#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/20/8102097.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_8102097
loop_
_publ_author_name
'Li, L.-Z.'
'Wang, L.-H.'
_publ_section_title
;
Crystal structure of hexaaquanickel(II) bis(bis(N-salicylideneglycinato-
O,O')nickelate(II)) dihydrate, [Ni(H₂O)₆][Ni(C₉H₇NO₃)₂] 
· H₂O
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              119
_journal_page_last               121
_journal_volume                  222
_journal_year                    2007
_chemical_formula_structural     '[Ni(H2O)6][Ni(C9H7NO3)2] &#x00B7; H2O'
_chemical_formula_sum            'C36 H44 N4 Ni3 O20'
_chemical_formula_weight         1028.88
_chemical_name_common
;
hexaaquanickel(II) 
bis(bis(((1-(2-hydroxyphenyl)methylidene)amino)acetato)nickel(II)) dihydrate
;
_chemical_name_systematic
; hexaaquanickel(II) bis(bis(N-salicylideneglycinato-O,O')nickelate(II)) 
  dihydrate
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.553(1)
_cell_length_b                   12.260(2)
_cell_length_c                   36.798(4)
_cell_measurement_reflns_used    2333
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      2.2
_cell_volume                     4309.8(10)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       omega
_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  0.1066
_diffrn_reflns_av_sigmaI/netI    0.0735
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            32789
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.11
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.381
_exptl_absorpt_correction_T_max  0.9597
_exptl_absorpt_correction_T_min  0.5754
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         4464
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0495P)²+6.4827P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1442
_reflns_number_gt                3152
_reflns_number_total             4464
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1974.cff
_cod_data_source_block           wang
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               8102097
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-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
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.46187(6) 0.45977(4) 0.137548(15) 0.03090(18) Uani 1 8 d d . . .
Ni2 Ni 1.0000 0.47443(7) 0.2500 0.0348(2) Uani 1 4 c d S . .
O1 O 0.5567(4) 0.5018(3) 0.09536(9) 0.0434(8) Uani 1 8 d d . . .
O2 O 0.3622(3) 0.4168(3) 0.18078(8) 0.0365(7) Uani 1 8 d d . . .
O3 O 0.3493(4) 0.2851(3) 0.22112(11) 0.0667(12) Uani 1 8 d d . . .
O4 O 0.3264(3) 0.3887(2) 0.10967(9) 0.0422(8) Uani 1 8 d d . . .
O5 O 0.6021(3) 0.5294(2) 0.16652(8) 0.0355(7) Uani 1 8 d d . . .
O6 O 0.6488(4) 0.6799(3) 0.19640(11) 0.0663(12) Uani 1 8 d d . . .
O7 O 0.8578(4) 0.5974(3) 0.24005(10) 0.0514(10) Uani 1 8 d d D . .
O8 O 0.8491(4) 0.3656(3) 0.23511(11) 0.0634(12) Uani 1 8 d d D . .
O9 O 1.0752(4) 0.4723(4) 0.19595(9) 0.0557(10) Uani 1 8 d d D . .
O10 O 0.8833(5) 0.4823(5) 0.14169(15) 0.0915(16) Uani 1 8 d d D . .
N1 N 0.5571(4) 0.3263(3) 0.14253(9) 0.0299(8) Uani 1 8 d d . . .
N2 N 0.3713(4) 0.5964(3) 0.13820(10) 0.0301(8) Uani 1 8 d d . . .
C1 C 0.6553(5) 0.3235(4) 0.08260(13) 0.0405(12) Uani 1 8 d d . . .
C2 C 0.6098(5) 0.4291(4) 0.07275(12) 0.0372(11) Uani 1 8 d d . . .
C3 C 0.6266(6) 0.4594(5) 0.03620(13) 0.0521(14) Uani 1 8 d d . . .
H3 H 0.5965 0.5278 0.0286 0.062 Uiso 1 8 d calc R . .
