#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/08/2220870.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_2220870
loop_
_publ_author_name
'Hunter, Gerald O.'
'Zeller, Matthias'
'Leskiw, Brian D.'
_publ_section_title
;cis-[Aqua/methanol(0.45/1.55)](1,1,1-trifluoro-5,5-dimethylhexane-2,4-dionato)nickel(II)--cis-[aqua/methanol(1.49/0.51)](1,1,1-trifluoro-5,5-dimethylhexane-2,4-dionato)nickel(II)
 (1/1)
;
_journal_coeditor_code           LX2082
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m221
_journal_page_last               m222
_journal_paper_doi               10.1107/S1600536809001846
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac
;
[Ni (C8 H10 F3 O2)2 (C H4 O)1.55 (H2 O1)0.45]
[Ni (C8 H10 F3 O2)2 (C H4 O)0.51 (H2 O1)1.49]
;
_chemical_formula_moiety
'C17.55 H27.09 F6 Ni O6, C16.51 H25.02 F6 Ni O6'
_chemical_formula_sum            'C34.05 H52.11 F12 Ni2 O12'
_chemical_formula_weight         998.89
_chemical_name_systematic
;cis-[Aqua/methanol(0.45/1.55)](1,1,1-trifluoro-5,5-dimethylhexane-
2,4-dionato)nickel(II)--cis-[aqua/methanol(1.49/0.51)](1,1,1-trifluoro-
5,5-dimethylhexane-2,4-dionato)nickel(II)
 (1/1)
;
_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                101.379(3)
_cell_angle_beta                 104.946(3)
_cell_angle_gamma                107.678(3)
_cell_formula_units_Z            2
_cell_length_a                   11.327(2)
_cell_length_b                   14.701(3)
_cell_length_c                   15.432(3)
_cell_measurement_reflns_used    3507
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.81
_cell_measurement_theta_min      2.34
_cell_volume                     2257.0(8)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       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  0.0750
_diffrn_reflns_av_sigmaI/netI    0.1569
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22225
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.43
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.937
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(APEX2; Bruker, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1032.9
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.602
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         10979
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1690
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0561P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1548
_reflns_number_gt                5010
_reflns_number_total             10979
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            lx2082.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 
;
_cod_original_sg_symbol_Hall     -P_1
_cod_database_code               2220870
_cod_database_fobs_code          2220870
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_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
C C1 0.2154(5) 0.0370(4) 0.2924(4) 0.0382(13) Uani d . 1 . .
C C2 0.2772(4) 0.1381(3) 0.2784(3) 0.0271(11) Uani d . 1 . .
C C3 0.3419(4) 0.1443(3) 0.2152(3) 0.0262(11) Uani d . 1 . .
H H3 0.3423 0.0836 0.1800 0.031 Uiso calc R 1 . .
C C4 0.4089(4) 0.2337(4) 0.1973(3) 0.0227(10) Uani d . 1 . .
C C5 0.4801(4) 0.2298(3) 0.1255(3) 0.0275(11) Uani d . 1 . .
C C6 0.5271(5) 0.1424(4) 0.1132(4) 0.0398(13) Uani d . 1 . .
H H6A 0.5862 0.1463 0.1738 0.060 Uiso calc R 1 . .
H H6B 0.5742 0.1458 0.0681 0.060 Uiso calc R 1 . .
H H6C 0.4509 0.0790 0.0896 0.060 Uiso calc R 1 . .
C C7 0.6002(5) 0.3285(4) 0.1560(4) 0.0366(13) Uani d . 1 . .
H H7A 0.5707 0.3849 0.1606 0.055 Uiso calc R 1 . .
H H7B 0.6448 0.3271 0.1095 0.055 Uiso calc R 1 . .
H H7C 0.6614 0.3362 0.2174 0.055 Uiso calc R 1 . .
C C8 0.3812(5) 0.2206(4) 0.0314(3) 0.0324(12) Uani d . 1 . .
H H8A 0.3035 0.1589 0.0127 0.049 Uiso calc R 1 . .
H H8B 0.4227 0.2187 -0.0169 0.049 Uiso calc R 1 . .
H H8C 0.3543 0.2783 0.0387 0.049 Uiso calc R 1 . .
C C9 -0.0415(5) 0.3477(5) 0.3914(4) 0.0423(14) Uani d . 1 . .
C C10 0.0368(5) 0.3223(4) 0.3293(3) 0.0282(11) Uani d . 1 . .
C C11 -0.0341(4) 0.2624(4) 0.2390(3) 0.0319(12) Uani d . 1 . .
H H11 -0.1273 0.2345 0.2219 0.038 Uiso calc R 1 . .
C C12 0.0219(4) 0.2388(3) 0.1682(3) 0.0255(11) Uani d . 1 . .
C C13 -0.0694(5) 0.1722(4) 0.0695(3) 0.0321(12) Uani d . 1 . .
C C14 0.0128(5) 0.1427(4) 0.0125(3) 0.0442(14) Uani d . 1 . .
H H14A 0.0772 0.2032 0.0099 0.066 Uiso calc R 1 . .
H H14B -0.0453 0.1014 -0.0514 0.066 Uiso calc R 1 . .
H H14C 0.0591 0.1046 0.0426 0.066 Uiso calc R 1 . .
