#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:33:56 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179335 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/32/4323278.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_4323278
loop_
_publ_author_name
'A. Döhring'
'R. Goddard'
'P. W. Jolly'
'C. Krüger'
'V. R. Polyakov'
_publ_section_title
;
 Monomer-Trimer Isomerism in 3-Substituted Pentane-2,4-dione Derivatives
 of Nickel(II)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              177
_journal_page_last               183
_journal_paper_doi               10.1021/ic960441c
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C30 H50 Ni O4'
_chemical_formula_weight         533.41
_chemical_name_common            'number 6'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                90.974(4)
_cell_angle_beta                 91.907(4)
_cell_angle_gamma                102.495(4)
_cell_formula_units_Z            1
_cell_length_a                   4.8067(2)
_cell_length_b                   8.2809(3)
_cell_length_c                   19.4014(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.9
_cell_measurement_theta_min      18.755
_cell_volume                     753.31(5)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.003
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3118
_diffrn_reflns_theta_max         74.93
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    1.156
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_F_000             290
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.0082(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.070
_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_restrained_S_obs      1.092
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_obs          0.0447
_refine_ls_shift/esd_max         -0.323
_refine_ls_shift/esd_mean        0.055
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0841P)²+0.1110P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1309
_refine_ls_wR_factor_obs         0.1292
_reflns_number_observed          2848
_reflns_number_total             3031
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960441c_3.cif
_cod_data_source_block           2068
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0841P)^2^+0.1110P] 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^)+(0.0841P)^2^+0.1110P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323278
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ni1 Ni 0.0000 0.0000 0.0000 0.0464(2) Uani 1 d S .
O1 O 0.2649(3) 0.1368(2) 0.05677(6) 0.0535(3) Uani 1 d . .
O2 O 0.1097(3) -0.1886(2) 0.02690(6) 0.0530(3) Uani 1 d . .
C1 C 0.6426(6) 0.2404(3) 0.13431(14) 0.0687(5) Uani 1 d . .
C2 C 0.4498(4) 0.0949(2) 0.09829(9) 0.0511(4) Uani 1 d . .
C3 C 0.4779(4) -0.0674(2) 0.10936(8) 0.0497(4) Uani 1 d . .
C4 C 0.3078(4) -0.2000(2) 0.07185(9) 0.0514(4) Uani 1 d . .
C5 C 0.3463(6) -0.3738(3) 0.07941(14) 0.0719(6) Uani 1 d . .
C6 C 0.6929(4) -0.0996(3) 0.16437(9) 0.0542(4) Uani 1 d . .
C7 C 0.5685(4) -0.1193(3) 0.23589(9) 0.0559(4) Uani 1 d . .
C8 C 0.7688(4) -0.1620(3) 0.29168(9) 0.0571(4) Uani 1 d . .
C9 C 0.6419(5) -0.1707(3) 0.36255(10) 0.0608(5) Uani 1 d . .
C10 C 0.8227(5) -0.2240(3) 0.42000(10) 0.0628(5) Uani 1 d . .
C11 C 0.6839(5) -0.2287(3) 0.48940(10) 0.0662(5) Uani 1 d . .
C12 C 0.8577(5) -0.2786(3) 0.54908(11) 0.0681(5) Uani 1 d . .
C13 C 0.7145(7) -0.2755(5) 0.61751(13) 0.0825(7) Uani 1 d . .
C14 C 0.8862(7) -0.3163(4) 0.67833(13) 0.0933(8) Uani 1 d . .
H14 H 1.0809(7) -0.2565(4) 0.68317(13) 0.080 Uiso 1 d R .
C15 C 0.8136(11) -0.4175(5) 0.7234(2) 0.1231(14) Uani 1 d . .
H15' H 0.6131(11) -0.4653(5) 0.7242(2) 0.080 Uiso 1 d R .
H7 H 0.5131(63) -0.0259(37) 0.2499(15) 0.089(8) Uiso 1 d . .
H11 H 0.6652(64) -0.1121(38) 0.5006(16) 0.089(8) Uiso 1 d . .
H9 H 0.6072(64) -0.0737(38) 0.3759(15) 0.087(8) Uiso 1 d . .
H7' H 0.4018(61) -0.1967(33) 0.2315(13) 0.077(7) Uiso 1 d . .
H8 H 0.8062(61) -0.2674(36) 0.2770(15) 0.083(8) Uiso 1 d . .