C4 C 0.6860(6) 0.3905(6) 0.01169(15) 0.0633(17) Uani 1 8 d d . . .
H4 H 0.6945 0.4126 -0.0124 0.076 Uiso 1 8 d calc R . .
C5 C 0.7339(7) 0.2891(6) 0.02156(16) 0.0678(18) Uani 1 8 d d . . .
H5 H 0.7752 0.2432 0.0045 0.081 Uiso 1 8 d calc R . .
C6 C 0.7196(6) 0.2569(4) 0.05683(15) 0.0517(14) Uani 1 8 d d . . .
H6 H 0.7536 0.1890 0.0639 0.062 Uiso 1 8 d calc R . .
C7 C 0.6332(5) 0.2808(4) 0.11842(13) 0.0375(11) Uani 1 8 d d . . .
H7 H 0.6772 0.2157 0.1245 0.045 Uiso 1 8 d calc R . .
C8 C 0.5331(5) 0.2768(4) 0.17804(13) 0.0407(12) Uani 1 8 d d . . .
H8A H 0.6136 0.2888 0.1936 0.049 Uiso 1 8 d calc R . .
H8B H 0.5196 0.1988 0.1754 0.049 Uiso 1 8 d calc R . .
C9 C 0.4051(5) 0.3276(4) 0.19471(13) 0.0389(11) Uani 1 8 d d . . .
C10 C 0.1971(4) 0.5516(4) 0.09394(12) 0.0343(10) Uani 1 8 d d . . .
C11 C 0.2309(5) 0.4392(4) 0.09127(12) 0.0345(10) Uani 1 8 d d . . .
C12 C 0.1515(6) 0.3763(5) 0.06658(14) 0.0518(14) Uani 1 8 d d . . .
H12 H 0.1725 0.3027 0.0636 0.062 Uiso 1 8 d calc R . .
C13 C 0.0444(6) 0.4214(6) 0.04702(16) 0.0653(17) Uani 1 8 d d . . .
H13 H -0.0086 0.3772 0.0318 0.078 Uiso 1 8 d calc R . .
C14 C 0.0129(6) 0.5317(5) 0.04945(16) 0.0613(16) Uani 1 8 d d . . .
H14 H -0.0585 0.5618 0.0355 0.074 Uiso 1 8 d calc R . .
C15 C 0.0891(5) 0.5951(5) 0.07280(13) 0.0479(13) Uani 1 8 d d . . .
H15 H 0.0685 0.6690 0.0747 0.057 Uiso 1 8 d calc R . .
C16 C 0.2669(4) 0.6235(4) 0.11865(12) 0.0329(10) Uani 1 8 d d . . .
H16 H 0.2338 0.6946 0.1206 0.039 Uiso 1 8 d calc R . .
C17 C 0.4363(5) 0.6731(4) 0.16370(15) 0.0495(14) Uani 1 8 d d . . .
H17A H 0.3746 0.6854 0.1842 0.059 Uiso 1 8 d calc R . .
H17B H 0.4529 0.7424 0.1518 0.059 Uiso 1 8 d calc R . .
C18 C 0.5726(5) 0.6255(4) 0.17656(14) 0.0411(12) Uani 1 8 d d . . .
H7B H 0.865(5) 0.650(3) 0.2550(13) 0.080 Uiso 1 8 d d D . .
H7A H 0.7725(19) 0.592(5) 0.2340(15) 0.080 Uiso 1 8 d d D . .
H8C H 0.867(6) 0.311(3) 0.2218(13) 0.080 Uiso 1 8 d d D . .
H8D H 0.787(5) 0.347(4) 0.2505(12) 0.080 Uiso 1 8 d d D . .
H9A H 1.021(4) 0.462(5) 0.1780(10) 0.080 Uiso 1 8 d d D . .
H9B H 1.157(2) 0.456(5) 0.1890(13) 0.080 Uiso 1 8 d d D . .