C C15 -0.1688(5) 0.0761(4) 0.0745(4) 0.0431(14) Uani d . 1 . .
H H15A -0.2250 0.0332 0.0107 0.065 Uiso calc R 1 . .
H H15B -0.2237 0.0942 0.1093 0.065 Uiso calc R 1 . .
H H15C -0.1209 0.0402 0.1067 0.065 Uiso calc R 1 . .
C C16 -0.1424(5) 0.2326(4) 0.0233(3) 0.0419(14) Uani d . 1 . .
H H16A -0.0781 0.2943 0.0226 0.063 Uiso calc R 1 . .
H H16B -0.1966 0.2495 0.0593 0.063 Uiso calc R 1 . .
H H16C -0.1989 0.1926 -0.0413 0.063 Uiso calc R 1 . .
C C17 0.2152(9) 0.5096(8) 0.2473(7) 0.033(3) Uani d P 0.508(12) A 1
H H17A 0.1703 0.4709 0.1808 0.050 Uiso calc PR 0.508(12) A 1
H H17B 0.2522 0.5809 0.2530 0.050 Uiso calc PR 0.508(12) A 1
H H17C 0.1521 0.4986 0.2809 0.050 Uiso calc PR 0.508(12) A 1
C C18 0.6284(5) 0.2615(4) 0.5218(3) 0.0374(13) Uani d . 1 . .
C C19 0.5238(5) 0.2489(4) 0.5689(3) 0.0295(11) Uani d . 1 . .
C C20 0.5083(5) 0.1814(4) 0.6188(3) 0.0332(12) Uani d . 1 . .
H H20 0.5686 0.1481 0.6259 0.040 Uiso calc R 1 . .
C C21 0.4099(5) 0.1568(4) 0.6610(3) 0.0343(12) Uani d . 1 . .
C C22 0.4030(6) 0.0779(4) 0.7129(4) 0.0468(15) Uani d . 1 . .
C C23 0.3917(8) -0.0193(4) 0.6472(4) 0.073(2) Uani d . 1 . .
H H23A 0.3114 -0.0435 0.5922 0.110 Uiso calc R 1 . .
H H23B 0.3880 -0.0698 0.6805 0.110 Uiso calc R 1 . .
H H23C 0.4686 -0.0069 0.6267 0.110 Uiso calc R 1 . .
C C24 0.5299(6) 0.1188(4) 0.7993(4) 0.0576(17) Uani d . 1 . .
H H24A 0.6068 0.1340 0.7787 0.086 Uiso calc R 1 . .
H H24B 0.5297 0.0685 0.8326 0.086 Uiso calc R 1 . .
H H24C 0.5341 0.1798 0.8415 0.086 Uiso calc R 1 . .
C C25 0.2841(7) 0.0601(5) 0.7459(4) 0.0661(19) Uani d . 1 . .
H H25A 0.2927 0.1229 0.7881 0.099 Uiso calc R 1 . .
H H25B 0.2800 0.0098 0.7795 0.099 Uiso calc R 1 . .
H H25C 0.2033 0.0363 0.6914 0.099 Uiso calc R 1 . .
C C26 0.5696(5) 0.4356(4) 0.8933(3) 0.0320(12) Uani d . 1 . .
C C27 0.4424(4) 0.4033(3) 0.8111(3) 0.0251(11) Uani d . 1 . .
C C28 0.3258(4) 0.3757(3) 0.8271(3) 0.0291(11) Uani d . 1 . .
H H28 0.3273 0.3768 0.8891 0.035 Uiso calc R 1 . .
C C29 0.2011(5) 0.3452(4) 0.7550(3) 0.0302(11) Uani d . 1 B .
C C30 0.0798(5) 0.3395(4) 0.7834(3) 0.0377(13) Uani d . 1 . .
C C31 -0.0429(8) 0.2896(9) 0.6985(6) 0.054(3) Uani d P 0.687(9) B 1
H H31A -0.1201 0.2843 0.7177 0.081 Uiso calc PR 0.687(9) B 1
H H31B -0.0487 0.2225 0.6679 0.081 Uiso calc PR 0.687(9) B 1
H H31C -0.0399 0.3293 0.6545 0.081 Uiso calc PR 0.687(9) B 1
C C32 0.0967(8) 0.4400(7) 0.8317(7) 0.053(3) Uani d P 0.687(9) B 1
H H32A 0.1105 0.4826 0.7909 0.080 Uiso calc PR 0.687(9) B 1
H H32B 0.1734 0.4668 0.8896 0.080 Uiso calc PR 0.687(9) B 1
H H32C 0.0178 0.4386 0.8473 0.080 Uiso calc PR 0.687(9) B 1
C C33 0.0716(8) 0.2709(7) 0.8505(6) 0.048(3) Uani d P 0.687(9) B 1
H H33A 0.1459 0.3047 0.9098 0.073 Uiso calc PR 0.687(9) B 1
H H33B 0.0753 0.2071 0.8201 0.073 Uiso calc PR 0.687(9) B 1
H H33C -0.0113 0.2584 0.8633 0.073 Uiso calc PR 0.687(9) B 1
C C31B 0.0110(18) 0.4102(13) 0.7309(13) 0.052(6) Uani d P 0.313(9) B 2
H H31D -0.0289 0.3769 0.6631 0.078 Uiso calc PR 0.313(9) B 2
H H31E 0.0790 0.4757 0.7429 0.078 Uiso calc PR 0.313(9) B 2
H H31F -0.0569 0.4191 0.7564 0.078 Uiso calc PR 0.313(9) B 2
C C32B 0.1036(17) 0.3959(16) 0.8881(12) 0.050(6) Uani d P 0.313(9) B 2
H H32D 0.0189 0.3915 0.8956 0.076 Uiso calc PR 0.313(9) B 2
H H32E 0.1600 0.4664 0.9033 0.076 Uiso calc PR 0.313(9) B 2
H H32F 0.1467 0.3650 0.9305 0.076 Uiso calc PR 0.313(9) B 2
C C33B -0.017(2) 0.2381(15) 0.746(2) 0.091(12) Uani d P 0.313(9) B 2
H H33D 0.0248 0.1920 0.7636 0.136 Uiso calc PR 0.313(9) B 2
H H33E -0.0524 0.2204 0.6771 0.136 Uiso calc PR 0.313(9) B 2
H H33F -0.0888 0.2333 0.7712 0.136 Uiso calc PR 0.313(9) B 2
C C34 0.0684(6) 0.1373(5) 0.4794(4) 0.069(2) Uani d . 1 B .
