#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/11/2211130.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_2211130
loop_
_publ_author_name
'Le-Hua Zhang'
'Zhe An'
'Ying-Ji Wang'
'Wei Qi '
'Ling Zhu'
_publ_section_title
;Poly[[bis(μ-1,4-dihydro-1-ethyl-6-fluoro-4-oxo-7-(piperazin-1-yl)-1,8-naphthyridine-3-carboxylato)cadmium(II)]
 trihydrate]
;
_journal_coeditor_code           NG2107
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2816
_journal_page_last               m2817
_journal_paper_doi               10.1107/S1600536806039663
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Cd (C15 H16 F1 N4 O3)2], 3H2 O'
_chemical_formula_moiety         'C30 H32 Cd F2 N8 O6, 3H2 O'
_chemical_formula_sum            'C30 H38 Cd F2 N8 O9'
_chemical_formula_weight         805.08
_chemical_name_systematic
;
Poly[[bis(μ-1,4-dihydro-1-ethyl-6-fluoro-4-oxo-7-(piperazin-1-yl)-
1,8-naphtyridine-3-carboxylato)cadmium(II)] trihydrate]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 98.5220(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.5628(3)
_cell_length_b                   22.2025(13)
_cell_length_c                   13.5034(8)
_cell_measurement_reflns_used    8360
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.78
_cell_volume                     1649.36(16)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8360
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.740
_exptl_absorpt_correction_T_max  0.8845
_exptl_absorpt_correction_T_min  0.8309
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.456
_refine_ls_extinction_coef       0.0029(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         2915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0522P)²+1.1028P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0930
_reflns_number_gt                2417
_reflns_number_total             2915
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng2107.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2211130
_cod_database_fobs_code          2211130
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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_disorder_assembly
_atom_site_disorder_group
Cd Cd1 0.5000 0.5000 0.5000 0.02468(14) Uani d S 1 . .
F F1 -0.1944(4) 0.75086(9) 0.32913(15) 0.0463(5) Uani d . 1 . .
C C1 0.7412(6) 0.51767(14) 0.2951(2) 0.0336(7) Uani d . 1 . .
C C2 0.5872(5) 0.57275(12) 0.2654(2) 0.0276(6) Uani d . 1 . .
C C3 0.6371(5) 0.60252(13) 0.1819(2) 0.0310(7) Uani d . 1 . .
H H3A 0.7551 0.5857 0.1482 0.037 Uiso calc R 1 . .
C C4 0.3539(5) 0.68036(12) 0.1914(2) 0.0270(6) Uani d . 1 . .
C C5 0.0617(5) 0.76164(13) 0.2029(2) 0.0279(6) Uani d . 1 . .
C C6 -0.0062(6) 0.83524(14) 0.0698(2) 0.0382(8) Uani d . 1 . .
H H6A 0.0021 0.8019 0.0241 0.046 Uiso calc R 1 . .
H H6B 0.1512 0.8549 0.0804 0.046 Uiso calc R 1 . .
C C7 -0.1984(6) 0.87945(13) 0.0245(2) 0.0349(7) Uani d . 1 . .
H H7A -0.1525 0.8953 -0.0370 0.042 Uiso calc R 1 . .
H H7B -0.3510 0.8581 0.0072 0.042 Uiso calc R 1 . .
C C8 -0.2862(6) 0.90622(13) 0.1868(2) 0.0317(7) Uani d . 1 . .
H H8A -0.4417 0.8856 0.1767 0.038 Uiso calc R 1 . .
H H8B -0.2980 0.9395 0.2323 0.038 Uiso calc R 1 . .
C C9 -0.0915(6) 0.86293(13) 0.2343(2) 0.0335(7) Uani d . 1 . .
H H9A 0.0618 0.8841 0.2501 0.040 Uiso calc R 1 . .
H H9B -0.1357 0.8472 0.2961 0.040 Uiso calc R 1 . .
C C10 -0.0067(5) 0.72956(13) 0.2857(2) 0.0300(7) Uani d . 1 . .
C C11 0.1009(5) 0.67772(13) 0.3200(2) 0.0289(6) Uani d . 1 . .
H H11 0.0505 0.6589 0.3749 0.035 Uiso calc R 1 . .
