#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/27/2202767.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_2202767
loop_
_publ_author_name
'He, Xiao-Hui'
'Yao, Ying-Zheng'
'Luo, Xiang'
'Zhang, Ling'
'Wu, Qing'
_publ_section_title
Di-μ-acetylacetonato-bis[diacetylacetonato(tert-butylamine)nickel(II)]
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1196
_journal_page_last               m1197
_journal_paper_doi               10.1107/S1600536803026606
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Ni2 (C5 H7 O2)4 (C4 H11 N)2]'
_chemical_formula_moiety         'C28 H50 N2 Ni2 O8'
_chemical_formula_sum            'C28 H50 N2 Ni2 O8'
_chemical_formula_weight         660.12
_chemical_name_systematic
;
Di-μ-acetylacetonato-bis[diacetylacetonato(tert-butylamine)nickel(II)]
;
_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           SHELXL97
_cell_angle_alpha                110.555(2)
_cell_angle_beta                 99.252(2)
_cell_angle_gamma                100.637(2)
_cell_formula_units_Z            1
_cell_length_a                   9.0730(10)
_cell_length_b                   9.1410(10)
_cell_length_c                   11.5130(10)
_cell_measurement_reflns_used    972
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.7
_cell_measurement_theta_min      3.4
_cell_volume                     851.88(15)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.95
_diffrn_measured_fraction_theta_max 0.95
_diffrn_measurement_device_type  'Bruker Model area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.019
_diffrn_reflns_av_sigmaI/netI    0.036
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5189
_diffrn_reflns_theta_full        27.2
_diffrn_reflns_theta_max         27.2
_diffrn_reflns_theta_min         2.4
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.149
_exptl_absorpt_correction_T_max  0.847
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.39
_refine_diff_density_min         -0.78
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         3608
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.14
_refine_ls_R_factor_all          0.078
_refine_ls_R_factor_gt           0.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.1088P)²+0.8863P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.176
_refine_ls_wR_factor_ref         0.193
_reflns_number_gt                2817
_reflns_number_total             3608
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng6002.cif
_cod_data_source_block           I
_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:

'_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_values 1715 2011-07-08 13:25:40Z adriana 

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 
;
_cod_original_cell_volume        851.9(2)
_cod_database_code               2202767
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_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Ni1 0.47244(6) 0.35588(7) 0.36053(5) 0.0463(2) Uani d . 1 . . Ni
O1 0.3624(3) 0.4216(4) 0.5085(3) 0.0490(10) Uani d . 1 . . O
O2 0.3001(4) 0.1530(4) 0.2612(3) 0.0620(10) Uani d . 1 . . O
O3 0.5857(4) 0.2348(4) 0.4462(3) 0.0560(10) Uani d . 1 . . O
O4 0.5745(4) 0.2907(4) 0.2155(3) 0.0570(10) Uani d . 1 . . O
N1 0.3511(8) 0.4967(6) 0.2936(4) 0.101(2) Uani d D 1 . . N
C1 0.1502(7) 0.4331(9) 0.6033(6) 0.083(2) Uani d . 1 . . C
C2 0.2212(5) 0.3552(6) 0.4977(5) 0.0520(10) Uani d . 1 . . C
C3 0.1300(6) 0.2176(6) 0.3937(5) 0.0600(10) Uani d . 1 . . C
C4 0.1730(5) 0.1231(6) 0.2867(5) 0.0550(10) Uani d . 1 . . C
C5 0.0560(7) -0.0287(7) 0.1924(6) 0.079(2) Uani d . 1 . . C
C6 0.7031(7) 0.0333(8) 0.4638(6) 0.075(2) Uani d . 1 . . C
C7 0.6461(5) 0.1260(6) 0.3885(5) 0.0550(10) Uani d . 1 . . C
C8 0.6687(6) 0.0908(6) 0.2663(5) 0.0600(10) Uani d . 1 . . C
C9 0.6384(5) 0.1743(6) 0.1888(5) 0.0560(10) Uani d . 1 . . C
C10 0.6891(8) 0.1342(8) 0.0667(6) 0.081(2) Uani d . 1 . . C
C11 0.3090(6) 0.5115(6) 0.1725(4) 0.0670(10) Uani d D 1 . . C
C12 0.2620(8) 0.3536(7) 0.0645(5) 0.094(2) Uani d DU 1 . . C
C13 0.1970(10) 0.6050(10) 0.1687(9) 0.187(5) Uani d DU 1 . . C
C14 0.4570(10) 0.6050(10) 0.1585(9) 0.170(5) Uani d DU 1 . . C
H1N1 0.2599 0.4764 0.3139 0.121 Uiso calc R 1 . . H
H1N2 0.4010 0.5986 0.3481 0.121 Uiso calc R 1 . . H
H1A 0.1994 0.4241 0.6799 0.125 Uiso calc R 1 . . H
H1B 0.0419 0.3802 0.5803 0.125 Uiso calc R 1 . . H
H1C 0.1636 0.5454 0.6179 0.125 Uiso calc R 1 . . H
H3 0.0276 0.1844 0.3959 0.072 Uiso calc R 1 . . H
H5A -0.0338 -0.0015 0.1581 0.118 Uiso calc R 1 . . H
H5B 0.0269 -0.0992 0.2347 0.118 Uiso calc R 1 . . H
H5C 0.1001 -0.0824 0.1242 0.118 Uiso calc R 1 . . H
H6A 0.7597 0.1076 0.5485 0.113 Uiso calc R 1 . . H
H6B 0.7695 -0.0264 0.4221 0.113 Uiso calc R 1 . . H
H6C 0.6165 -0.0404 0.4688 0.113 Uiso calc R 1 . . H
H8 0.7082 0.0023 0.2328 0.071 Uiso calc R 1 . . H
H10A 0.6128 0.1423 0.0027 0.122 Uiso calc R 1 . . H
H10B 0.7008 0.0259 0.0385 0.122 Uiso calc R 1 . . H
H10C 0.7861 0.2086 0.0805 0.122 Uiso calc R 1 . . H
H12A 0.1679 0.2901 0.0690 0.142 Uiso calc R 1 . . H
H12B 0.3418 0.2983 0.0681 0.142 Uiso calc R 1 . . H
H12C 0.2455 0.3691 -0.0144 0.142 Uiso calc R 1 . . H
H13A 0.1012 0.5491 0.1770 0.280 Uiso calc R 1 . . H
H13B 0.1807 0.6174 0.0887 0.280 Uiso calc R 1 . . H