H H34A 0.0956 0.0816 0.4885 0.104 Uiso calc R 1 . .
H H34B 0.0012 0.1164 0.4172 0.104 Uiso calc R 1 . .
H H34C 0.0320 0.1569 0.5279 0.104 Uiso calc R 1 . .
C C35 0.2792(10) 0.5035(7) 0.6105(7) 0.038(3) Uani d P 0.546(15) B 1
H H35A 0.1921 0.4725 0.6149 0.057 Uiso calc PR 0.546(15) B 1
H H35B 0.2785 0.5554 0.5794 0.057 Uiso calc PR 0.546(15) B 1
H H35C 0.3453 0.5335 0.6738 0.057 Uiso calc PR 0.546(15) B 1
F F1 0.2653(4) 0.0395(2) 0.3817(2) 0.0601(10) Uani d . 1 . .
F F2 0.2309(3) -0.0384(2) 0.2390(2) 0.0493(8) Uani d . 1 . .
F F3 0.0859(3) 0.0125(2) 0.2729(2) 0.0579(9) Uani d . 1 . .
F F4 0.0066(3) 0.3460(3) 0.4771(2) 0.0767(13) Uani d . 1 . .
F F5 -0.1676(3) 0.2897(3) 0.3588(2) 0.0867(14) Uani d . 1 . .
F F6 -0.0380(5) 0.4389(4) 0.3985(3) 0.1089(18) Uani d . 1 . .
F F7 0.7002(3) 0.2064(2) 0.5379(2) 0.0514(9) Uani d . 1 . .
F F8 0.7119(3) 0.3569(2) 0.5511(2) 0.0502(8) Uani d . 1 . .
F F9 0.5724(3) 0.2372(2) 0.42870(19) 0.0478(8) Uani d . 1 . .
F F10 0.6442(3) 0.3849(2) 0.8754(2) 0.0463(8) Uani d . 1 . .
F F11 0.5512(3) 0.4239(2) 0.97410(18) 0.0427(8) Uani d . 1 . .
F F12 0.6426(3) 0.53284(19) 0.91291(18) 0.0367(7) Uani d . 1 . .
Ni Ni1 0.28898(6) 0.34142(4) 0.30511(4) 0.02390(16) Uani d . 1 A .
Ni Ni2 0.32213(6) 0.31408(5) 0.61117(4) 0.02661(17) Uani d . 1 B .
O O1 0.2590(3) 0.2076(2) 0.3312(2) 0.0269(7) Uani d . 1 . .
O O2 0.4093(3) 0.3171(2) 0.2352(2) 0.0236(7) Uani d . 1 . .
O O3 0.1611(3) 0.3641(2) 0.3708(2) 0.0265(7) Uani d . 1 . .
O O4 0.1419(3) 0.2711(2) 0.1825(2) 0.0271(8) Uani d . 1 . .
O O5 0.3153(3) 0.4793(2) 0.2856(2) 0.0305(8) Uani d D 1 . .
H H5A 0.382(3) 0.511(3) 0.277(3) 0.046 Uiso d D 1 . .
H H5B 0.311(7) 0.509(5) 0.336(4) 0.046 Uiso d PD 0.492(12) A 2
O O6 0.4469(3) 0.4085(2) 0.4268(2) 0.0300(8) Uani d D 1 . .
H H6D 0.455(5) 0.369(3) 0.458(3) 0.045 Uiso d D 1 . .
H H6E 0.518(3) 0.442(3) 0.426(4) 0.045 Uiso d D 1 . .
O O7 0.4599(3) 0.3051(2) 0.5532(2) 0.0271(7) Uani d . 1 . .
O O8 0.3270(3) 0.1969(2) 0.6578(2) 0.0325(8) Uani d . 1 . .
O O9 0.4634(3) 0.4058(2) 0.7340(2) 0.0274(7) Uani d . 1 . .
O O10 0.1850(3) 0.3252(3) 0.6687(2) 0.0335(8) Uani d . 1 . .
O O11 0.1784(3) 0.2192(3) 0.4861(2) 0.0349(9) Uani d D 1 . .
H H11A 0.205(5) 0.206(4) 0.440(3) 0.052 Uiso d D 1 . .