H10B H 0.802(3) 0.497(4) 0.1493(16) 0.080 Uiso 1 8 d d D . .
H10A H 0.891(6) 0.4142(13) 0.139(2) 0.080 Uiso 1 8 d d D . .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Ni1 O1 90.48(15) . . y
O4 Ni1 N1 89.00(14) . . y
O1 Ni1 N1 94.95(15) . . y
O4 Ni1 N2 95.96(14) . . y
O1 Ni1 N2 89.32(15) . . y
N1 Ni1 N2 173.44(16) . . y
O4 Ni1 O5 178.67(14) . . y
O1 Ni1 O5 90.01(15) . . y
N1 Ni1 O5 89.72(14) . . y
N2 Ni1 O5 85.28(14) . . y
O4 Ni1 O2 89.05(15) . . y
O1 Ni1 O2 179.39(14) . . y
N1 Ni1 O2 85.43(14) . . y
N2 Ni1 O2 90.34(14) . . y
O5 Ni1 O2 90.46(14) . . y
O8 Ni2 O8 98.3(3) . 3_755 y
O8 Ni2 O7 172.62(17) . 3_755 y
O8 Ni2 O7 88.01(17) 3_755 3_755 ?
O8 Ni2 O7 88.01(17) . . y
O8 Ni2 O7 172.62(17) 3_755 . ?
O7 Ni2 O7 86.0(2) 3_755 . y
O8 Ni2 O9 90.26(15) . 3_755 y
O8 Ni2 O9 88.83(16) 3_755 3_755 ?
O7 Ni2 O9 93.77(15) 3_755 3_755 ?
O7 Ni2 O9 87.25(16) . 3_755 y
O8 Ni2 O9 88.83(16) . . y
O8 Ni2 O9 90.26(15) 3_755 . ?
O7 Ni2 O9 87.25(16) 3_755 . ?
O7 Ni2 O9 93.77(15) . . y
O9 Ni2 O9 178.6(3) 3_755 . y
C2 O1 Ni1 121.5(3) . . ?
C9 O2 Ni1 114.1(3) . . ?
C11 O4 Ni1 123.5(3) . . ?
C18 O5 Ni1 114.9(3) . . ?
Ni2 O7 H7B 113(4) . . ?
Ni2 O7 H7A 129(4) . . ?
H7B O7 H7A 108(5) . . ?
Ni2 O8 H8C 122(4) . . ?
Ni2 O8 H8D 119(4) . . ?
H8C O8 H8D 108(3) . . ?
Ni2 O9 H9B 127(4) . . ?
Ni2 O9 H9A 122(4) . . ?
H9B O9 H9A 107(2) . . ?
H10B O10 H10A 109(3) . . ?
C7 N1 C8 122.1(4) . . ?
C7 N1 Ni1 126.0(3) . . ?
C8 N1 Ni1 111.9(3) . . ?
C16 N2 C17 121.7(4) . . ?
C16 N2 Ni1 125.7(3) . . ?
C17 N2 Ni1 112.5(3) . . ?
C6 C1 C2 119.9(5) . . ?
C6 C1 C7 118.5(5) . . ?
C2 C1 C7 121.7(4) . . ?
O1 C2 C3 118.0(5) . . ?
O1 C2 C1 125.1(4) . . ?
C3 C2 C1 116.9(5) . . ?
C4 C3 C2 121.3(6) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 121.7(5) . . ?
C3 C4 H4 119.1 . . ?
C5 C4 H4 119.1 . . ?
C6 C5 C4 118.7(5) . . ?
C6 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?
C5 C6 C1 121.5(6) . . ?
C5 C6 H6 119.3 . . ?
C1 C6 H6 119.3 . . ?
N1 C7 C1 124.3(4) . . ?
N1 C7 H7 117.8 . . ?
C1 C7 H7 117.8 . . ?
N1 C8 C9 108.7(4) . . ?
N1 C8 H8A 109.9 . . ?
C9 C8 H8A 109.9 . . ?
