#------------------------------------------------------------------------------
#$Date: 2016-02-21 11:56:54 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176809 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/01/2240148.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2240148
loop_
_publ_author_name
'Wang, Chun-Xiang'
'Li, Zhi-Feng'
_publ_section_title
;
 Crystal structure of
 catena-poly[[diaqua(4,5-diazafluoren-9-one-κ²N,N')cadmium]-μ-2-hydroxy-5-sulfonatobenzoato-κ³O¹,O^1'^:O⁵]
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m387
_journal_page_last               m388
_journal_paper_doi               10.1107/S1600536814023472
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Cd (C7 H4 O6 S) (C11 H6 N2 O) (H2 O)2]'
_chemical_formula_moiety         'C18 H14 Cd N2 O9 S'
_chemical_formula_sum            'C18 H14 Cd N2 O9 S'
_chemical_formula_weight         546.77
_chemical_name_systematic
catena-Poly[[diaqua(4,5-diazafluoren-9-one-κ²N,N')cadmium]-μ-2-hydroxy-5-sulfonatobenzoato-κ³O¹,O^1'^:O⁵]
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 98.1550(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.6233(6)
_cell_length_b                   12.8461(10)
_cell_length_c                   9.4625(7)
_cell_measurement_reflns_used    387
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.1
_cell_volume                     917.29(12)
_computing_cell_refinement
;
SAINT (Bruker, 2004)
;
_computing_data_collection
;
APEX2 (Bruker, 2004)
;
_computing_data_reduction
;
SAINT (Bruker, 2004)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD area-detector'
_diffrn_measurement_method       'φ 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  0.0096
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5158
_diffrn_reflns_theta_full        26.65
_diffrn_reflns_theta_max         26.65
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    1.365
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2003)
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.349
_exptl_crystal_size_mid          0.324
_exptl_crystal_size_min          0.195
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.229
_refine_ls_abs_structure_details
;
Flack (1983), 1559 Friedel pairs
;
_refine_ls_abs_structure_Flack   0.040(13)
_refine_ls_extinction_coef       0.0055(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL97 (Sheldrick, 2008)
;
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3545
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0151
_refine_ls_R_factor_gt           0.0148
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0198P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0373
_refine_ls_wR_factor_ref         0.0374
_reflns_number_gt                3469
_reflns_number_total             3545
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            im2455sup1.cf
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2240148
_cod_database_fobs_code          2240148
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
C C1 0.7119(3) 0.11149(18) 0.4387(2) 0.0325(5) Uani d . 1 1