O O12 0.3086(3) 0.4347(3) 0.5613(2) 0.0301(8) Uani d D 1 . .
H H12A 0.260(4) 0.416(4) 0.5048(16) 0.045 Uiso d D 1 . .
H H12B 0.266(8) 0.454(10) 0.593(4) 0.045 Uiso d PD 0.454(15) B 2
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
F2 C1 F3 . . 106.6(4) ?
F2 C1 F1 . . 107.1(4) ?
F3 C1 F1 . . 106.7(4) ?
F2 C1 C2 . . 114.4(4) ?
F3 C1 C2 . . 110.6(4) ?
F1 C1 C2 . . 111.0(4) ?
O1 C2 C3 . . 129.0(4) ?
O1 C2 C1 . . 111.7(4) ?
C3 C2 C1 . . 119.3(4) ?
C2 C3 C4 . . 125.7(4) ?
C2 C3 H3 . . 117.1 ?
C4 C3 H3 . . 117.1 ?
O2 C4 C3 . . 123.0(4) ?
O2 C4 C5 . . 116.8(4) ?
C3 C4 C5 . . 120.1(4) ?
C4 C5 C6 . . 113.8(4) ?
C4 C5 C8 . . 106.3(4) ?
C6 C5 C8 . . 109.5(4) ?
C4 C5 C7 . . 109.1(4) ?
C6 C5 C7 . . 108.7(4) ?
C8 C5 C7 . . 109.2(4) ?
C5 C6 H6A . . 109.5 ?
C5 C6 H6B . . 109.5 ?
H6A C6 H6B . . 109.5 ?
C5 C6 H6C . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
C5 C7 H7A . . 109.5 ?
C5 C7 H7B . . 109.5 ?
H7A C7 H7B . . 109.5 ?
C5 C7 H7C . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
C5 C8 H8A . . 109.5 ?
C5 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
C5 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
F4 C9 F6 . . 105.9(5) ?
F4 C9 F5 . . 107.4(5) ?
F6 C9 F5 . . 105.7(5) ?
F4 C9 C10 . . 113.0(4) ?
F6 C9 C10 . . 109.8(5) ?
F5 C9 C10 . . 114.4(4) ?
O3 C10 C11 . . 130.0(4) ?
O3 C10 C9 . . 113.0(4) ?
C11 C10 C9 . . 116.9(4) ?
C10 C11 C12 . . 124.7(4) ?
C10 C11 H11 . . 117.6 ?
C12 C11 H11 . . 117.6 ?
O4 C12 C11 . . 123.3(4) ?
O4 C12 C13 . . 117.5(4) ?
C11 C12 C13 . . 119.2(4) ?
C12 C13 C14 . . 109.3(4) ?
C12 C13 C16 . . 107.8(4) ?
C14 C13 C16 . . 110.1(4) ?
C12 C13 C15 . . 110.3(4) ?
C14 C13 C15 . . 108.8(4) ?
C16 C13 C15 . . 110.4(4) ?
C13 C14 H14A . . 109.5 ?
C13 C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
C13 C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
C13 C15 H15A . . 109.5 ?
C13 C15 H15B . . 109.5 ?
H15A C15 H15B . . 109.5 ?
C13 C15 H15C . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
C13 C16 H16A . . 109.5 ?
C13 C16 H16B . . 109.5 ?
H16A C16 H16B . . 109.5 ?
C13 C16 H16C . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
O5 C17 H17A . . 109.5 ?
O5 C17 H17B . . 109.5 ?
O5 C17 H17C . . 109.5 ?
H17A C17 H5B . . 140.5 ?
H17B C17 H5B . . 99.1 ?
H17C C17 H5B . . 84.8 ?
F7 C18 F9 . . 107.1(4) ?
F7 C18 F8 . . 107.1(4) ?
F9 C18 F8 . . 107.1(4) ?
F7 C18 C19 . . 114.2(4) ?
F9 C18 C19 . . 110.4(4) ?
F8 C18 C19 . . 110.6(4) ?
O7 C19 C20 . . 128.9(5) ?
O7 C19 C18 . . 111.7(4) ?
C20 C19 C18 . . 119.4(5) ?
C19 C20 C21 . . 125.7(5) ?
C19 C20 H20 . . 117.2 ?
C21 C20 H20 . . 117.2 ?
O8 C21 C20 . . 122.8(4) ?
O8 C21 C22 . . 117.5(5) ?
C20 C21 C22 . . 119.7(5) ?
C21 C22 C23 . . 109.4(4) ?
C21 C22 C25 . . 109.6(5) ?
C23 C22 C25 . . 110.3(5) ?
C21 C22 C24 . . 107.7(4) ?
C23 C22 C24 . . 110.7(5) ?
C25 C22 C24 . . 109.1(5) ?
C22 C23 H23A . . 109.5 ?
C22 C23 H23B . . 109.5 ?
H23A C23 H23B . . 109.5 ?
C22 C23 H23C . . 109.5 ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?
C22 C24 H24A . . 109.5 ?
C22 C24 H24B . . 109.5 ?
H24A C24 H24B . . 109.5 ?
C22 C24 H24C . . 109.5 ?
H24A C24 H24C . . 109.5 ?
H24B C24 H24C . . 109.5 ?
C22 C25 H25A . . 109.5 ?
