#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/08/2010802.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_2010802
loop_
_publ_author_name
'Song, You'
'Xu, Yan'
'Zhu, Dun-Ru'
'You, Xiao-Zeng'
_publ_section_title
;
 Acetatodiaqua[3-(salicyloylhydrazono)butan-2-one oximato]nickel(II)
 ethanol solvate
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              430
_journal_page_last               431
_journal_paper_doi               10.1107/S0108270100000329
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac
'[Ni (C11 H12 N3 O3) (C2 H3 O2) (H2 O)2] , C2 H5 O H'
_chemical_formula_sum            'C15 H25 N3 Ni O8'
_chemical_formula_weight         434.09
_chemical_name_systematic
;
Acetatodiaqua[3-(salicyloylhydrazone)butan-2-one oximato]nickel(II) ethanol
solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                103.13(3)
_cell_angle_beta                 103.97(3)
_cell_angle_gamma                106.80(3)
_cell_formula_units_Z            2
_cell_length_a                   7.4120(15)
_cell_length_b                   11.505(2)
_cell_length_c                   13.255(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      6.68
_cell_measurement_theta_min      1.56
_cell_volume                     995.0(5)
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)?'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1990b)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990a)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'FR590 CAD-4'
_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     .71073
_diffrn_reflns_av_R_equivalents  .022
_diffrn_reflns_av_sigmaI/netI    .067
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3784
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.020
_exptl_absorpt_correction_T_max  .947
_exptl_absorpt_correction_T_min  .654
_exptl_absorpt_correction_type   'empirical via \y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             456
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .05
_refine_diff_density_max         .629
_refine_diff_density_min         -.588
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.000
_refine_ls_goodness_of_fit_obs   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3484
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.014
_refine_ls_restrained_S_obs      1.110
_refine_ls_R_factor_all          .085
_refine_ls_R_factor_obs          .047
_refine_ls_shift/esd_max         <0.001
_refine_ls_shift/esd_mean        .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0842P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .134
_refine_ls_wR_factor_obs         .122
_reflns_number_observed          2472
_reflns_number_total             3486
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            de1121.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0842P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0842P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        995.0(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2010802
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
Ni1 -.95134(8) .25295(4) .23640(4) .0304(2) Uani d . 1 . Ni
N1 -1.0929(5) .0716(3) .1346(2) .0305(7) Uani d . 1 . N
N2 -.9171(5) .1378(3) .3365(3) .0363(8) Uani d . 1 . N
N3 -1.1903(5) .0604(3) .0295(2) .0335(8) Uani d . 1 . N
H3A -1.2606 -.0127 -.0200 .040 Uiso calc R 1 . H
O1W -.6908(4) .2616(3) .2069(3) .0505(8) Uani d . 1 . O
H1W -.5784 .3375 .2423 .061 Uiso d R 1 . H
H2W -.6541 .1965 .2028 .061 Uiso d R 1 . H
O2W -1.2076(4) .2539(2) .2669(2) .0411(7) Uani d . 1 . O
H3W -1.3167 .2030 .2380 .049 Uiso d R 1 . H
H4W -1.2134 .3320 .2782 .049 Uiso d R 1 . H
O1 -.8240(4) .4371(2) .3269(2) .0420(7) Uani d . 1 . O
O2 -.7556(5) .4196(3) .4951(2) .0538(9) Uani d . 1 . O
O3 -.3284(5) .4624(3) .2937(2) .0451(7) Uani d . 1 . O
H6A -.2927 .4998 .3597 .068 Uiso calc R 1 . H
O4 -.8149(5) .1788(3) .4474(2) .0517(8) Uani d . 1 . O