C C12 0.2858(5) 0.65145(12) 0.2753(2) 0.0258(6) Uani d . 1 . .
C C13 0.3988(5) 0.59572(12) 0.3161(2) 0.0254(6) Uani d . 1 . .
C C14 0.5989(6) 0.67862(15) 0.0503(2) 0.0382(8) Uani d . 1 . .
H H14A 0.7525 0.6612 0.0391 0.046 Uiso calc R 1 . .
H H14B 0.6216 0.7218 0.0578 0.046 Uiso calc R 1 . .
C C15 0.4107(8) 0.6665(2) -0.0397(3) 0.0615(11) Uani d . 1 . .
H H15A 0.4018 0.6240 -0.0526 0.092 Uiso calc R 1 . .
H H15B 0.4552 0.6870 -0.0969 0.092 Uiso calc R 1 . .
H H15C 0.2553 0.6807 -0.0270 0.092 Uiso calc R 1 . .
N N1 0.5315(4) 0.65370(11) 0.14404(17) 0.0309(6) Uani d . 1 . .
N N2 0.2465(5) 0.73545(13) 0.1572(2) 0.0464(7) Uani d . 1 . .
N N3 -0.0633(4) 0.81258(11) 0.16538(17) 0.0296(5) Uani d . 1 . .
N N4 -0.2361(4) 0.93001(10) 0.09036(17) 0.0272(5) Uani d . 1 . .
H H4 -0.0897 0.9489 0.1038 0.033 Uiso calc R 1 . .
O O1 0.7523(4) 0.49668(8) 0.38224(17) 0.0330(5) Uani d . 1 . .
O O2 0.3261(4) 0.57352(9) 0.39234(15) 0.0319(5) Uani d . 1 . .
O O3 0.8536(7) 0.49635(11) 0.2315(2) 0.0701(10) Uani d . 1 . .
O O1W 0.444(3) 0.5135(5) -0.0311(7) 0.163(6) Uani d P 0.50 . .
H H1 0.4057 0.5248 -0.0916 0.196 Uiso d R 1 . .
O O2W 1.076(4) 0.4607(7) 0.0607(11) 0.299(14) Uani d P 0.50 . .
H H2 1.0943 0.4261 0.0879 0.358 Uiso d R 1 A .
O O2W' 1.109(2) 0.5295(8) 0.0776(9) 0.201(7) Uani d P 0.50 A 1
H H3 1.1837 0.5578 0.1118 0.242 Uiso d R 1 A 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'
F F 0.0171 0.0103 '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
O1 Cd1 O1 . 3_666 180.0000(10)
O1 Cd1 O2 . . 80.01(7)
O1 Cd1 O2 3_666 . 99.99(7)
O1 Cd1 O2 . 3_666 99.99(7)
O1 Cd1 O2 3_666 3_666 80.01(7)
O2 Cd1 O2 . 3_666 180.00(8)
O1 Cd1 N4 . 2_545 91.06(8)
O1 Cd1 N4 3_666 2_545 88.94(8)
O2 Cd1 N4 . 2_545 88.24(8)
O2 Cd1 N4 3_666 2_545 91.76(8)
O1 Cd1 N4 . 4_676 88.94(8)
O1 Cd1 N4 3_666 4_676 91.06(8)
O2 Cd1 N4 . 4_676 91.76(8)
O2 Cd1 N4 3_666 4_676 88.24(8)
N4 Cd1 N4 2_545 4_676 180.00(8)
O3 C1 O1 . . 123.4(3)
O3 C1 C2 . . 116.9(3)
O1 C1 C2 . . 119.6(3)
C3 C2 C13 . . 118.3(2)
C3 C2 C1 . . 115.6(3)
C13 C2 C1 . . 126.1(2)
N1 C3 C2 . . 126.1(3)
N1 C3 H3A . . 116.9
C2 C3 H3A . . 116.9
N1 C4 C12 . . 118.3(2)
N1 C4 N2 . . 121.1(2)