C22 C25 H25B . . 109.5 ?
H25A C25 H25B . . 109.5 ?
C22 C25 H25C . . 109.5 ?
H25A C25 H25C . . 109.5 ?
H25B C25 H25C . . 109.5 ?
F10 C26 F12 . . 106.8(4) ?
F10 C26 F11 . . 106.5(4) ?
F12 C26 F11 . . 105.9(4) ?
F10 C26 C27 . . 112.0(4) ?
F12 C26 C27 . . 111.2(4) ?
F11 C26 C27 . . 114.0(4) ?
O9 C27 C28 . . 129.1(4) ?
O9 C27 C26 . . 112.1(4) ?
C28 C27 C26 . . 118.8(4) ?
C27 C28 C29 . . 123.1(4) ?
C27 C28 H28 . . 118.5 ?
C29 C28 H28 . . 118.5 ?
O10 C29 C28 . . 123.9(4) ?
O10 C29 C30 . . 117.3(4) ?
C28 C29 C30 . . 118.7(4) ?
C32 C30 C33B . . 141.5(10) ?
C32 C30 C31 . . 112.8(7) ?
C32 C30 C29 . . 108.1(5) ?
C33B C30 C29 . . 110.1(10) ?
C31 C30 C29 . . 110.1(5) ?
C33B C30 C32B . . 116.1(14) ?
C29 C30 C32B . . 117.6(7) ?
C32 C30 C33 . . 111.1(6) ?
C31 C30 C33 . . 107.3(6) ?
C29 C30 C33 . . 107.4(5) ?
C33B C30 C31B . . 106.6(15) ?
C29 C30 C31B . . 106.6(7) ?
C30 C31 H31A . . 109.5 ?
C30 C31 H31B . . 109.5 ?
C30 C31 H31C . . 109.5 ?
C30 C32 H32A . . 109.5 ?
C30 C32 H32B . . 109.5 ?
C30 C32 H32C . . 109.5 ?
C30 C33 H33A . . 109.5 ?
C30 C33 H33B . . 109.5 ?
C30 C33 H33C . . 109.5 ?
C30 C31B H31D . . 109.5 ?
C30 C31B H31E . . 109.5 ?
H31D C31B H31E . . 109.5 ?
C30 C31B H31F . . 109.5 ?
H31D C31B H31F . . 109.5 ?
H31E C31B H31F . . 109.5 ?
C30 C32B H32D . . 109.5 ?
C30 C32B H32E . . 109.5 ?
H32D C32B H32E . . 109.5 ?
C30 C32B H32F . . 109.5 ?
H32D C32B H32F . . 109.5 ?
H32E C32B H32F . . 109.5 ?
C30 C33B H33D . . 109.5 ?
C30 C33B H33E . . 109.5 ?
H33D C33B H33E . . 109.5 ?
C30 C33B H33F . . 109.5 ?
H33D C33B H33F . . 109.5 ?
H33E C33B H33F . . 109.5 ?
O11 C34 H34A . . 109.5 ?
O11 C34 H34B . . 109.5 ?
H34A C34 H34B . . 109.5 ?
O11 C34 H34C . . 109.5 ?
H34A C34 H34C . . 109.5 ?
H34B C34 H34C . . 109.5 ?
O12 C35 H35A . . 109.5 ?
O12 C35 H35B . . 109.5 ?
O12 C35 H35C . . 109.5 ?
O4 Ni1 O2 . . 86.61(12) ?
O4 Ni1 O1 . . 88.71(13) ?
O2 Ni1 O1 . . 90.57(12) ?
O4 Ni1 O3 . . 91.10(12) ?
O2 Ni1 O3 . . 177.68(12) ?
O1 Ni1 O3 . . 89.75(12) ?
O4 Ni1 O6 . . 176.00(14) ?
O2 Ni1 O6 . . 89.65(13) ?
O1 Ni1 O6 . . 89.89(13) ?
O3 Ni1 O6 . . 92.65(13) ?
O4 Ni1 O5 . . 92.70(13) ?
O2 Ni1 O5 . . 92.81(12) ?
O1 Ni1 O5 . . 176.41(13) ?
O3 Ni1 O5 . . 86.92(12) ?
O6 Ni1 O5 . . 88.91(13) ?
O8 Ni2 O10 . . 89.86(14) ?
O8 Ni2 O7 . . 91.07(13) ?
O10 Ni2 O7 . . 179.05(14) ?
O8 Ni2 O9 . . 88.98(13) ?
O10 Ni2 O9 . . 89.01(13) ?
O7 Ni2 O9 . . 90.81(13) ?
O8 Ni2 O11 . . 90.45(13) ?
O10 Ni2 O11 . . 91.16(13) ?
O7 Ni2 O11 . . 89.03(13) ?
O9 Ni2 O11 . . 179.40(14) ?
O8 Ni2 O12 . . 177.62(13) ?
O10 Ni2 O12 . . 88.24(13) ?
O7 Ni2 O12 . . 90.84(13) ?
O9 Ni2 O12 . . 92.41(13) ?
O11 Ni2 O12 . . 88.17(13) ?
C2 O1 Ni1 . . 120.1(3) ?
C4 O2 Ni1 . . 125.9(3) ?
C10 O3 Ni1 . . 121.3(3) ?
C12 O4 Ni1 . . 128.1(3) ?