H H1 0.6659 0.0842 0.5167 0.039 Uiso calc R 1 1
C C2 0.7228(3) 0.04706(19) 0.3233(3) 0.0369(5) Uani d . 1 1
H H2 0.6851 -0.0217 0.3254 0.044 Uiso calc R 1 1
C C3 0.7902(3) 0.08485(19) 0.2036(3) 0.0377(5) Uani d . 1 1
H H3 0.7993 0.0427 0.1251 0.045 Uiso calc R 1 1
C C4 0.8423(3) 0.18736(18) 0.2071(2) 0.0305(5) Uani d . 1 1
C C5 0.9171(3) 0.2583(2) 0.1039(3) 0.0349(5) Uani d . 1 1
C C6 0.9390(2) 0.3622(3) 0.17581(19) 0.0327(4) Uani d . 1 1
C C7 1.0001(3) 0.4579(2) 0.1391(3) 0.0412(6) Uani d . 1 1
H H7 1.0365 0.4693 0.0506 0.049 Uiso calc R 1 1
C C8 1.0049(3) 0.5374(2) 0.2407(3) 0.0434(6) Uani d . 1 1
H H8 1.0489 0.6026 0.2215 0.052 Uiso calc R 1 1
C C9 0.9445(3) 0.51923(17) 0.3698(3) 0.0355(5) Uani d . 1 1
H H9 0.9428 0.5746 0.4329 0.043 Uiso calc R 1 1
C C10 0.8864(2) 0.3516(2) 0.3100(2) 0.0280(4) Uani d . 1 1
C C11 0.8275(3) 0.24562(16) 0.3282(2) 0.0282(4) Uani d . 1 1
C C12 0.4313(3) 0.19306(15) 0.9233(2) 0.0248(4) Uani d . 1 1
C C13 0.3771(3) 0.11221(16) 1.0031(2) 0.0261(4) Uani d . 1 1
H H13 0.3678 0.0454 0.9650 0.031 Uiso calc R 1 1
C C14 0.3361(3) 0.12964(15) 1.1403(2) 0.0241(4) Uani d . 1 1
C C15 0.3489(3) 0.23148(16) 1.1954(2) 0.0262(4) Uani d . 1 1
C C16 0.4067(3) 0.31269(17) 1.1150(2) 0.0308(5) Uani d . 1 1
H H16 0.4169 0.3797 1.1525 0.037 Uiso calc R 1 1
C C17 0.4488(3) 0.29364(16) 0.9797(2) 0.0291(5) Uani d . 1 1
H H17 0.4885 0.3475 0.9267 0.035 Uiso calc R 1 1
C C18 0.2836(3) 0.04158(16) 1.2294(2) 0.0277(4) Uani d . 1 1
Cd Cd1 0.760273(16) 0.360333(13) 0.613628(12) 0.02682(5) Uani d . 1 1
N N1 0.7645(2) 0.21201(14) 0.44437(19) 0.0281(4) Uani d . 1 1
N N2 0.8881(2) 0.42577(14) 0.4086(2) 0.0301(4) Uani d . 1 1
O O1 0.9547(2) 0.23396(15) -0.01156(18) 0.0460(4) Uani d . 1 1
O O2 0.2854(2) -0.04920(12) 1.18426(18) 0.0392(4) Uani d . 1 1
O O3 0.2427(2) 0.06334(13) 1.35128(17) 0.0377(4) Uani d . 1 1
O O4 0.3065(2) 0.25331(12) 1.32612(16) 0.0344(4) Uani d . 1 1
H H4 0.2813 0.1972 1.3664 0.052 Uiso d . 1 1
O O5 0.3267(2) 0.22249(15) 0.65477(18) 0.0418(4) Uani d . 1 1
O O6 0.4806(2) 0.06102(12) 0.72661(17) 0.0394(4) Uani d . 1 1
O O7 0.6409(2) 0.22356(13) 0.73467(17) 0.0359(4) Uani d . 1 1
O O8 0.4984(2) 0.40770(12) 0.48081(17) 0.0338(3) Uani d . 1 1
O O9 1.0370(2) 0.32540(13) 0.73495(18) 0.0411(4) Uani d . 1 1
S S1 0.47242(7) 0.17302(4) 0.74579(5) 0.02593(11) Uani d . 1 1
H H8B 0.4229 0.3687 0.4315 0.039 Uiso d . 1 1
H H8A 0.5159 0.4564 0.4233 0.039 Uiso d . 1 1
H H9B 1.0268 0.3091 0.8205 0.039 Uiso d . 1 1
H H9A 1.1283 0.3117 0.6959 0.039 Uiso d . 1 1
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'
Cd Cd -0.8075 1.2024 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 C1 C2 . . 123.6(2)
N1 C1 H1 . . 118.2
C2 C1 H1 . . 118.2
C1 C2 C3 . . 120.2(2)
C1 C2 H2 . . 119.9
C3 C2 H2 . . 119.9
C4 C3 C2 . . 116.9(2)
C4 C3 H3 . . 121.6
C2 C3 H3 . . 121.6
C3 C4 C11 . . 118.7(2)
C3 C4 C5 . . 134.4(2)
C11 C4 C5 . . 107.0(2)
O1 C5 C6 . . 128.0(2)
O1 C5 C4 . . 126.1(2)
C6 C5 C4 . . 105.86(19)
C7 C6 C10 . . 118.0(3)
C7 C6 C5 . . 134.6(2)
C10 C6 C5 . . 107.4(2)
C6 C7 C8 . . 117.1(2)
C6 C7 H7 . . 121.5
C8 C7 H7 . . 121.5