C12 C4 N2 . . 120.6(3)
N3 C5 N2 . . 122.7(3)
N3 C5 C10 . . 121.2(3)
N2 C5 C10 . . 115.9(3)
N3 C6 C7 . . 110.3(2)
N3 C6 H6A . . 109.6
C7 C6 H6A . . 109.6
N3 C6 H6B . . 109.6
C7 C6 H6B . . 109.6
H6A C6 H6B . . 108.1
N4 C7 C6 . . 114.0(3)
N4 C7 H7A . . 108.8
C6 C7 H7A . . 108.8
N4 C7 H7B . . 108.8
C6 C7 H7B . . 108.8
H7A C7 H7B . . 107.6
N4 C8 C9 . . 112.6(2)
N4 C8 H8A . . 109.1
C9 C8 H8A . . 109.1
N4 C8 H8B . . 109.1
C9 C8 H8B . . 109.1
H8A C8 H8B . . 107.8
N3 C9 C8 . . 110.4(2)
N3 C9 H9A . . 109.6
C8 C9 H9A . . 109.6
N3 C9 H9B . . 109.6
C8 C9 H9B . . 109.6
H9A C9 H9B . . 108.1
C11 C10 F1 . . 118.7(3)
C11 C10 C5 . . 122.7(3)
F1 C10 C5 . . 118.5(3)
C10 C11 C12 . . 121.8(3)
C10 C11 H11 . . 119.1
C12 C11 H11 . . 119.1
C11 C12 C4 . . 117.6(2)
C11 C12 C13 . . 119.7(2)
C4 C12 C13 . . 122.7(2)
O2 C13 C2 . . 126.8(2)
O2 C13 C12 . . 117.9(2)
C2 C13 C12 . . 115.4(2)
N1 C14 C15 . . 112.9(3)
N1 C14 H14A . . 109.0
C15 C14 H14A . . 109.0
N1 C14 H14B . . 109.0
C15 C14 H14B . . 109.0
H14A C14 H14B . . 107.8
C14 C15 H15A . . 109.5
C14 C15 H15B . . 109.5
H15A C15 H15B . . 109.5
C14 C15 H15C . . 109.5
H15A C15 H15C . . 109.5
H15B C15 H15C . . 109.5
C3 N1 C4 . . 119.1(2)
C3 N1 C14 . . 119.3(2)
C4 N1 C14 . . 121.5(2)
C5 N2 C4 . . 121.3(3)
C5 N3 C6 . . 116.2(2)
C5 N3 C9 . . 118.8(2)
C6 N3 C9 . . 110.6(2)
C7 N4 C8 . . 109.0(2)
C7 N4 Cd1 . 2 108.99(16)
C8 N4 Cd1 . 2 120.76(17)
C7 N4 H4 . . 105.7
C8 N4 H4 . . 105.7
Cd1 N4 H4 2 . 105.7
C1 O1 Cd1 . . 133.8(2)
C13 O2 Cd1 . . 129.59(18)
O1W O1W H1 3_665 . 153.2
O2W' O2W H2 . . 145.2
O2W O2W' H3 . . 147.8
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cd1 O1 . 2.273(2)
Cd1 O1 3_666 2.273(2)
Cd1 O2 . 2.3015(19)
Cd1 O2 3_666 2.3015(19)
Cd1 N4 2_545 2.351(2)
Cd1 N4 4_676 2.351(2)
F1 C10 . 1.357(3)
C1 O3 . 1.229(4)
C1 O1 . 1.258(4)
C1 C2 . 1.513(4)
C2 C3 . 1.371(4)
C2 C13 . 1.428(4)
C3 N1 . 1.345(4)
C3 H3A . 0.9300
C4 N1 . 1.386(4)
C4 C12 . 1.403(4)
C4 N2 . 1.409(4)
C5 N3 . 1.384(4)
C5 N2 . 1.402(4)
C5 C10 . 1.424(4)
C6 N3 . 1.463(4)
C6 C7 . 1.513(4)
C6 H6A . 0.9700
C6 H6B . 0.9700
C7 N4 . 1.467(4)
C7 H7A . 0.9700
C7 H7B . 0.9700
C8 N4 . 1.470(4)
C8 C9 . 1.517(4)
C8 H8A . 0.9700
