#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/87/2018725.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_2018725
loop_
_publ_author_name
'Trdin, Miha'
'Lah, Nina'
_publ_section_title
;
 A new polymorphic form of
 bis(acetato-κO)bis[2-(pyridin-2-yl)ethanol-κ²N,O]nickel(II)
;
_journal_coeditor_code           SK3457
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m359
_journal_page_last               m362
_journal_paper_doi               10.1107/S0108270112046422
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Ni (C2 H3 O2)2 (C7 H9 N O)2]'
_chemical_formula_moiety         'C18 H24 N2 Ni O6'
_chemical_formula_sum            'C18 H24 N2 Ni O6'
_chemical_formula_weight         423.10
_chemical_name_systematic
;
Bis(acetato-κO)bis[2-(pyridin-2-yl)ethanol-
κ²N,O]nickel(II)
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 131.175(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.4292(3)
_cell_length_b                   12.4129(4)
_cell_length_c                   12.0850(4)
_cell_measurement_reflns_used    2802
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.3609
_cell_measurement_theta_min      2.7705
_cell_volume                     951.76(6)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009) and
CrystalMaker (CrystalMaker, 2007)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 10.4933
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Agilent SuperNova (Dual, Cu at zero, Atlas)'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5104
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    1.056
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Agilent, 2011)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.336
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         2178
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0263P)²+0.3819P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0753
_reflns_number_gt                1862
_reflns_number_total             2178
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sk3457.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2018725
_cod_database_fobs_code          2018725
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_symmetry_multiplicity
Ni Ni1 0.5000 0.0000 0.5000 0.01492(11) Uani d S 1 2
N N11 0.2163(2) 0.04986(13) 0.29641(15) 0.0169(3) Uani d . 1 1
C C12 0.1659(3) 0.15434(15) 0.25796(18) 0.0199(4) Uani d . 1 1
C C13 -0.0312(3) 0.18454(16) 0.12683(19) 0.0243(4) Uani d . 1 1
H H13 -0.0649 0.2570 0.1033 0.029 Uiso calc R 1 1
C C14 -0.1762(3) 0.10616(17) 0.03208(19) 0.0259(4) Uani d . 1 1
H H14 -0.3069 0.1251 -0.0568 0.031 Uiso calc R 1 1
C C15 -0.1241(3) -0.00049(16) 0.0713(2) 0.0230(4) Uani d . 1 1
H H15 -0.2191 -0.0547 0.0092 0.028 Uiso calc R 1 1
C C16 0.0709(3) -0.02575(16) 0.20397(19) 0.0200(4) Uani d . 1 1
H H16 0.1039 -0.0978 0.2310 0.024 Uiso calc R 1 1
C C2A 0.3283(3) 0.23731(15) 0.36254(19) 0.0247(4) Uani d . 1 1
H H2A 0.2743 0.3081 0.3189 0.030 Uiso calc R 1 1
H H2B 0.4538 0.2250 0.3761 0.030 Uiso calc R 1 1
C C1A 0.3889(3) 0.23659(15) 0.51194(19) 0.0262(4) Uani d . 1 1
H H12A 0.4688 0.3011 0.5656 0.031 Uiso calc R 1 1
H H12B 0.2623 0.2371 0.4987 0.031 Uiso calc R 1 1
O O1A 0.51246(19) 0.14359(10) 0.59543(13) 0.0224(3) Uani d . 1 1
H H1A 0.4708 0.1178 0.6348 0.034 Uiso calc R 1 1
O O31 0.32257(18) -0.07155(10) 0.54228(13) 0.0200(3) Uani d . 1 1
O O32 0.3705(2) 0.04846(13) 0.70003(14) 0.0315(3) Uani d . 1 1
C C31 0.2984(3) -0.03858(16) 0.62914(18) 0.0211(4) Uani d . 1 1
C C32 0.1691(3) -0.10893(19) 0.6463(2) 0.0298(5) Uani d . 1 1
H H32A 0.1755 -0.0806 0.7231 0.045 Uiso calc R 1 1
H H32B 0.2245 -0.1809 0.6711 0.045 Uiso calc R 1 1
H H32C 0.0252 -0.1100 0.5556 0.045 Uiso calc R 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'
Ni Ni 0.3393 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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O31 Ni1 O31 3_656 . 180.0 ?
