#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:04:46 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180372 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/41/7204154.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_7204154
loop_
_publ_author_name
'Williams, Paul A.'
'Jones, Anthony C.'
'Bickley, Jamie F.'
'Steiner, Alexander'
'Davies, Hywel O.'
'Leedham, Timothy J.'
'Impey, Susan A.'
'Garcia, Joanne'
'Allen, Stephen'
'Rougier, Aline'
'Blyr, Alexandra'
_publ_section_title
;
 Synthesis and crystal structures of dimethylaminoethanol adducts of
 Ni(ii) acetate and Ni(ii) acetylacetonate. Precursors for the sol--gel
 deposition of electrochromic nickel oxide thin films
;
_journal_issue                   9
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              2329
_journal_paper_doi               10.1039/b103288g
_journal_volume                  11
_journal_year                    2001
_chemical_formula_sum            'C12 H28 N2 Ni O6'
_chemical_formula_weight         355.13
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.917(19)
_cell_angle_beta                 95.92(2)
_cell_angle_gamma                109.469(19)
_cell_formula_units_Z            2
_cell_length_a                   8.2993(14)
_cell_length_b                   8.5256(14)
_cell_length_c                   13.017(2)
_cell_measurement_temperature    213(2)
_cell_volume                     854.4(3)
_computing_data_collection       'IPDS (STOE, 1997)'
_computing_data_reduction        'X-RED (STOE, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'Image plate'
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0607
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5492
_diffrn_reflns_theta_full        24.21
_diffrn_reflns_theta_max         24.21
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    1.161
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0391P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0755
_reflns_number_gt                1936
_reflns_number_total             2544
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103288g.txt
_cod_data_source_block           tony36
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+0.0000P] 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^)+(0.0391P)^2^+0.0000P] 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        854.4(2)
_cod_database_code               7204154
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2855(4) 0.3639(4) 0.0660(3) 0.0436(9) Uani 1 d . . .
H1A H 0.2165 0.4007 0.0145 0.052 Uiso 1 calc R . .
H1B H 0.3728 0.3338 0.0315 0.052 Uiso 1 calc R . .
C2 C 0.3733(4) 0.5053(4) 0.1547(3) 0.0401(8) Uani 1 d . . .
H2A H 0.4539 0.4736 0.2014 0.048 Uiso 1 calc R . .
H2B H 0.4397 0.6059 0.1269 0.048 Uiso 1 calc R . .
C3 C 0.3324(5) 0.6354(4) 0.3185(3) 0.0472(9) Uani 1 d . . .
H3A H 0.3838 0.5667 0.3556 0.057 Uiso 1 calc R . .
H3B H 0.2481 0.6604 0.3574 0.057 Uiso 1 calc R . .
H3C H 0.4218 0.7396 0.3112 0.057 Uiso 1 calc R . .
C4 C 0.1702(4) 0.6517(4) 0.1604(3) 0.0411(8) Uani 1 d . . .
H4A H 0.0865 0.6759 0.2002 0.049 Uiso 1 calc R . .
H4B H 0.1133 0.5946 0.0912 0.049 Uiso 1 calc R . .
H4C H 0.2607 0.7561 0.1547 0.049 Uiso 1 calc R . .
C5 C -0.2533(4) 0.1583(4) 0.0730(3) 0.0418(8) Uani 1 d . . .
H5A H -0.2097 0.0936 0.0233 0.050 Uiso 1 calc R . .
H5B H -0.3589 0.1680 0.0376 0.050 Uiso 1 calc R . .
C6 C -0.2939(4) 0.0679(4) 0.1651(3) 0.0397(8) Uani 1 d . . .
H6A H -0.3491 0.1260 0.2111 0.048 Uiso 1 calc R . .
H6B H -0.3747 -0.0468 0.1412 0.048 Uiso 1 calc R . .
C7 C -0.1619(5) 0.0306(5) 0.3304(3) 0.0470(9) Uani 1 d . . .
H7A H -0.1925 0.1205 0.3655 0.056 Uiso 1 calc R . .
