#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:04:46 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180372 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/41/7204153.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_7204153
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            'C14 H25 N Ni O5'
_chemical_formula_weight         346.11
_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                105.97(8)
_cell_angle_beta                 104.33(11)
_cell_angle_gamma                97.56(11)
_cell_formula_units_Z            2
_cell_length_a                   7.737(8)
_cell_length_b                   10.309(7)
_cell_length_c                   11.812(8)
_cell_measurement_temperature    213(2)
_cell_volume                     857.2(14)
_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 0.911
_diffrn_measured_fraction_theta_max 0.911
_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  0.0851
_diffrn_reflns_av_sigmaI/netI    0.0940
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5380
_diffrn_reflns_theta_full        24.25
_diffrn_reflns_theta_max         24.25
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    1.15
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0463
_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)+(0.0512P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1141
_reflns_number_gt                1798
_reflns_number_total             2519
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103288g.txt
_cod_data_source_block           tony25
_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^)+(0.0512P)^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^)+(0.0512P)^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        857.2(12)
_cod_database_code               7204153
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 1.1023(7) -0.2381(6) 0.2176(5) 0.0536(14) Uani 1 d . . .
H1A H 0.9871 -0.2932 0.1591 0.064 Uiso 1 calc R . .
H1B H 1.1037 -0.2375 0.3001 0.064 Uiso 1 calc R . .
H1C H 1.2018 -0.2775 0.1964 0.064 Uiso 1 calc R . .
C2 C 1.1270(7) -0.1004(6) 0.0861(4) 0.0487(13) Uani 1 d . . .
H2A H 1.0131 -0.1566 0.0267 0.058 Uiso 1 calc R . .
H2B H 1.2280 -0.1397 0.0678 0.058 Uiso 1 calc R . .
H2C H 1.1416 -0.0072 0.0815 0.058 Uiso 1 calc R . .
C3 C 1.2995(6) -0.0101(5) 0.3018(4) 0.0410(12) Uani 1 d . . .
H3A H 1.3271 0.0759 0.2833 0.049 Uiso 1 calc R . .
H3B H 1.3980 -0.0593 0.2932 0.049 Uiso 1 calc R . .
C4 C 1.2900(6) 0.0230(6) 0.4326(4) 0.0436(13) Uani 1 d . . .
H4A H 1.2763 -0.0615 0.4553 0.052 Uiso 1 calc R . .
H4B H 1.4019 0.0873 0.4899 0.052 Uiso 1 calc R . .
C5 C 1.1385(8) 0.3996(6) 0.2274(5) 0.0604(15) Uani 1 d . . .
H5A H 1.1205 0.4916 0.2631 0.073 Uiso 1 calc R . .
H5B H 1.1010 0.3751 0.1382 0.073 Uiso 1 calc R . .
H5C H 1.2665 0.3977 0.2567 0.073 Uiso 1 calc R . .
C6 C 1.0247(6) 0.2967(5) 0.2653(4) 0.0365(11) Uani 1 d . . .
C7 C 0.9166(6) 0.3454(5) 0.3391(4) 0.0422(11) Uani 1 d . . .
H7 H 0.9255 0.4413 0.3678 0.051 Uiso 1 calc R . .
C8 C 0.7953(6) 0.2609(5) 0.3736(4) 0.0384(11) Uani 1 d . . .
C9 C 0.6748(6) 0.3320(6) 0.4431(4) 0.0476(12) Uani 1 d . . .
H9A H 0.7042 0.4305 0.4563 0.057 Uiso 1 calc R . .
H9B H 0.6957 0.3161 0.5222 0.057 Uiso 1 calc R . .
H9C H 0.5476 0.2949 0.3953 0.057 Uiso 1 calc R . .
C10 C 0.4993(6) -0.2102(6) -0.0717(4) 0.0524(14) Uani 1 d . . .
H10A H 0.4155 -0.2982 -0.0944 0.063 Uiso 1 calc R . .
H10B H 0.5755 -0.2168 -0.1262 0.063 Uiso 1 calc R . .