O31 Ni1 O1A . . 90.67(5) no
O31 Ni1 O1A 3_656 3_656 90.67(5) ?
O31 Ni1 O1A . 3_656 89.33(5) ?
O31 Ni1 N11 . . 87.99(5) no
O31 Ni1 N11 3_656 3_656 87.99(5) ?
O31 Ni1 N11 . 3_656 92.01(5) ?
O1A Ni1 N11 . . 89.99(5) no
O1A Ni1 N11 3_656 3_656 89.99(5) ?
O31 Ni1 N11 3_656 . 92.01(5) ?
O31 Ni1 N11 . . 87.99(5) ?
O1A Ni1 N11 3_656 . 90.01(5) ?
N11 Ni1 N11 3_656 . 180.0 ?
C12 N11 C16 . . 118.32(15) ?
C12 N11 Ni1 . . 123.00(11) ?
C16 N11 Ni1 . . 118.50(12) ?
N11 C12 C13 . . 121.28(16) ?
N11 C12 C2A . . 117.64(15) ?
C13 C12 C2A . . 121.07(17) ?
C14 C13 C12 . . 119.63(18) ?
C14 C13 H13 . . 120.2 ?
C12 C13 H13 . . 120.2 ?
C15 C14 C13 . . 118.97(17) ?
C15 C14 H14 . . 120.5 ?
C13 C14 H14 . . 120.5 ?
C14 C15 C16 . . 118.99(17) ?
C14 C15 H15 . . 120.5 ?
C16 C15 H15 . . 120.5 ?
N11 C16 C15 . . 122.76(18) ?
N11 C16 H16 . . 118.6 ?
C15 C16 H16 . . 118.6 ?
C12 C2A C1A . . 113.79(16) ?
C12 C2A H2A . . 108.8 ?
C1A C2A H2A . . 108.8 ?
C12 C2A H2B . . 108.8 ?
C1A C2A H2B . . 108.8 ?
H2A C2A H2B . . 107.7 ?
O1A C1A C2A . . 111.21(15) ?
O1A C1A H12A . . 109.4 ?
C2A C1A H12A . . 109.4 ?
O1A C1A H12B . . 109.4 ?
C2A C1A H12B . . 109.4 ?
H12A C1A H12B . . 108.0 ?
C1A O1A H1A . . 109.5 ?
C31 O31 Ni1 . . 127.18(12) ?
O32 C31 O31 . . 125.02(18) ?
O32 C31 C32 . . 118.08(17) ?
O31 C31 C32 . . 116.89(17) ?
C31 C32 H32A . . 109.5 ?
C31 C32 H32B . . 109.5 ?
H32A C32 H32B . . 109.5 ?
C31 C32 H32C . . 109.5 ?
H32A C32 H32C . . 109.5 ?
H32B C32 H32C . . 109.5 ?
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 O31 3_656 2.0719(12) no
Ni1 O31 . 2.0719(12) no
Ni1 O1A . 2.0877(13) no
Ni1 O1A 3_656 2.0877(13) no
Ni1 N11 3_656 2.0996(13) no
Ni1 N11 . 2.0996(13) no
N11 C12 . 1.349(2) no
N11 C16 . 1.352(2) no
C12 C13 . 1.395(2) no
C12 C2A . 1.501(2) no
C13 C14 . 1.381(3) no
C13 H13 . 0.9300 no
C14 C15 . 1.377(3) no
C14 H14 . 0.9300 no
C15 C16 . 1.379(3) no
C15 H15 . 0.9300 no
C16 H16 . 0.9300 no
C2A C1A . 1.519(3) no
C2A H2A . 0.9700 no
C2A H2B . 0.9700 no
C1A O1A . 1.432(2) no
C1A H12A . 0.9700 no
C1A H12B . 0.9700 no
O1A H1A . 0.8200 no
O31 C31 . 1.262(2) no
O32 C31 . 1.259(2) no
C31 C32 . 1.514(3) no
C32 H32A . 0.9600 no
C32 H32B . 0.9600 no
C32 H32C . 0.9600 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1A H1A O31 0.82 2.55 2.9585(18) 112
O1A H1A O32 0.82 1.72 2.533(2) 172