H7B H -0.0568 0.0265 0.3684 0.056 Uiso 1 calc R . .
H7C H -0.2548 -0.0758 0.3279 0.056 Uiso 1 calc R . .
C8 C -0.0878(4) -0.0760(4) 0.1724(3) 0.0433(9) Uani 1 d . . .
H8A H 0.0171 -0.0794 0.2111 0.052 Uiso 1 calc R . .
H8B H -0.0692 -0.0577 0.1016 0.052 Uiso 1 calc R . .
H8C H -0.1809 -0.1819 0.1709 0.052 Uiso 1 calc R . .
C9 C 0.3215(4) 0.1740(4) 0.3228(3) 0.0337(8) Uani 1 d . . .
C10 C 0.4068(6) 0.1370(6) 0.4205(3) 0.0642(12) Uani 1 d . . .
H10A H 0.4809 0.0746 0.4020 0.077 Uiso 1 calc R . .
H10B H 0.3190 0.0706 0.4577 0.077 Uiso 1 calc R . .
H10C H 0.4754 0.2417 0.4647 0.077 Uiso 1 calc R . .
C11 C -0.1535(4) 0.4867(4) 0.3231(3) 0.0326(7) Uani 1 d . . .
C12 C -0.1884(6) 0.5746(6) 0.4195(3) 0.0615(12) Uani 1 d . . .
H12A H -0.2740 0.6251 0.4004 0.074 Uiso 1 calc R . .
H12B H -0.0824 0.6615 0.4539 0.074 Uiso 1 calc R . .
H12C H -0.2315 0.4940 0.4664 0.074 Uiso 1 calc R . .
N1 N 0.2461(3) 0.5433(3) 0.21378(19) 0.0284(6) Uani 1 d . . .
N2 N -0.1339(3) 0.0620(3) 0.22357(19) 0.0290(6) Uani 1 d . . .
O1 O 0.1761(3) 0.2204(3) 0.10412(16) 0.0321(5) Uani 1 d . . .
H1 H 0.2364 0.1808 0.1409 0.048 Uiso 1 calc R . .
O2 O -0.1267(2) 0.3224(3) 0.10546(16) 0.0310(5) Uani 1 d . . .
H2 H -0.1669 0.3799 0.1434 0.046 Uiso 1 calc R . .
O3 O 0.3523(3) 0.1186(3) 0.23721(18) 0.0428(6) Uani 1 d . . .
O4 O 0.2205(3) 0.2551(3) 0.33483(15) 0.0311(5) Uani 1 d . . .
O5 O -0.0442(3) 0.4141(3) 0.33457(16) 0.0320(5) Uani 1 d . . .
O6 O -0.2330(3) 0.4923(3) 0.23641(18) 0.0417(6) Uani 1 d . . .
Ni1 Ni 0.05745(5) 0.30424(5) 0.22361(3) 0.02292(13) Uani 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0020 0.0020 '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 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.2850 1.1130 '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
O1 C1 C2 110.3(3) . . ?
N1 C2 C1 110.9(3) . . ?
O2 C5 C6 110.6(3) . . ?
N2 C6 C5 110.3(2) . . ?
O3 C9 O4 125.7(3) . . ?
O3 C9 C10 117.7(3) . . ?
O4 C9 C10 116.6(3) . . ?
O6 C11 O5 124.6(3) . . ?
O6 C11 C12 118.0(3) . . ?
O5 C11 C12 117.4(3) . . ?
C2 N1 C4 110.3(3) . . ?
C2 N1 C3 109.6(2) . . ?
C4 N1 C3 107.7(3) . . ?
C2 N1 Ni1 105.47(19) . . ?
C4 N1 Ni1 112.24(18) . . ?
C3 N1 Ni1 111.5(2) . . ?
C7 N2 C8 108.3(3) . . ?
C7 N2 C6 109.7(2) . . ?
C8 N2 C6 109.8(2) . . ?
C7 N2 Ni1 111.24(19) . . ?