C8 H8B . 0.9700
C9 N3 . 1.477(4)
C9 H9A . 0.9700
C9 H9B . 0.9700
C10 C11 . 1.347(4)
C11 C12 . 1.395(4)
C11 H11 . 0.9300
C12 C13 . 1.458(4)
C13 O2 . 1.261(3)
C14 N1 . 1.479(4)
C14 C15 . 1.506(6)
C14 H14A . 0.9700
C14 H14B . 0.9700
C15 H15A . 0.9600
C15 H15B . 0.9600
C15 H15C . 0.9600
N4 Cd1 2 2.351(2)
N4 H4 . 0.9100
O1W O1W 3_665 1.14(2)
O1W H1 . 0.8500
O2W O2W' . 1.55(2)
O2W H2 . 0.8519
O2W' H3 . 0.8499
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
O3 C1 C2 C3 . . -16.6(4)
O1 C1 C2 C3 . . 162.2(3)
O3 C1 C2 C13 . . 163.5(3)
O1 C1 C2 C13 . . -17.8(5)
C13 C2 C3 N1 . . 3.0(5)
C1 C2 C3 N1 . . -177.0(3)
N3 C6 C7 N4 . . 55.7(4)
N4 C8 C9 N3 . . -56.9(3)
N3 C5 C10 C11 . . 175.6(3)
N2 C5 C10 C11 . . 1.1(5)
N3 C5 C10 F1 . . -1.6(5)
N2 C5 C10 F1 . . -176.1(2)
F1 C10 C11 C12 . . 176.4(3)
C5 C10 C11 C12 . . -0.9(5)
C10 C11 C12 C4 . . -1.2(4)
C10 C11 C12 C13 . . 179.2(3)
N1 C4 C12 C11 . . -177.8(3)
N2 C4 C12 C11 . . 3.1(4)
N1 C4 C12 C13 . . 1.8(4)
N2 C4 C12 C13 . . -177.4(3)
C3 C2 C13 O2 . . 178.5(3)
C1 C2 C13 O2 . . -1.5(5)
C3 C2 C13 C12 . . -3.1(4)
C1 C2 C13 C12 . . 176.9(3)
C11 C12 C13 O2 . . -1.0(4)
C4 C12 C13 O2 . . 179.4(3)
C11 C12 C13 C2 . . -179.6(3)
C4 C12 C13 C2 . . 0.8(4)
C2 C3 N1 C4 . . -0.2(4)
C2 C3 N1 C14 . . -177.3(3)
C12 C4 N1 C3 . . -2.1(4)
N2 C4 N1 C3 . . 177.0(3)
C12 C4 N1 C14 . . 174.9(3)
N2 C4 N1 C14 . . -6.0(4)
C15 C14 N1 C3 . . 102.7(3)
C15 C14 N1 C4 . . -74.3(4)
N3 C5 N2 C4 . . -173.7(3)
C10 C5 N2 C4 . . 0.7(5)
N1 C4 N2 C5 . . 178.0(3)
C12 C4 N2 C5 . . -2.9(4)
N2 C5 N3 C6 . . 4.9(4)
C10 C5 N3 C6 . . -169.2(3)
N2 C5 N3 C9 . . -131.0(3)
C10 C5 N3 C9 . . 54.8(4)
C7 C6 N3 C5 . . 164.8(3)
C7 C6 N3 C9 . . -55.8(3)
C8 C9 N3 C5 . . -164.9(3)
C8 C9 N3 C6 . . 56.9(3)
C6 C7 N4 C8 . . -53.9(3)
C6 C7 N4 Cd1 . 2 172.4(2)
C9 C8 N4 C7 . . 54.2(3)
C9 C8 N4 Cd1 . 2 -178.59(18)
O3 C1 O1 Cd1 . . -156.1(3)
C2 C1 O1 Cd1 . . 25.2(4)
O2 Cd1 O1 C1 . . -13.6(3)
O2 Cd1 O1 C1 3_666 . 166.4(3)
N4 Cd1 O1 C1 2_545 . 74.4(3)
N4 Cd1 O1 C1 4_676 . -105.6(3)
C2 C13 O2 Cd1 . . 12.8(4)
C12 C13 O2 Cd1 . . -165.53(18)
O1 Cd1 O2 C13 . . -6.5(2)
O1 Cd1 O2 C13 3_666 . 173.5(2)
N4 Cd1 O2 C13 2_545 . -97.9(2)
N4 Cd1 O2 C13 4_676 . 82.1(2)