C9 C8 C7 . . 120.2(2)
C9 C8 H8 . . 119.9
C7 C8 H8 . . 119.9
N2 C9 C8 . . 123.4(2)
N2 C9 H9 . . 118.3
C8 C9 H9 . . 118.3
N2 C10 C6 . . 126.4(3)
N2 C10 C11 . . 124.04(19)
C6 C10 C11 . . 109.5(2)
N1 C11 C4 . . 126.0(2)
N1 C11 C10 . . 123.74(19)
C4 C11 C10 . . 110.22(19)
C13 C12 C17 . . 120.43(19)
C13 C12 S1 . . 121.07(15)
C17 C12 S1 . . 118.46(16)
C12 C13 C14 . . 120.76(19)
C12 C13 H13 . . 119.6
C14 C13 H13 . . 119.6
C13 C14 C15 . . 118.78(18)
C13 C14 C18 . . 121.01(18)
C15 C14 C18 . . 120.19(18)
O4 C15 C16 . . 118.54(19)
O4 C15 C14 . . 121.31(19)
C16 C15 C14 . . 120.15(19)
C17 C16 C15 . . 120.2(2)
C17 C16 H16 . . 119.9
C15 C16 H16 . . 119.9
C16 C17 C12 . . 119.62(19)
C16 C17 H17 . . 120.2
C12 C17 H17 . . 120.2
O2 C18 O3 . . 122.4(2)
O2 C18 C14 . . 119.85(19)
O3 C18 C14 . . 117.73(19)
O8 Cd1 O9 . . 174.22(6)
O8 Cd1 O2 . 2_657 95.69(6)
O9 Cd1 O2 . 2_657 85.41(6)
O8 Cd1 O7 . . 95.66(6)
O9 Cd1 O7 . . 90.12(6)
O2 Cd1 O7 2_657 . 81.84(6)
O8 Cd1 N2 . . 83.53(6)
O9 Cd1 N2 . . 91.30(6)
O2 Cd1 N2 2_657 . 127.58(6)
O7 Cd1 N2 . . 150.56(6)
O8 Cd1 N1 . . 86.57(6)
O9 Cd1 N1 . . 94.42(6)
O2 Cd1 N1 2_657 . 159.30(6)
O7 Cd1 N1 . . 77.46(6)
N2 Cd1 N1 . . 73.11(6)
O8 Cd1 O3 . 2_657 77.46(5)
O9 Cd1 O3 . 2_657 98.87(6)
O2 Cd1 O3 2_657 2_657 52.44(5)
O7 Cd1 O3 . 2_657 132.00(5)
N2 Cd1 O3 . 2_657 76.72(5)
N1 Cd1 O3 . 2_657 147.20(5)
C11 N1 C1 . . 114.62(19)
C11 N1 Cd1 . . 108.76(13)
C1 N1 Cd1 . . 136.50(16)
C10 N2 C9 . . 114.8(2)
C10 N2 Cd1 . . 110.21(14)
C9 N2 Cd1 . . 134.77(16)
C18 O2 Cd1 . 2_647 100.22(14)
C18 O3 Cd1 . 2_647 84.48(13)
C15 O4 H4 . . 109.5
S1 O7 Cd1 . . 140.81(11)
Cd1 O8 H8B . . 128.0
Cd1 O8 H8A . . 110.0
H8B O8 H8A . . 103.7
Cd1 O9 H9B . . 108.8
Cd1 O9 H9A . . 124.9
H9B O9 H9A . . 123.6
O5 S1 O6 . . 113.71(11)
O5 S1 O7 . . 111.74(11)
O6 S1 O7 . . 112.26(10)
O5 S1 C12 . . 106.01(10)
O6 S1 C12 . . 106.20(9)
O7 S1 C12 . . 106.27(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 N1 . 1.351(3)
C1 C2 . 1.382(3)
C1 H1 . 0.9300
C2 C3 . 1.395(4)
C2 H2 . 0.9300
C3 C4 . 1.375(3)
C3 H3 . 0.9300
C4 C11 . 1.386(3)
C4 C5 . 1.506(3)
C5 O1 . 1.209(3)
C5 C6 . 1.497(4)
C6 C7 . 1.376(4)
C6 C10 . 1.391(3)
C7 C8 . 1.399(4)
C7 H7 . 0.9300
C8 C9 . 1.385(4)
C8 H8 . 0.9300
C9 N2 . 1.344(3)
C9 H9 . 0.9300
C10 N2 . 1.333(3)
C10 C11 . 1.452(3)
C11 N1 . 1.333(3)
C12 C13 . 1.381(3)
C12 C17 . 1.397(3)
C12 S1 . 1.771(2)
C13 C14 . 1.395(3)
C13 H13 . 0.9300
C14 C15 . 1.407(3)
C14 C18 . 1.499(3)
C15 O4 . 1.351(3)
C15 C16 . 1.399(3)
C16 C17 . 1.385(3)
C16 H16 . 0.9300
C17 H17 . 0.9300
C18 O2 . 1.243(3)
C18 O3 . 1.268(3)
Cd1 O8 . 2.2857(16)
Cd1 O9 . 2.2984(16)
Cd1 O2 2_657 2.3061(16)
Cd1 O7 . 2.3501(16)
Cd1 N2 . 2.4404(19)
Cd1 N1 . 2.4922(18)
Cd1 O3 2_657 2.6294(17)
O2 Cd1 2_647 2.3061(16)
O3 Cd1 2_647 2.6294(17)
O4 H4 . 0.8504
O5 S1 . 1.4518(18)
O6 S1 . 1.4527(16)
O7 S1 . 1.4561(17)
O8 H8B . 0.8500
O8 H8A . 0.8519
O9 H9B . 0.8507
O9 H9A . 0.8510
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O8 H8A O6 2_656 0.85 1.96 2.801(3) 171 yes
O8 H8B O4 1_554 0.85 1.93 2.758(3) 164 yes
O9 H9A O5 1_655 0.85 1.98 2.771(3) 154 yes
O9 H9B O1 1_556 0.85 2.00 2.820(3) 161 yes