C17 O5 Ni1 . . 125.0(5) ?
C17 O5 H5A . . 109(4) ?
Ni1 O5 H5A . . 121(4) ?
Ni1 O5 H5B . . 100(6) ?
H5A O5 H5B . . 111(3) ?
Ni1 O6 H6D . . 112(4) ?
Ni1 O6 H6E . . 120(4) ?
H6D O6 H6E . . 112(5) ?
C19 O7 Ni2 . . 122.4(3) ?
C21 O8 Ni2 . . 127.8(3) ?
C27 O9 Ni2 . . 119.3(3) ?
C29 O10 Ni2 . . 125.7(3) ?
C34 O11 Ni2 . . 124.2(3) ?
C34 O11 H11A . . 111(4) ?
Ni2 O11 H11A . . 116(4) ?
C35 O12 Ni2 . . 118.8(5) ?
C35 O12 H12A . . 110(4) ?
Ni2 O12 H12A . . 112(4) ?
Ni2 O12 H12B . . 99(9) ?
H12A O12 H12B . . 107(3) ?
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
C1 F2 . 1.332(6) ?
C1 F3 . 1.334(6) ?
C1 F1 . 1.337(6) ?
C1 C2 . 1.522(6) ?
C2 O1 . 1.279(5) ?
C2 C3 . 1.364(6) ?
C3 C4 . 1.424(6) ?
C3 H3 . 0.9500 ?
C4 O2 . 1.247(5) ?
C4 C5 . 1.530(6) ?
C5 C6 . 1.531(6) ?
C5 C8 . 1.540(6) ?
C5 C7 . 1.542(6) ?
C6 H6A . 0.9800 ?
C6 H6B . 0.9800 ?
C6 H6C . 0.9800 ?
C7 H7A . 0.9800 ?
C7 H7B . 0.9800 ?
C7 H7C . 0.9800 ?
C8 H8A . 0.9800 ?
C8 H8B . 0.9800 ?
C8 H8C . 0.9800 ?
C9 F4 . 1.302(6) ?
C9 F6 . 1.310(7) ?
C9 F5 . 1.319(6) ?
C9 C10 . 1.532(7) ?
C10 O3 . 1.274(5) ?
C10 C11 . 1.368(6) ?
C11 C12 . 1.434(6) ?
C11 H11 . 0.9500 ?
C12 O4 . 1.239(5) ?
C12 C13 . 1.527(6) ?
C13 C14 . 1.531(6) ?
C13 C16 . 1.540(7) ?
C13 C15 . 1.547(6) ?
C14 H14A . 0.9800 ?
C14 H14B . 0.9800 ?
C14 H14C . 0.9800 ?
C15 H15A . 0.9800 ?
C15 H15B . 0.9800 ?
C15 H15C . 0.9800 ?
C16 H16A . 0.9800 ?
C16 H16B . 0.9800 ?
C16 H16C . 0.9800 ?
C17 O5 . 1.377(9) ?
C17 H17A . 0.9800 ?
C17 H17B . 0.9800 ?
C17 H17C . 0.9800 ?
C18 F7 . 1.326(6) ?
C18 F9 . 1.336(5) ?
C18 F8 . 1.337(6) ?
C18 C19 . 1.526(7) ?
C19 O7 . 1.273(5) ?
C19 C20 . 1.369(6) ?
C20 C21 . 1.421(7) ?
C20 H20 . 0.9500 ?
C21 O8 . 1.248(6) ?
C21 C22 . 1.528(7) ?
C22 C23 . 1.528(8) ?
C22 C25 . 1.528(8) ?
C22 C24 . 1.542(8) ?
C23 H23A . 0.9800 ?
C23 H23B . 0.9800 ?
C23 H23C . 0.9800 ?
C24 H24A . 0.9800 ?
C24 H24B . 0.9800 ?
C24 H24C . 0.9800 ?
C25 H25A . 0.9800 ?
C25 H25B . 0.9800 ?
C25 H25C . 0.9800 ?
C26 F10 . 1.330(6) ?
C26 F12 . 1.342(5) ?
C26 F11 . 1.350(5) ?
C26 C27 . 1.522(6) ?
C27 O9 . 1.278(5) ?
C27 C28 . 1.361(6) ?
C28 C29 . 1.429(6) ?
C28 H28 . 0.9500 ?
C29 O10 . 1.256(5) ?
C29 C30 . 1.531(7) ?
C30 C32 . 1.447(10) ?
C30 C33B . 1.45(2) ?
C30 C31 . 1.499(9) ?
C30 C32B . 1.575(17) ?
C30 C33 . 1.582(9) ?
C30 C31B . 1.68(2) ?
C31 H31A . 0.9800 ?
C31 H31B . 0.9800 ?
C31 H31C . 0.9800 ?
C32 H32A . 0.9800 ?
C32 H32B . 0.9800 ?
C32 H32C . 0.9800 ?
C33 H33A . 0.9800 ?
C33 H33B . 0.9800 ?
C33 H33C . 0.9800 ?
C31B H31D . 0.9800 ?
C31B H31E . 0.9800 ?
C31B H31F . 0.9800 ?
C32B H32D . 0.9800 ?
C32B H32E . 0.9800 ?
C32B H32F . 0.9800 ?
C33B H33D . 0.9800 ?
C33B H33E . 0.9800 ?
