#------------------------------------------------------------------------------
#$Date: 2016-02-14 15:26:36 +0100 (dom 14 de feb de 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/17/1511769.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_1511769
loop_
_publ_author_name
'M. Ruiz'
'Rosa Ortiz'
'Lourdes Perelló'
'Alfonso Castiñeiras'
'Miguel Quirós'
_publ_section_title
;
 Ni(II) and Zn(II) Complexes with Cinoxacin. Synthesis and
 Characterization of M(Cx)2(DMSO)n(H2O)m (n = 0,2; m = 2,4). Crystal
 Structures of [M(Cx)2(DMSO)2].4H2O (M = Ni(II), Zn(II))
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              133
_journal_page_last               139
_journal_paper_doi               10.1016/S0020-1693(00)85592-9
_journal_volume                  211
_journal_year                    1993
_chemical_formula_moiety
;
C28 H30 N4 Ni1 O12 S2,4(H2 O1)
;
_chemical_formula_sum            'C28 H38 N4 Ni O16 S2'
_chemical_formula_weight         809.5
_chemical_name_systematic
;
bis(1-Ethyl-1,4-dihydro-4-oxo(1,3)dioxolo(4,5-g)cinnoline-3-carboxylato)-bis(d
imethylsulfoxide)-nickel tetrahydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             1994-07-14
_cell_angle_alpha                90
_cell_angle_beta                 104.66(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.684(2)
_cell_length_b                   7.729(1)
_cell_length_c                   20.862(1)
_cell_volume                     1666.6(4)
_diffrn_ambient_temperature      298
_diffrn_measurement_device_type  'Enraf Nonius CAD-4'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_number            3690
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.7815
_exptl_absorpt_correction_T_max  1.133
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'bright green'
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepipedic
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.344
_refine_ls_goodness_of_fit_ref   1.223
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_reflns         2500
_refine_ls_R_factor_gt           0.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_ref         0.041
_reflns_number_gt                2500
_reflns_number_total             3308
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            valenciani.cif
_cod_data_source_block           valenciani
_cod_original_cell_volume        1666.7(3)
_cod_original_formula_sum        'C28 H38 N4 Ni1 O16 S2'
_cod_database_code               1511769
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2-x,1/2+y,1/2-z
3 -x,-y,-z
4 -1/2+x,-1/2-y,-1/2+z
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
Ni Ni 0.50000 0.00000 0.50000 0.0240(2) Uani
N1 N -0.0232(2) -0.1220(4) 0.4016(1) 0.028(1) Uani
C11 C -0.1555(3) -0.1239(5) 0.3560(2) 0.038(2) Uani
H111 H -0.22070 -0.08390 0.38470 0.05 Uiso
H112 H -0.19330 -0.25000 0.35150 0.05 Uiso
C12 C -0.1624(4) -0.0416(7) 0.2909(2) 0.058(3) Uani
H121 H -0.25000 -0.04290 0.26750 0.05 Uiso
H122 H -0.12980 0.07300 0.29850 0.05 Uiso
H123 H -0.10930 -0.08390 0.26750 0.05 Uiso
N2 N 0.0678(2) -0.0467(3) 0.3789(1) 0.028(1) Uani
C2 C 0.1887(3) -0.0441(4) 0.4144(1) 0.025(1) Uani
C1 C 0.2783(3) 0.0508(4) 0.3800(1) 0.025(1) Uani
O1 O 0.3920(2) 0.0847(3) 0.4127(1) 0.0275(9) Uani
O2 O 0.2334(2) 0.0884(3) 0.3207(1) 0.037(1) Uani
C3 C 0.2299(3) -0.1243(4) 0.4786(1) 0.023(1) Uani
O3 O 0.3451(2) -0.1301(3) 0.5133(1) 0.029(1) Uani
C4 C 0.1278(3) -0.2034(4) 0.5024(1) 0.025(1) Uani
C5 C 0.1572(3) -0.2799(4) 0.5663(2) 0.032(1) Uani
H5 H 0.25000 -0.29100 0.59960 0.05 Uiso
C6 C 0.0561(3) -0.3467(4) 0.5867(2) 0.032(1) Uani
O4 O 0.0583(2) -0.4272(4) 0.6454(1) 0.047(1) Uani
C7 C -0.0744(3) -0.4476(6) 0.6467(2) 0.049(2) Uani
H71 H -0.10930 -0.37500 0.68350 0.05 Uiso
H72 H -0.08200 -0.58200 0.66790 0.05 Uiso
O5 O -0.1508(2) -0.4153(4) 0.5805(1) 0.047(1) Uani
C8 C -0.0702(3) -0.3411(4) 0.5474(2) 0.033(1) Uani
C9 C -0.1037(3) -0.2707(5) 0.4860(2) 0.034(2) Uani
H9 H -0.19330 -0.25000 0.46670 0.05 Uiso
C10 C 0.0001(3) -0.1991(4) 0.4630(1) 0.026(1) Uani
S1 S 0.5477(1) 0.2998(1) 0.6049(1) 0.0343(4) Uani
O6 O 0.4434(2) 0.2166(3) 0.5501(1) 0.035(1) Uani
C21 C 0.5429(5) 0.5200(6) 0.5811(2) 0.063(2) Uani
H211 H 0.44530 0.54290 0.58390 0.05 Uiso
H212 H 0.58390 0.58390 0.63470 0.05 Uiso
H213 H 0.55660 0.54290 0.55070 0.05 Uiso
C22 C 0.4844(5) 0.3039(7) 0.6753(2) 0.074(3) Uani
H221 H 0.55660 0.37500 0.71670 0.05 Uiso
H222 H 0.39060 0.37500 0.65030 0.05 Uiso
H223 H 0.47070 0.20890 0.69920 0.05 Uiso
O1W O 0.3604(3) 0.2617(4) 0.2406(1) 0.063(1) Uani
H21W H 0.33210 0.37500 0.23250 0.05 Uiso
H22W H 0.30670 0.20700 0.26760 0.05 Uiso
O2W O 0.9902(3) 0.6313(5) 0.1705(1) 0.064(1) Uani
H21W H 1.00000 0.66600 0.19920 0.05 Uiso
H22W H 0.97070 0.58200 0.13280 0.05 Uiso
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
N 0.68
Ni 1.50
O 0.68
S 1.02
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ni O1 2.003(2)
Ni O3 2.015(2)
Ni O6 2.140(2)
N1 C11 1.491(4)
N1 N2 1.320(4)
N1 C10 1.377(4)
C11 C12 1.485(6)
N2 C2 1.317(3)
C2 C1 1.522(5)
C2 C3 1.440(4)
C1 O1 1.262(3)
C1 O2 1.244(3)
C3 O3 1.260(3)
C3 C4 1.443(4)
C4 C5 1.419(4)
C4 C10 1.404(4)
C5 C6 1.360(5)
C6 O4 1.369(4)
C6 C8 1.391(4)
O4 C7 1.434(5)
C7 O5 1.439(5)
O5 C8 1.359(4)
C8 C9 1.353(5)
C9 C10 1.428(5)
S1 O6 1.522(2)
S1 C21 1.770(4)
S1 C22 1.766(5)