N1 C8 H8B 109.9 . . ?
C9 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
O3 C9 O2 122.9(4) . . ?
O3 C9 C8 120.2(4) . . ?
O2 C9 C8 116.9(4) . . ?
C15 C10 C11 120.0(4) . . ?
C15 C10 C16 117.5(4) . . ?
C11 C10 C16 122.4(4) . . ?
O4 C11 C12 117.0(4) . . ?
O4 C11 C10 126.1(4) . . ?
C12 C11 C10 116.9(4) . . ?
C13 C12 C11 121.3(5) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C12 C13 C14 121.5(5) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C15 C14 C13 118.6(5) . . ?
C15 C14 H14 120.7 . . ?
C13 C14 H14 120.7 . . ?
C14 C15 C10 121.7(5) . . ?
C14 C15 H15 119.2 . . ?
C10 C15 H15 119.2 . . ?
N2 C16 C10 124.2(4) . . ?
N2 C16 H16 117.9 . . ?
C10 C16 H16 117.9 . . ?
N2 C17 C18 108.6(4) . . ?
N2 C17 H17A 110.0 . . ?
C18 C17 H17A 110.0 . . ?
N2 C17 H17B 110.0 . . ?
C18 C17 H17B 110.0 . . ?
H17A C17 H17B 108.3 . . ?
O6 C18 O5 123.1(4) . . ?
O6 C18 C17 119.3(4) . . ?
O5 C18 C17 117.5(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 1.870(3) . y
Ni1 O2 1.927(3) . y
Ni1 O4 1.867(3) . y
Ni1 O5 1.913(3) . y
Ni1 N1 1.881(3) . y
Ni1 N2 1.885(3) . y
Ni2 O7 2.062(3) 3_755 ?
Ni2 O7 2.062(3) . y
Ni2 O8 2.039(4) . y
Ni2 O8 2.039(4) 3_755 ?
Ni2 O9 2.115(3) 3_755 ?
Ni2 O9 2.115(3) . y
O1 C2 1.320(6) . ?
O2 C9 1.275(5) . ?
O3 C9 1.224(5) . ?
O4 C11 1.294(5) . ?
O5 C18 1.266(5) . ?
O6 C18 1.228(5) . ?
O7 H7B 0.85(4) . ?
O7 H7A 0.848(10) . ?
O8 H8C 0.85(4) . ?
O8 H8D 0.85(5) . ?
O9 H9B 0.85(5) . ?
O9 H9A 0.85(5) . ?
O10 H10B 0.85(4) . ?
O10 H10A 0.845(10) . ?
N1 C7 1.276(5) . ?
N1 C8 1.459(6) . ?
N2 C16 1.274(5) . ?
N2 C17 1.466(6) . ?
C1 C6 1.394(6) . ?
C1 C2 1.413(7) . ?
C1 C7 1.434(7) . ?
C2 C3 1.404(6) . ?
C3 C4 1.360(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.373(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.363(7) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.503(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C10 C15 1.398(6) . ?
C10 C11 1.419(6) . ?
C10 C16 1.431(6) . ?
C11 C12 1.413(6) . ?
C12 C13 1.368(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.388(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.368(7) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C18 1.503(6) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
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
_geom_hbond_site_symmetry_A
O10 H10B O5 0.85(4) 2.05(3) 2.895(6) 178(6) .
O7 H7A O6 0.848(10) 2.11(5) 2.754(5) 132(5) .
O7 H7B O3 0.85(4) 1.88(4) 2.710(5) 165(5) 6_666
O8 H8D O3 0.85(5) 1.83(5) 2.676(5) 170(5) 3_655
O9 H9A O10 0.85(5) 1.89(2) 2.714(6) 163(6) .
O9 H9B O2 0.85(5) 2.04(3) 2.880(4) 171(5) 1_655
O8 H8C O6 0.85(4) 1.87(2) 2.686(5) 162(5) 8_755