H13C 0.2351 0.7091 0.2378 0.280 Uiso calc R 1 . . H
H14A 0.4927 0.7096 0.2275 0.255 Uiso calc R 1 . . H
H14B 0.4379 0.6171 0.0784 0.255 Uiso calc R 1 . . H
H14C 0.5349 0.5466 0.1608 0.255 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 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
O1 Ni1 O1 . 2_666 79.70(10) yes
O1 Ni1 O2 . . 91.00(10) yes
O1 Ni1 O3 . . 90.00(10) yes
O1 Ni1 O4 . . 178.90(10) yes
O1 Ni1 N1 . . 83.5(2) yes
O1 Ni1 O2 2_666 . 170.70(10) yes
O1 Ni1 O3 2_666 . 88.80(10) yes
O1 Ni1 O4 2_666 . 101.20(10) yes
O1 Ni1 N1 2_666 . 87.7(2) yes
O2 Ni1 O3 . . 90.2(2) yes
O2 Ni1 O4 . . 88.10(10) yes
O2 Ni1 N1 . . 92.3(2) yes
O3 Ni1 O4 . . 90.70(10) yes
O3 Ni1 N1 . . 173.1(2) yes
O4 Ni1 N1 . . 95.9(2) yes
C2 O1 Ni1 . . 123.2(3) no
C2 O1 Ni1 . 2_666 134.8(3) no
Ni1 O1 Ni1 . 2_666 100.30(10) no
C4 O2 Ni1 . . 125.3(3) no
C7 O3 Ni1 . . 123.7(3) no
C9 O4 Ni1 . . 124.5(3) no
C11 N1 Ni1 . . 135.4(4) no
O1 C2 C3 . . 124.6(4) no
O1 C2 C1 . . 117.0(4) no
C3 C2 C1 . . 118.4(5) no
C2 C3 C4 . . 128.2(5) no
O2 C4 C3 . . 125.9(5) no
O2 C4 C5 . . 116.2(5) no
C3 C4 C5 . . 117.8(5) no
O3 C7 C8 . . 125.6(5) no
O3 C7 C6 . . 115.4(5) no
C8 C7 C6 . . 118.9(5) no
C7 C8 C9 . . 126.7(5) no
O4 C9 C8 . . 125.1(5) no
O4 C9 C10 . . 115.1(5) no
C8 C9 C10 . . 119.7(5) no
C13 C11 N1 . . 113.7(5) no
C13 C11 C12 . . 112.2(5) no
N1 C11 C12 . . 111.9(4) no
C13 C11 C14 . . 107.0(5) no
N1 C11 C14 . . 105.0(4) no
C12 C11 C14 . . 106.4(5) no
C11 N1 H1N1 . . 103.3 no
Ni1 N1 H1N1 . . 103.3 no
C11 N1 H1N2 . . 103.3 no
Ni1 N1 H1N2 . . 103.3 no
H1N1 N1 H1N2 . . 105.2 no
C2 C1 H1A . . 109.5 no
C2 C1 H1B . . 109.5 no
H1A C1 H1B . . 109.5 no
C2 C1 H1C . . 109.5 no
H1A C1 H1C . . 109.5 no
H1B C1 H1C . . 109.5 no
C2 C3 H3 . . 115.9 no
C4 C3 H3 . . 115.9 no
C4 C5 H5A . . 109.5 no
C4 C5 H5B . . 109.5 no
H5A C5 H5B . . 109.5 no
C4 C5 H5C . . 109.5 no
H5A C5 H5C . . 109.5 no
H5B C5 H5C . . 109.5 no
C7 C6 H6A . . 109.5 no
C7 C6 H6B . . 109.5 no
H6A C6 H6B . . 109.5 no
C7 C6 H6C . . 109.5 no
H6A C6 H6C . . 109.5 no
H6B C6 H6C . . 109.5 no
C7 C8 H8 . . 116.7 no
C9 C8 H8 . . 116.7 no
C9 C10 H10A . . 109.5 no
C9 C10 H10B . . 109.5 no
H10A C10 H10B . . 109.5 no
C9 C10 H10C . . 109.5 no
H10A C10 H10C . . 109.5 no
H10B C10 H10C . . 109.5 no
C11 C12 H12A . . 109.5 no
C11 C12 H12B . . 109.5 no
H12A C12 H12B . . 109.5 no
C11 C12 H12C . . 109.5 no
H12A C12 H12C . . 109.5 no
H12B C12 H12C . . 109.5 no
C11 C13 H13A . . 109.5 no
C11 C13 H13B . . 109.5 no
H13A C13 H13B . . 109.5 no
C11 C13 H13C . . 109.5 no
H13A C13 H13C . . 109.5 no
H13B C13 H13C . . 109.5 no
C11 C14 H14A . . 109.5 no