H4A -.7736 .2573 .4710 .078 Uiso calc R 1 . H
O5 -1.0607(4) .2772(2) .0800(2) .0412(7) Uani d . 1 . O
O6 -1.4390(4) -.0671(3) -.1595(2) .0403(7) Uani d . 1 . O
C1 -1.1683(6) .1727(4) .0086(3) .0328(9) Uani d . 1 . C
C2 -1.2767(6) .1614(4) -.1042(3) .0330(9) Uani d . 1 . C
C3 -1.2509(7) .2738(4) -.1314(3) .0424(10) Uani d . 1 . C
H3 -1.1455 .3536 -.0820 .051 Uiso d R 1 . H
C4 -1.3482(7) .2730(5) -.2330(4) .0511(12) Uani d . 1 . C
H4 -1.3202 .3498 -.2626 .061 Uiso d R 1 . H
C5 -1.4760(7) .1554(5) -.3110(4) .0532(12) Uani d . 1 . C
H5A -1.5428 .1530 -.3810 .064 Uiso calc R 1 . H
C6 -1.5048(7) .0441(5) -.2865(3) .0472(11) Uani d . 1 . C
H6 -1.6127 -.0459 -.3363 .057 Uiso d R 1 . H
C7 -1.4064(6) .0417(4) -.1821(3) .0352(9) Uani d . 1 . C
C8 -1.1026(6) -.0237(4) .1700(3) .0319(9) Uani d . 1 . C
C9 -.9899(6) .0160(4) .2894(3) .0346(9) Uani d . 1 . C
C10 -1.2192(7) -.1608(4) .1040(4) .0445(11) Uani d . 1 . C
H10A -1.2809 -.1671 .0294 .067 Uiso calc R 1 . H
H10B -1.3203 -.1955 .1339 .067 Uiso calc R 1 . H
H10C -1.1314 -.2080 .1061 .067 Uiso calc R 1 . H
C11 -.9705(7) -.0796(4) .3464(4) .0497(12) Uani d . 1 . C
H11A -.8931 -.0358 .4224 .075 Uiso calc R 1 . H
H11B -.9051 -.1305 .3131 .075 Uiso calc R 1 . H
H11C -1.1007 -.1342 .3404 .075 Uiso calc R 1 . H
C12 -.3206(14) .4900(7) .1225(6) .113(3) Uani d U 1 . C
H12A -.2727 .5529 .0889 .169 Uiso calc R 1 . H
H12B -.4635 .4520 .0925 .169 Uiso calc R 1 . H
H12C -.2648 .4248 .1085 .169 Uiso calc R 1 . H
C13 -.2613(10) .5510(5) .2398(5) .071(2) Uani d U 1 . C
H13A -.1170 .5907 .2696 .085 Uiso calc R 1 . H
H13B -.3158 .6180 .2536 .085 Uiso calc R 1 . H
C14 -.7693(6) .4834(4) .4296(3) .0394(10) Uani d . 1 . C
C15 -.7206(8) .6247(4) .4781(4) .0568(13) Uani d . 1 . C
H15A -.6810 .6478 .5566 .085 Uiso calc R 1 . H
H15B -.8362 .6450 .4512 .085 Uiso calc R 1 . H
H15C -.6135 .6716 .4574 .085 Uiso calc R 1 . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni .3393 1.1124 '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_publ_flag
O1 Ni1 N1 174.98(12) n
O1 Ni1 O2W 88.09(12) n
N1 Ni1 O2W 90.55(12) n
O1 Ni1 O1W 89.34(12) n
N1 Ni1 O1W 91.90(13) n
O2W Ni1 O1W 177.10(11) yes
O1 Ni1 N2 109.91(12) yes
N1 Ni1 N2 74.92(13) yes
O2W Ni1 N2 89.82(13) n
O1W Ni1 N2 92.31(14) n
O1 Ni1 O5 98.23(11) yes
N1 Ni1 O5 76.94(12) yes
O2W Ni1 O5 90.42(12) n
O1W Ni1 O5 88.64(13) n
N2 Ni1 O5 151.86(12) n
C8 N1 N3 123.8(3) n
C8 N1 Ni1 121.3(3) n
N3 N1 Ni1 114.7(2) n
C9 N2 O4 115.7(3) n
C9 N2 Ni1 117.2(3) n
O4 N2 Ni1 127.0(2) n
C1 N3 N1 115.1(3) n
C14 O1 Ni1 127.4(3) n
C1 O5 Ni1 111.2(2) n
O5 C1 N3 121.6(4) n
O5 C1 C2 123.0(4) n
N3 C1 C2 115.4(3) n
C3 C2 C7 120.6(4) ?
C3 C2 C1 117.6(3) ?
C7 C2 C1 121.7(4) ?
C4 C3 C2 121.8(4) ?
C3 C4 C5 118.2(4) ?
C6 C5 C4 121.2(4) ?
C5 C6 C7 122.0(4) ?
O6 C7 C6 121.0(4) ?
O6 C7 C2 122.8(4) ?
C6 C7 C2 116.2(4) ?
N1 C8 C10 125.6(4) n
N1 C8 C9 112.6(3) n
C10 C8 C9 121.7(4) n
N2 C9 C11 124.5(4) n
N2 C9 C8 113.7(3) n
C11 C9 C8 121.7(4) n
O3 C13 C12 111.9(5) ?
O1 C14 O2 124.8(4) ?
O1 C14 C15 117.7(4) ?
O2 C14 C15 117.5(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 O1 . 1.990(3) yes
Ni1 N1 . 2.012(3) yes
Ni1 O2W . 2.037(3) yes
Ni1 O1W . 2.040(3) yes
Ni1 N2 . 2.100(3) yes
Ni1 O5 . 2.148(3) yes
N1 C8 . 1.278(5) n
N1 N3 . 1.363(4) n
N2 C9 . 1.283(5) n
N2 O4 . 1.378(4) n
N3 C1 . 1.355(5) n
O1 C14 . 1.258(5) ?
O2 C14 . 1.261(5) ?
O3 C13 . 1.417(6) ?
O5 C1 . 1.241(5) n
O6 C7 . 1.321(5) n
C1 C2 . 1.473(5) ?
C2 C3 . 1.393(6) ?
C2 C7 . 1.413(5) ?
C3 C4 . 1.363(6) ?
C4 C5 . 1.396(7) ?
C5 C6 . 1.363(7) ?
C6 C7 . 1.410(6) ?
C8 C10 . 1.489(5) n
C8 C9 . 1.491(5) n
C9 C11 . 1.490(6) n
C12 C13 . 1.448(8) ?
C14 C15 . 1.504(6) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O4 H4A O2 . . . 2.576(5) 163 y
O1W H2 O6 2_355 2_355 . 2.688(5) 164 y
O2W H3 O6 2_255 2_255 . 2.658(5) 172 y
O1W H1 O3 . . . 2.754(4) 166 y
O2W H4 O3 1_655 1_655 . 2.773(5) 158 y
O3 H6A O2 . . 2_466 2.648(4) 173 y
N3 H3A O6 . . . ? ? y