C33B H33F . 0.9800 ?
C34 O11 . 1.409(6) ?
C34 H34A . 0.9800 ?
C34 H34B . 0.9800 ?
C34 H34C . 0.9800 ?
C35 O12 . 1.320(10) ?
C35 H35A . 0.9800 ?
C35 H35B . 0.9800 ?
C35 H35C . 0.9800 ?
C35 H12B . 0.67(13) ?
Ni1 O4 . 1.995(3) ?
Ni1 O2 . 2.013(3) ?
Ni1 O1 . 2.032(3) ?
Ni1 O3 . 2.039(3) ?
Ni1 O6 . 2.040(3) ?
Ni1 O5 . 2.051(3) ?
Ni2 O8 . 2.004(3) ?
Ni2 O10 . 2.010(3) ?
Ni2 O7 . 2.013(3) ?
Ni2 O9 . 2.022(3) ?
Ni2 O11 . 2.063(3) ?
Ni2 O12 . 2.098(4) ?
O5 H5A . 0.82(4) ?
O5 H5B . 0.83(2) ?
O6 H6D . 0.84(4) ?
O6 H6E . 0.81(4) ?
O11 H11A . 0.85(5) ?
O12 H12A . 0.838(19) ?
O12 H12B . 0.84(2) ?
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
O5 H5A O9 2_666 0.82(4) 1.87(2) 2.692(4) 175(5)
O6 H6D O7 . 0.84(4) 1.89(2) 2.701(4) 164(5)
O6 H6E O12 2_666 0.81(4) 2.16(2) 2.951(5) 164(5)
O11 H11A O1 . 0.85(5) 1.93(5) 2.764(4) 166(5)
O12 H12A O3 . 0.84(2) 1.94(2) 2.778(4) 173(5)
O12 H12B O10 . 0.84(2) 2.50(10) 2.861(4) 108(11)
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
F2 C1 C2 O1 . . . . 179.9(4) ?
F3 C1 C2 O1 . . . . 59.5(5) ?
F1 C1 C2 O1 . . . . -58.8(6) ?
F2 C1 C2 C3 . . . . -0.2(7) ?
F3 C1 C2 C3 . . . . -120.6(5) ?
F1 C1 C2 C3 . . . . 121.1(5) ?
O1 C2 C3 C4 . . . . 2.6(8) ?
C1 C2 C3 C4 . . . . -177.3(4) ?
C2 C3 C4 O2 . . . . -4.0(7) ?
C2 C3 C4 C5 . . . . 178.7(4) ?
O2 C4 C5 C6 . . . . 155.5(4) ?
C3 C4 C5 C6 . . . . -27.0(6) ?
O2 C4 C5 C8 . . . . -83.9(5) ?
C3 C4 C5 C8 . . . . 93.6(5) ?
O2 C4 C5 C7 . . . . 33.8(5) ?
C3 C4 C5 C7 . . . . -148.7(4) ?
F4 C9 C10 O3 . . . . -42.5(7) ?
F6 C9 C10 O3 . . . . 75.5(6) ?
F5 C9 C10 O3 . . . . -165.9(5) ?
F4 C9 C10 C11 . . . . 139.4(5) ?
F6 C9 C10 C11 . . . . -102.6(6) ?
F5 C9 C10 C11 . . . . 16.1(7) ?
O3 C10 C11 C12 . . . . -4.0(9) ?
C9 C10 C11 C12 . . . . 173.7(5) ?
C10 C11 C12 O4 . . . . -0.2(8) ?
C10 C11 C12 C13 . . . . -178.9(5) ?
O4 C12 C13 C14 . . . . 11.2(6) ?
C11 C12 C13 C14 . . . . -170.0(4) ?
O4 C12 C13 C16 . . . . -108.5(5) ?
C11 C12 C13 C16 . . . . 70.3(5) ?
O4 C12 C13 C15 . . . . 130.8(4) ?
C11 C12 C13 C15 . . . . -50.3(6) ?
F7 C18 C19 O7 . . . . 178.4(4) ?
F9 C18 C19 O7 . . . . -60.8(6) ?
F8 C18 C19 O7 . . . . 57.5(5) ?
F7 C18 C19 C20 . . . . -2.7(6) ?
F9 C18 C19 C20 . . . . 118.1(5) ?
F8 C18 C19 C20 . . . . -123.6(5) ?
O7 C19 C20 C21 . . . . 3.1(8) ?
C18 C19 C20 C21 . . . . -175.6(4) ?
C19 C20 C21 O8 . . . . -1.3(8) ?
C19 C20 C21 C22 . . . . 178.6(5) ?
O8 C21 C22 C23 . . . . 124.7(6) ?
C20 C21 C22 C23 . . . . -55.2(7) ?
O8 C21 C22 C25 . . . . 3.6(7) ?
C20 C21 C22 C25 . . . . -176.3(5) ?
O8 C21 C22 C24 . . . . -115.0(5) ?
C20 C21 C22 C24 . . . . 65.1(6) ?
F10 C26 C27 O9 . . . . -52.4(5) ?
F12 C26 C27 O9 . . . . 66.9(5) ?
F11 C26 C27 O9 . . . . -173.4(4) ?
F10 C26 C27 C28 . . . . 127.0(5) ?
F12 C26 C27 C28 . . . . -113.6(5) ?