H6 H 0.7571(54) -0.1919(31) 0.1516(13) 0.067(6) Uiso 1 d . .
H10 H 0.8505(58) -0.3323(34) 0.4089(14) 0.075(7) Uiso 1 d . .
H6' H 0.8583(50) -0.0081(28) 0.1644(11) 0.058(6) Uiso 1 d . .
H12 H 0.8891(63) -0.3747(38) 0.5405(15) 0.085(9) Uiso 1 d . .
H8 H 0.9532(57) -0.0838(32) 0.2954(13) 0.073(7) Uiso 1 d . .
H5 H 0.3521(72) -0.4005(39) 0.1247(18) 0.099(9) Uiso 1 d . .
H12' H 1.0195(70) -0.1458(37) 0.4217(15) 0.093(9) Uiso 1 d . .
H13 H 0.6900(74) -0.1658(45) 0.6247(17) 0.107(11) Uiso 1 d . .
H9' H 0.4502(62) -0.2470(34) 0.3622(14) 0.082(8) Uiso 1 d . .
H11' H 0.5058(66) -0.3166(36) 0.4839(15) 0.087(8) Uiso 1 d . .
H1 H 0.6351(80) 0.2375(44) 0.1749(21) 0.114(12) Uiso 1 d . .
H1' H 0.6155(85) 0.3412(50) 0.1194(20) 0.117(12) Uiso 1 d . .
H5' H 0.2379(71) -0.4358(38) 0.0515(17) 0.096(10) Uiso 1 d . .
H15 H 0.9391(91) -0.4511(52) 0.7622(23) 0.142(15) Uiso 1 d . .
H5" H 0.5280(95) -0.3865(45) 0.0605(20) 0.126(13) Uiso 1 d . .
H13' H 0.5619(79) -0.3583(43) 0.6122(18) 0.103(11) Uiso 1 d . .
H1" H 0.8254(88) 0.2629(48) 0.1225(20) 0.118(13) Uiso 1 d . .
H12' H 1.0652(80) -0.2072(41) 0.5533(17) 0.106(10) Uiso 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 0.0181 0.0091 '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'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
O2 Ni1 O2 180.0 2 . ?
O2 Ni1 O1 85.81(5) 2 . ?
O2 Ni1 O1 94.19(5) . . ?
O2 Ni1 O1 94.19(5) 2 2 ?
O2 Ni1 O1 85.81(5) . 2 ?
O1 Ni1 O1 180.0 . 2 ?
C2 O1 Ni1 127.27(12) . . ?
C4 O2 Ni1 127.21(12) . . ?
C2 C1 H1 113.0(27) . . ?
C2 C1 H1' 113.8(23) . . ?
H1 C1 H1' 109.7(32) . . ?
C2 C1 H1" 116.6(26) . . ?
H1 C1 H1" 109.5(35) . . ?
H1' C1 H1" 92.4(29) . . ?
O1 C2 C3 125.2(2) . . ?
O1 C2 C1 112.8(2) . . ?
C3 C2 C1 121.9(2) . . ?
C4 C3 C2 120.8(2) . . ?
C4 C3 C6 119.8(2) . . ?
C2 C3 C6 119.4(2) . . ?
O2 C4 C3 125.3(2) . . ?
O2 C4 C5 112.9(2) . . ?
C3 C4 C5 121.9(2) . . ?
C4 C5 H5 110.9(21) . . ?
C4 C5 H5' 109.6(21) . . ?
H5 C5 H5' 120.1(27) . . ?
C4 C5 H5" 110.8(21) . . ?
H5 C5 H5" 106.6(30) . . ?
H5' C5 H5" 97.9(28) . . ?
C7 C6 C3 112.45(15) . . ?
C7 C6 H6 110.6(15) . . ?
C3 C6 H6 109.1(16) . . ?
C7 C6 H6' 110.8(13) . . ?
C3 C6 H6' 107.8(13) . . ?
H6 C6 H6' 105.8(19) . . ?
C8 C7 C6 114.4(2) . . ?
C8 C7 H7 108.1(19) . . ?
C6 C7 H7 111.1(18) . . ?
C8 C7 H7' 112.1(17) . . ?
C6 C7 H7' 106.9(17) . . ?
H7 C7 H7' 103.8(24) . . ?
C9 C8 C7 112.4(2) . . ?
C9 C8 H8 111.7(16) . . ?