H10C H 0.4306 -0.1391 -0.0790 0.063 Uiso 1 calc R . .
C11 C 0.6186(6) -0.1734(5) 0.0603(4) 0.0364(11) Uani 1 d . . .
C12 C 0.5899(6) -0.2688(5) 0.1239(4) 0.0410(11) Uani 1 d . . .
H12 H 0.5022 -0.3512 0.0801 0.049 Uiso 1 calc R . .
C13 C 0.6822(6) -0.2491(5) 0.2464(4) 0.0379(11) Uani 1 d . . .
C14 C 0.6325(7) -0.3594(5) 0.3021(5) 0.0513(14) Uani 1 d . . .
H14A H 0.5355 -0.4329 0.2409 0.062 Uiso 1 calc R . .
H14B H 0.5915 -0.3193 0.3726 0.062 Uiso 1 calc R . .
H14C H 0.7388 -0.3965 0.3284 0.062 Uiso 1 calc R . .
O1 O 1.1359(4) 0.0840(4) 0.4376(3) 0.0388(8) Uani 1 d . . .
H1 H 1.1345 0.1123 0.5103 0.058 Uiso 1 calc R . .
O2 O 1.0373(4) 0.1728(4) 0.2242(3) 0.0380(8) Uani 1 d . . .
O3 O 0.7707(4) 0.1321(3) 0.3504(3) 0.0386(8) Uani 1 d . . .
O4 O 0.8099(4) -0.1455(3) 0.3185(3) 0.0353(7) Uani 1 d . . .
O5 O 0.7341(4) -0.0619(3) 0.1027(3) 0.0381(8) Uani 1 d . . .
N1 N 1.1241(5) -0.0966(4) 0.2132(3) 0.0362(9) Uani 1 d . . .
Ni1 Ni 0.92312(7) 0.01337(6) 0.26945(5) 0.0329(2) 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'
O O 0.0080 0.0060 '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'
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
N1 C3 C4 110.8(3) . . ?
O1 C4 C3 107.2(4) . . ?
O2 C6 C7 126.3(4) . . ?
O2 C6 C5 115.2(4) . . ?
C7 C6 C5 118.5(4) . . ?
C6 C7 C8 124.5(5) . . ?
O3 C8 C7 127.5(4) . . ?
O3 C8 C9 115.9(4) . . ?
C7 C8 C9 116.6(5) . . ?
O5 C11 C12 126.0(4) . . ?
O5 C11 C10 116.8(4) . . ?
C12 C11 C10 117.2(4) . . ?
C13 C12 C11 124.8(4) . . ?
O4 C13 C12 126.0(4) . . ?
O4 C13 C14 115.5(4) . . ?
C12 C13 C14 118.4(4) . . ?
C6 O2 Ni1 125.3(3) . . ?
C8 O3 Ni1 124.2(3) . . ?
C13 O4 Ni1 125.6(3) . . ?
C11 O5 Ni1 127.4(3) . . ?
C1 N1 C3 110.5(4) . . ?
C1 N1 C2 108.3(4) . . ?
C3 N1 C2 108.3(3) . . ?
C1 N1 Ni1 114.8(3) . . ?
C3 N1 Ni1 103.2(3) . . ?
C2 N1 Ni1 111.6(3) . . ?
O5 Ni1 O3 95.01(15) . . ?
O5 Ni1 O2 91.33(16) . . ?
O3 Ni1 O2 90.65(14) . . ?
O5 Ni1 O4 89.65(16) . . ?
O3 Ni1 O4 88.87(14) . . ?
O2 Ni1 O4 178.94(13) . . ?
O5 Ni1 N1 95.04(16) . . ?
O3 Ni1 N1 169.90(13) . . ?
O2 Ni1 N1 88.07(15) . . ?
O4 Ni1 N1 92.24(14) . . ?
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 N1 1.463(6) . ?
C2 N1 1.496(5) . ?
C3 N1 1.482(6) . ?
C3 C4 1.510(6) . ?