F11 C26 C27 C28 . . . . 6.1(7) ?
O9 C27 C28 C29 . . . . -1.3(8) ?
C26 C27 C28 C29 . . . . 179.3(4) ?
C27 C28 C29 O10 . . . . 12.1(8) ?
C27 C28 C29 C30 . . . . -165.8(5) ?
O10 C29 C30 C32 . . . . -111.8(6) ?
C28 C29 C30 C32 . . . . 66.2(7) ?
O10 C29 C30 C33B . . . . 63.0(16) ?
C28 C29 C30 C33B . . . . -119.0(16) ?
O10 C29 C30 C31 . . . . 11.8(8) ?
C28 C29 C30 C31 . . . . -170.2(6) ?
O10 C29 C30 C32B . . . . -160.8(11) ?
C28 C29 C30 C32B . . . . 17.2(12) ?
O10 C29 C30 C33 . . . . 128.3(6) ?
C28 C29 C30 C33 . . . . -53.7(7) ?
O10 C29 C30 C31B . . . . -52.3(8) ?
C28 C29 C30 C31B . . . . 125.7(8) ?
C3 C2 O1 Ni1 . . . . 15.5(6) ?
C1 C2 O1 Ni1 . . . . -164.6(3) ?
O4 Ni1 O1 C2 . . . . 63.7(3) ?
O2 Ni1 O1 C2 . . . . -22.9(3) ?
O3 Ni1 O1 C2 . . . . 154.8(3) ?
O6 Ni1 O1 C2 . . . . -112.5(3) ?
C3 C4 O2 Ni1 . . . . -14.1(6) ?
C5 C4 O2 Ni1 . . . . 163.3(3) ?
O4 Ni1 O2 C4 . . . . -65.2(3) ?
O1 Ni1 O2 C4 . . . . 23.5(3) ?
O6 Ni1 O2 C4 . . . . 113.4(3) ?
O5 Ni1 O2 C4 . . . . -157.7(3) ?
C11 C10 O3 Ni1 . . . . -3.3(7) ?
C9 C10 O3 Ni1 . . . . 179.0(3) ?
O4 Ni1 O3 C10 . . . . 9.4(3) ?
O1 Ni1 O3 C10 . . . . -79.3(3) ?
O6 Ni1 O3 C10 . . . . -169.2(3) ?
O5 Ni1 O3 C10 . . . . 102.0(3) ?
C11 C12 O4 Ni1 . . . . 11.3(7) ?
C13 C12 O4 Ni1 . . . . -169.9(3) ?
O2 Ni1 O4 C12 . . . . 166.5(4) ?
O1 Ni1 O4 C12 . . . . 75.8(4) ?
O3 Ni1 O4 C12 . . . . -13.9(4) ?
O5 Ni1 O4 C12 . . . . -100.9(4) ?
O4 Ni1 O5 C17 . . . . 39.8(5) ?
O2 Ni1 O5 C17 . . . . 126.6(5) ?
O3 Ni1 O5 C17 . . . . -51.1(5) ?
O6 Ni1 O5 C17 . . . . -143.8(5) ?
C20 C19 O7 Ni2 . . . . 5.1(7) ?
C18 C19 O7 Ni2 . . . . -176.1(3) ?
O8 Ni2 O7 C19 . . . . -10.1(3) ?
O9 Ni2 O7 C19 . . . . 78.9(3) ?
O11 Ni2 O7 C19 . . . . -100.5(3) ?
O12 Ni2 O7 C19 . . . . 171.3(3) ?
C20 C21 O8 Ni2 . . . . -8.8(7) ?
C22 C21 O8 Ni2 . . . . 171.3(3) ?
O10 Ni2 O8 C21 . . . . -167.3(4) ?
O7 Ni2 O8 C21 . . . . 12.5(4) ?
O9 Ni2 O8 C21 . . . . -78.3(4) ?
O11 Ni2 O8 C21 . . . . 101.5(4) ?
C28 C27 O9 Ni2 . . . . -26.1(7) ?
C26 C27 O9 Ni2 . . . . 153.3(3) ?
O8 Ni2 O9 C27 . . . . -57.6(3) ?
O10 Ni2 O9 C27 . . . . 32.3(3) ?
O7 Ni2 O9 C27 . . . . -148.6(3) ?
O12 Ni2 O9 C27 . . . . 120.5(3) ?
C28 C29 O10 Ni2 . . . . 8.3(7) ?
C30 C29 O10 Ni2 . . . . -173.8(3) ?
O8 Ni2 O10 C29 . . . . 63.7(4) ?
O9 Ni2 O10 C29 . . . . -25.3(4) ?
O11 Ni2 O10 C29 . . . . 154.1(4) ?
O12 Ni2 O10 C29 . . . . -117.8(4) ?
O8 Ni2 O11 C34 . . . . 44.0(5) ?
O10 Ni2 O11 C34 . . . . -45.9(5) ?
O7 Ni2 O11 C34 . . . . 135.0(5) ?
O12 Ni2 O11 C34 . . . . -134.1(5) ?
O10 Ni2 O12 C35 . . . . 31.0(5) ?
O7 Ni2 O12 C35 . . . . -148.8(5) ?
O9 Ni2 O12 C35 . . . . -57.9(5) ?
O11 Ni2 O12 C35 . . . . 122.2(5) ?
