Cu1 N1 87.4(2) . . ?
O4 Cu1 N1 89.7(2) 6_565 . ?
O7 Cu1 O8 76.8(2) . . ?
O1 Cu1 O8 116.3(2) . . ?
O4 Cu1 O8 97.0(2) 6_565 . ?
N1 Cu1 O8 99.4(3) . . ?
O2 Cu2 O3 86.2(2) . 5_767 ?
O2 Cu2 O7 177.6(2) . 2_756 ?
O3 Cu2 O7 96.1(2) 5_767 2_756 ?
O2 Cu2 O7 94.9(2) . . ?
O3 Cu2 O7 165.1(2) 5_767 . ?
O7 Cu2 O7 82.7(2) 2_756 . ?
O2 Cu2 Cu2 134.96(16) . 2_756 ?
O3 Cu2 Cu2 138.87(16) 5_767 2_756 ?
O7 Cu2 Cu2 42.80(13) 2_756 2_756 ?
O7 Cu2 Cu2 42.61(14) . 2_756 ?
C7 O1 Cu1 134.6(5) . . ?
C7 O2 Cu2 132.2(5) . . ?
C8 O3 Cu2 130.8(5) . 5_767 ?
C8 O4 Cu1 131.3(5) . 6_566 ?
Cu1 O7 Cu2 108.8(2) . 2_756 ?
Cu1 O7 Cu2 117.7(2) . . ?
Cu2 O7 Cu2 94.6(2) 2_756 . ?
S O8 Cu1 129.7(3) . . ?
C6 C1 C2 119.5(7) . . ?
C6 C1 C7 121.4(7) . . ?
C2 C1 C7 119.1(7) . . ?
C3 C2 C1 119.2(7) . . ?
C2 C3 C4 119.9(7) . . ?
C2 C3 C8 119.2(7) . . ?
C4 C3 C8 120.9(7) . . ?
C5 C4 C3 120.7(7) . . ?
C4 C5 C6 119.9(7) . . ?
C4 C5 C9 118.1(7) . . ?
C6 C5 C9 121.9(7) . . ?
C5 C6 C1 120.6(7) . . ?
O2 C7 O1 126.5(7) . . ?
O2 C7 C1 118.1(7) . . ?
O1 C7 C1 115.3(7) . . ?
O4 C8 O3 125.7(6) . . ?
O4 C8 C3 116.5(7) . . ?
O3 C8 C3 117.7(7) . . ?
O5 C9 O6 124.8(7) . . ?
O5 C9 C5 121.8(8) . . ?
O6 C9 C5 113.4(7) . . ?
N1 C10 C11 123.4(9) . . ?
C10 C11 C12 121.3(9) . . ?
C13 C12 C11 115.3(8) . . ?
C13 C12 C12 121.9(10) . 7_676 ?
C11 C12 C12 122.8(10) . 7_676 ?
C14 C13 C12 120.3(9) . . ?
N1 C14 C13 124.9(9) . . ?
N2 C15 C16 123.2(8) . . ?
C15 C16 C17 118.5(8) . . ?
C18 C17 C16 117.3(8) . . ?
C18 C17 C17 121.4(9) . 5_757 ?
C16 C17 C17 121.2(9) . 5_757 ?
C19 C18 C17 120.4(8) . . ?
N2 C19 C18 122.4(8) . . ?
C14 N1 C10 114.8(7) . . ?
C14 N1 Cu1 125.4(6) . . ?
C10 N1 Cu1 119.8(6) . . ?
C15 N2 C19 118.1(7) . . ?
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 O9 1.449(6) 2_756 ?
S O9 1.449(6) . ?
S O8 1.486(6) . ?
S O8 1.486(6) 2_756 ?
Cu1 O7 1.944(5) . ?
Cu1 O1 1.944(5) . ?
Cu1 O4 1.952(5) 6_565 ?
Cu1 N1 2.018(7) . ?
Cu1 O8 2.325(6) . ?
Cu2 O2 1.916(5) . ?
Cu2 O3 1.919(5) 5_767 ?
Cu2 O7 1.970(5) 2_756 ?
Cu2 O7 1.978(5) . ?
Cu2 Cu2 2.9012(17) 2_756 ?
O1 C7 1.268(9) . ?
O2 C7 1.236(9) . ?
O3 C8 1.260(9) . ?
O3 Cu2 1.919(5) 5_767 ?
O4 C8 1.259(9) . ?
O4 Cu1 1.952(5) 6_566 ?
O5 C9 1.203(10) . ?
O6 C9 1.314(10) . ?
O7 Cu2 1.970(5) 2_756 ?
C1 C6 1.389(10) . ?
C1 C2 1.402(10) . ?
C1 C7 1.506(11) . ?
C2 C3 1.387(10) . ?
C3 C4 1.391(11) . ?
C3 C8 1.492(10) . ?
C4 C5 1.368(10) . ?
C5 C6 1.376(11) . ?
C5 C9 1.514(11) . ?
C10 N1 1.358(11) . ?
C10 C11 1.361(13) . ?
C11 C12 1.389(12) . ?
C12 C13 1.385(12) . ?
C12 C12 1.486(16) 7_676 ?
C13 C14 1.363(13) . ?
C14 N1 1.340(11) . ?
C15 N2 1.333(11) . ?
C15 C16 1.397(12) . ?
C16 C17 1.399(12) . ?
C17 C18 1.388(12) . ?
C17 C17 1.487(15) 5_757 ?
C18 C19 1.376(12) . ?
C19 N2 1.337(11) . ?