C4 O1 1.426(6) . ?
C5 C6 1.520(6) . ?
C6 O2 1.262(6) . ?
C6 C7 1.393(6) . ?
C7 C8 1.406(6) . ?
C8 O3 1.258(6) . ?
C8 C9 1.519(7) . ?
C10 C11 1.516(6) . ?
C11 O5 1.250(6) . ?
C11 C12 1.419(7) . ?
C12 C13 1.390(6) . ?
C13 O4 1.285(6) . ?
C13 C14 1.514(6) . ?
O2 Ni1 2.026(3) . ?
O3 Ni1 2.024(4) . ?
O4 Ni1 2.045(3) . ?
O5 Ni1 2.013(4) . ?
N1 Ni1 2.169(4) . ?
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
N1 C3 C4 O1 -54.5(5) . . . . ?
O2 C6 C7 C8 -3.9(7) . . . . ?
C5 C6 C7 C8 175.3(4) . . . . ?
C6 C7 C8 O3 4.0(8) . . . . ?
C6 C7 C8 C9 -173.7(4) . . . . ?
O5 C11 C12 C13 2.9(8) . . . . ?
C10 C11 C12 C13 -177.5(4) . . . . ?
C11 C12 C13 O4 -2.5(7) . . . . ?
C11 C12 C13 C14 178.5(4) . . . . ?
C7 C6 O2 Ni1 -6.8(6) . . . . ?
C5 C6 O2 Ni1 174.0(3) . . . . ?
C7 C8 O3 Ni1 6.6(6) . . . . ?
C9 C8 O3 Ni1 -175.7(3) . . . . ?
C12 C13 O4 Ni1 -4.0(6) . . . . ?
C14 C13 O4 Ni1 175.1(3) . . . . ?
C12 C11 O5 Ni1 3.4(7) . . . . ?
C10 C11 O5 Ni1 -176.2(3) . . . . ?
C4 C3 N1 C1 -73.7(5) . . . . ?
C4 C3 N1 C2 167.9(4) . . . . ?
C4 C3 N1 Ni1 49.5(4) . . . . ?
C11 O5 Ni1 O3 -95.6(4) . . . . ?
C11 O5 Ni1 O2 173.6(4) . . . . ?
C11 O5 Ni1 O4 -6.8(4) . . . . ?
C11 O5 Ni1 N1 85.4(4) . . . . ?
C8 O3 Ni1 O5 -103.3(4) . . . . ?
C8 O3 Ni1 O2 -11.9(3) . . . . ?
C8 O3 Ni1 O4 167.2(3) . . . . ?
C8 O3 Ni1 N1 70.7(8) . . . . ?
C6 O2 Ni1 O5 107.1(3) . . . . ?
C6 O2 Ni1 O3 12.1(3) . . . . ?
C6 O2 Ni1 O4 -51(7) . . . . ?
C6 O2 Ni1 N1 -157.9(3) . . . . ?
C13 O4 Ni1 O5 7.0(3) . . . . ?
C13 O4 Ni1 O3 102.1(4) . . . . ?
C13 O4 Ni1 O2 165(7) . . . . ?
C13 O4 Ni1 N1 -88.0(4) . . . . ?
C1 N1 Ni1 O5 -84.7(3) . . . . ?
C3 N1 Ni1 O5 154.9(2) . . . . ?
C2 N1 Ni1 O5 38.9(3) . . . . ?
C1 N1 Ni1 O3 101.2(8) . . . . ?
C3 N1 Ni1 O3 -19.1(8) . . . . ?
C2 N1 Ni1 O3 -135.1(7) . . . . ?
C1 N1 Ni1 O2 -175.9(3) . . . . ?
C3 N1 Ni1 O2 63.8(3) . . . . ?
C2 N1 Ni1 O2 -52.3(3) . . . . ?
C1 N1 Ni1 O4 5.1(3) . . . . ?
C3 N1 Ni1 O4 -115.2(3) . . . . ?
C2 N1 Ni1 O4 128.8(3) . . . . ?