C11 C14 H14B . . 109.5 no
H14A C14 H14B . . 109.5 no
C11 C14 H14C . . 109.5 no
H14A C14 H14C . . 109.5 no
H14B C14 H14C . . 109.5 no
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 . 2.076(3) yes
Ni1 O1 2_666 2.156(3) yes
Ni1 O2 . 2.014(4) yes
Ni1 O3 . 2.028(3) yes
Ni1 O4 . 2.001(3) yes
Ni1 N1 . 2.100(4) yes
O1 C2 . 1.278(5) no
O2 C4 . 1.240(6) no
O3 C7 . 1.259(6) no
O4 C9 . 1.271(6) no
N1 C11 . 1.445(5) no
C1 C2 . 1.488(7) no
C2 C3 . 1.393(7) no
C3 C4 . 1.396(7) no
C4 C5 . 1.504(7) no
C6 C7 . 1.507(7) no
C7 C8 . 1.387(7) no
C8 C9 . 1.389(7) no
C9 C10 . 1.493(7) no
C11 C13 . 1.444(6) no
C11 C12 . 1.468(6) no
C11 C14 . 1.518(7) no
N1 H1N1 . 0.90 no
N1 H1N2 . 0.90 no
C1 H1A . 0.96 no
C1 H1B . 0.96 no
C1 H1C . 0.96 no
C3 H3 . 0.93 no
C5 H5A . 0.96 no
C5 H5B . 0.96 no
C5 H5C . 0.96 no
C6 H6A . 0.96 no
C6 H6B . 0.96 no
C6 H6C . 0.96 no
C8 H8 . 0.93 no
C10 H10A . 0.96 no
C10 H10B . 0.96 no
C10 H10C . 0.96 no
C12 H12A . 0.96 no
C12 H12B . 0.96 no
C12 H12C . 0.96 no
C13 H13A . 0.96 no
C13 H13B . 0.96 no
C13 H13C . 0.96 no
C14 H14A . 0.96 no
C14 H14B . 0.96 no
C14 H14C . 0.96 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1N2 O3 2_666 0.90 2.29 3.015(6) 137 no
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O2 Ni1 O1 C2 . . -13.9(4) no
O3 Ni1 O1 C2 . . -104.1(4) no
N1 Ni1 O1 C2 . . 78.3(4) no
O1 Ni1 O1 C2 2_666 . 167.1(4) no
O2 Ni1 O1 Ni1 . 2_666 179.00(10) no
O3 Ni1 O1 Ni1 . 2_666 88.80(10) no
N1 Ni1 O1 Ni1 . 2_666 -88.8(2) no
O1 Ni1 O1 Ni1 2_666 2_666 0.0 no
O4 Ni1 O2 C4 . . -167.3(4) no
O3 Ni1 O2 C4 . . 102.0(4) no
O1 Ni1 O2 C4 . . 12.0(4) no
N1 Ni1 O2 C4 . . -71.5(4) no
O4 Ni1 O3 C7 . . -19.1(4) no
O2 Ni1 O3 C7 . . 69.0(4) no
O1 Ni1 O3 C7 . . 160.0(4) no
O1 Ni1 O3 C7 2_666 . -120.2(4) no
O2 Ni1 O4 C9 . . -71.7(4) no
O3 Ni1 O4 C9 . . 18.5(4) no
N1 Ni1 O4 C9 . . -163.8(4) no
O1 Ni1 O4 C9 2_666 . 107.4(4) no
O4 Ni1 N1 C11 . . 17.1(6) no
O2 Ni1 N1 C11 . . -71.2(6) no
O1 Ni1 N1 C11 . . -162.0(6) no
O1 Ni1 N1 C11 2_666 . 118.1(6) no
Ni1 O1 C2 C3 . . 9.4(7) no
Ni1 O1 C2 C3 2_666 . 171.3(4) no
Ni1 O1 C2 C1 . . -169.7(4) no
Ni1 O1 C2 C1 2_666 . -7.8(7) no
O1 C2 C3 C4 . . 2.8(9) no
C1 C2 C3 C4 . . -178.1(6) no
Ni1 O2 C4 C3 . . -5.3(7) no
Ni1 O2 C4 C5 . . 174.4(4) no
C2 C3 C4 O2 . . -5.4(9) no
C2 C3 C4 C5 . . 174.8(5) no
Ni1 O3 C7 C8 . . 11.7(7) no
Ni1 O3 C7 C6 . . -171.0(3) no
O3 C7 C8 C9 . . 4.3(9) no
C6 C7 C8 C9 . . -173.0(5) no
Ni1 O4 C9 C8 . . -10.5(7) no
Ni1 O4 C9 C10 . . 172.5(4) no
C7 C8 C9 O4 . . -5.1(9) no
C7 C8 C9 C10 . . 171.8(5) no
Ni1 N1 C11 C13 . . 168.2(6) no
Ni1 N1 C11 C12 . . 39.9(8) no
Ni1 N1 C11 C14 . . -75.2(7) no