C7 C8 H8 105.2(18) . . ?
C9 C8 H8 107.3(15) . . ?
C7 C8 H8 113.3(15) . . ?
H8 C8 H8 106.7(22) . . ?
C10 C9 C8 115.2(2) . . ?
C10 C9 H9 106.9(20) . . ?
C8 C9 H9 111.5(19) . . ?
C10 C9 H9' 107.4(16) . . ?
C8 C9 H9' 111.6(15) . . ?
H9 C9 H9' 103.5(24) . . ?
C11 C10 C9 112.4(2) . . ?
C11 C10 H10 108.6(16) . . ?
C9 C10 H10 108.8(16) . . ?
C11 C10 H12' 111.3(17) . . ?
C9 C10 H12' 108.5(17) . . ?
H10 C10 H12' 107.0(24) . . ?
C10 C11 C12 114.7(2) . . ?
C10 C11 H11 106.7(17) . . ?
C12 C11 H11 106.1(17) . . ?
C10 C11 H11' 105.1(17) . . ?
C12 C11 H11' 106.6(17) . . ?
H11 C11 H11' 118.1(24) . . ?
C13 C12 C11 112.6(2) . . ?
C13 C12 H12 110.6(20) . . ?
C11 C12 H12 109.4(20) . . ?
C13 C12 H12' 109.7(19) . . ?
C11 C12 H12' 112.8(18) . . ?
H12 C12 H12' 101.2(26) . . ?
C14 C13 C12 114.2(2) . . ?
C14 C13 H13 107.5(21) . . ?
C12 C13 H13 106.6(21) . . ?
C14 C13 H13' 106.6(22) . . ?
C12 C13 H13' 102.7(23) . . ?
H13 C13 H13' 119.6(30) . . ?
C15 C14 C13 129.1(4) . . ?
C15 C14 H14 114.3(3) . . ?
C13 C14 H14 116.7(2) . . ?
C14 C15 H15' 115.7(3) . . ?
C14 C15 H15 127.9(25) . . ?
H15' C15 H15 116.2(24) . . ?
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 O2 1.8318(12) 2 ?
Ni1 O2 1.8318(12) . ?
Ni1 O1 1.8326(13) . ?
Ni1 O1 1.8326(13) 2 ?
O1 C2 1.286(2) . ?
O2 C4 1.289(2) . ?
C1 C2 1.498(3) . ?
C1 H1 0.79(4) . ?
C1 H1' 0.92(4) . ?
C1 H1" 0.90(4) . ?
C2 C3 1.399(3) . ?
C3 C4 1.396(3) . ?
C3 C6 1.528(2) . ?
C4 C5 1.499(3) . ?
C5 H5 0.91(3) . ?
C5 H5' 0.83(3) . ?
C5 H5" 0.98(4) . ?
C6 C7 1.526(2) . ?
C6 H6 0.92(3) . ?
C6 H6' 0.97(2) . ?
C7 C8 1.522(2) . ?
C7 H7 0.91(3) . ?
C7 H7' 0.91(3) . ?
C8 C9 1.519(3) . ?
C8 H8 0.97(3) . ?
C8 H8 0.98(3) . ?
C9 C10 1.520(3) . ?
C9 H9 0.89(3) . ?
C9 H9' 1.00(3) . ?
C10 C11 1.520(3) . ?
C10 H10 0.96(3) . ?
C10 H12' 1.02(3) . ?
C11 C12 1.520(3) . ?
C11 H11 1.01(3) . ?
C11 H11' 1.00(3) . ?
C12 C13 1.518(3) . ?
C12 H12 0.86(3) . ?
C12 H12' 1.04(4) . ?
C13 C14 1.502(4) . ?
C13 H13 0.95(4) . ?
C13 H13' 0.89(4) . ?
C14 C15 1.227(4) . ?
C14 H14 0.96 . ?
C15 H15' 0.96 . ?
C15 H15 1.03(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
C3 C6 C7 C8 176.4(2) . . . . ?
C6 C7 C8 C9 176.8(2) . . . . ?
C7 C8 C9 C10 176.2(2) . . . . ?
C8 C9 C10 C11 179.6(2) . . . . ?
C9 C10 C11 C12 -179.1(2) . . . . ?
C10 C11 C12 C13 178.0(2) . . . . ?
C11 C12 C13 C14 -177.3(3) . . . . ?
C12 C13 C14 C15 -129.0(5) . . . . ?