C8 N2 Ni1 112.60(19) . . ?
C6 N2 Ni1 105.2(2) . . ?
C9 O4 Ni1 128.7(2) . . ?
C11 O5 Ni1 129.2(2) . . ?
O5 Ni1 O4 91.87(8) . . ?
O5 Ni1 N1 90.64(9) . . ?
O4 Ni1 N1 91.91(9) . . ?
O5 Ni1 N2 91.78(9) . . ?
O4 Ni1 N2 90.38(9) . . ?
N1 Ni1 N2 176.61(10) . . ?
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
C1 O1 1.430(4) . ?
C1 C2 1.507(5) . ?
C2 N1 1.467(4) . ?
C3 N1 1.480(4) . ?
C4 N1 1.471(4) . ?
C5 O2 1.431(4) . ?
C5 C6 1.499(5) . ?
C6 N2 1.480(4) . ?
C7 N2 1.471(4) . ?
C8 N2 1.471(4) . ?
C9 O3 1.249(4) . ?
C9 O4 1.263(4) . ?
C9 C10 1.504(5) . ?
C11 O6 1.260(4) . ?
C11 O5 1.263(4) . ?
C11 C12 1.498(5) . ?
N1 Ni1 2.142(3) . ?
N2 Ni1 2.145(3) . ?
O4 Ni1 2.050(2) . ?
O5 Ni1 2.043(2) . ?
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
O1 H1 O3 0.83 1.73 2.554(3) 169.2 .
O2 H2 O6 0.83 1.71 2.536(3) 171.8 .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 N1 -54.2(4) . . . . ?
O2 C5 C6 N2 -55.5(4) . . . . ?
C1 C2 N1 C4 -81.4(3) . . . . ?
C1 C2 N1 C3 160.2(3) . . . . ?
C1 C2 N1 Ni1 40.0(3) . . . . ?
C5 C6 N2 C7 159.7(3) . . . . ?
C5 C6 N2 C8 -81.4(3) . . . . ?
C5 C6 N2 Ni1 40.0(3) . . . . ?
O3 C9 O4 Ni1 6.4(5) . . . . ?
C10 C9 O4 Ni1 -171.4(3) . . . . ?
O6 C11 O5 Ni1 6.3(5) . . . . ?
C12 C11 O5 Ni1 -172.7(2) . . . . ?
C11 O5 Ni1 O4 175.8(3) . . . . ?
C11 O5 Ni1 N1 83.8(3) . . . . ?
C11 O5 Ni1 N2 -93.8(3) . . . . ?
C9 O4 Ni1 O5 174.7(3) . . . . ?
C9 O4 Ni1 N1 -94.6(3) . . . . ?
C9 O4 Ni1 N2 82.9(3) . . . . ?
C2 N1 Ni1 O5 167.17(19) . . . . ?
C4 N1 Ni1 O5 -72.7(2) . . . . ?
C3 N1 Ni1 O5 48.2(2) . . . . ?
C2 N1 Ni1 O4 75.28(19) . . . . ?
C4 N1 Ni1 O4 -164.6(2) . . . . ?
C3 N1 Ni1 O4 -43.7(2) . . . . ?
C2 N1 Ni1 N2 -57.2(18) . . . . ?
C4 N1 Ni1 N2 63.0(18) . . . . ?
C3 N1 Ni1 N2 -176.1(16) . . . . ?
C7 N2 Ni1 O5 -43.0(2) . . . . ?
C8 N2 Ni1 O5 -164.7(2) . . . . ?
C6 N2 Ni1 O5 75.72(19) . . . . ?
C7 N2 Ni1 O4 48.9(2) . . . . ?
C8 N2 Ni1 O4 -72.8(2) . . . . ?
C6 N2 Ni1 O4 167.61(19) . . . . ?
C7 N2 Ni1 N1 -178.6(16) . . . . ?
C8 N2 Ni1 N1 59.6(18) . . . . ?
C6 N2 Ni1 N1 -59.9(18) . . . . ?
