 
data_a_sq
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C85.50 H127.50 F6 N17.50 Ni2 O19 Si' 
_chemical_formula_weight          1964.05

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'
 'F'  'F'   0.0171   0.0103
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Si'  'Si'   0.0817   0.0704
 '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'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            62
_space_group_name_H-M_alt         'P n m a'
_space_group_name_Hall            '-P 2ac 2n'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z'
 'x+1/2, -y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 'x, -y-1/2, z'
 '-x-1/2, y-1/2, z-1/2'
 
_cell_length_a                    21.4817(9)
_cell_length_b                    23.3867(10)
_cell_length_c                    19.8758(8)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      9985.3(7)
_cell_formula_units_Z             4
_cell_measurement_temperature     296(2)
_cell_measurement_reflns_used    8103
_cell_measurement_theta_min        2.23
_cell_measurement_theta_max       24.65
 
_exptl_crystal_description        block
_exptl_crystal_colour             green
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.306          
_exptl_crystal_F_000              4156
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.220
_exptl_crystal_size_mid           0.200
_exptl_crystal_size_min           0.180
_exptl_absorpt_coefficient_mu     0.472
_shelx_estimated_absorpt_T_min    0.903
_shelx_estimated_absorpt_T_max    0.920
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       296(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   ccd
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             63784
_diffrn_reflns_av_unetI/netI      0.0292
_diffrn_reflns_av_R_equivalents   0.0479
_diffrn_reflns_limit_h_min        -25
_diffrn_reflns_limit_h_max        25
_diffrn_reflns_limit_k_min        -27
_diffrn_reflns_limit_k_max        27
_diffrn_reflns_limit_l_min        -23
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          1.345
_diffrn_reflns_theta_max          25.095
_diffrn_reflns_theta_full         25.095
_diffrn_measured_fraction_theta_max   0.999
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.999
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.999
_diffrn_reflns_point_group_measured_fraction_full  0.999
_reflns_number_total              9106
_reflns_number_gt                 7436
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          9106
_refine_ls_number_parameters      481
_refine_ls_number_restraints      185
_refine_ls_R_factor_all           0.0879
_refine_ls_R_factor_gt            0.0788
_refine_ls_wR_factor_ref          0.2937
_refine_ls_wR_factor_gt           0.2834
_refine_ls_goodness_of_fit_ref    1.297
_refine_ls_restrained_S_all       1.300
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Ni1 Ni 0.12714(2) 0.32374(2) 0.01604(2) 0.0227(2) Uani 1 1 d . . . . .
C25A C 0.4833(4) 0.4233(4) 0.3826(4) 0.039(2) Uani 0.455(6) 1 d . . P A 1
H25A H 0.4777 0.4617 0.3724 0.047 Uiso 0.455(6) 1 calc R U P A 1
C26A C 0.5360(4) 0.4062(3) 0.4155(4) 0.035(2) Uani 0.455(6) 1 d . . P A 1
H26A H 0.5651 0.4338 0.4275 0.042 Uiso 0.455(6) 1 calc R U P A 1
C24A C 0.5041(4) 0.3121(4) 0.4138(6) 0.050(3) Uani 0.455(6) 1 d . . P A 1
H24A H 0.5106 0.2739 0.4246 0.060 Uiso 0.455(6) 1 calc R U P A 1
C23A C 0.4508(5) 0.3275(4) 0.3803(7) 0.058(4) Uani 0.455(6) 1 d . . P A 1
H23A H 0.4223 0.2994 0.3681 0.069 Uiso 0.455(6) 1 calc R U P A 1
C25B C 0.4490(4) 0.3994(4) 0.4318(4) 0.051(2) Uani 0.545(6) 1 d . . P A 2
H25B H 0.4203 0.4222 0.4542 0.061 Uiso 0.545(6) 1 calc R U P A 2
C26B C 0.5005(3) 0.3813(3) 0.4645(4) 0.0386(18) Uani 0.545(6) 1 d . . P A 2
H26B H 0.5045 0.3888 0.5102 0.046 Uiso 0.545(6) 1 calc R U P A 2
C24B C 0.5361(4) 0.3351(4) 0.3691(4) 0.047(2) Uani 0.545(6) 1 d . . P A 2
H24B H 0.5650 0.3120 0.3473 0.057 Uiso 0.545(6) 1 calc R U P A 2
C23B C 0.4827(4) 0.3509(4) 0.3349(4) 0.047(2) Uani 0.545(6) 1 d . . P A 2
H23B H 0.4769 0.3385 0.2909 0.057 Uiso 0.545(6) 1 calc R U P A 2
C19A C 0.3012(4) 0.5295(4) 0.4081(5) 0.060(3) Uani 0.543(6) 1 d . . P B 1
H19A H 0.2614 0.5147 0.4021 0.072 Uiso 0.543(6) 1 calc R U P B 1
C20A C 0.3115(3) 0.5780(3) 0.4466(4) 0.0424(19) Uani 0.543(6) 1 d . . P B 1
H20A H 0.2770 0.5969 0.4641 0.051 Uiso 0.543(6) 1 calc R U P B 1
C22A C 0.4144(3) 0.5773(3) 0.4322(4) 0.0445(19) Uani 0.543(6) 1 d . . P B 1
H22A H 0.4525 0.5952 0.4393 0.053 Uiso 0.543(6) 1 calc R U P B 1
C21A C 0.4134(4) 0.5286(3) 0.3921(4) 0.048(2) Uani 0.543(6) 1 d . . P B 1
H21A H 0.4501 0.5133 0.3750 0.057 Uiso 0.543(6) 1 calc R U P B 1
C19B C 0.3463(5) 0.5575(4) 0.3522(4) 0.047(3) Uani 0.457(6) 1 d . . P B 2
H19B H 0.3365 0.5628 0.3071 0.057 Uiso 0.457(6) 1 calc R U P B 2
C20B C 0.3521(5) 0.6026(4) 0.3934(4) 0.047(2) Uani 0.457(6) 1 d . . P B 2
H20B H 0.3460 0.6388 0.3754 0.057 Uiso 0.457(6) 1 calc R U P B 2
C22B C 0.3738(4) 0.5473(4) 0.4824(4) 0.036(2) Uani 0.457(6) 1 d . . P B 2
H22B H 0.3832 0.5435 0.5278 0.044 Uiso 0.457(6) 1 calc R U P B 2
C21B C 0.3691(4) 0.4958(4) 0.4446(5) 0.041(2) Uani 0.457(6) 1 d . . P B 2
H21B H 0.3751 0.4600 0.4638 0.050 Uiso 0.457(6) 1 calc R U P B 2
C13A C 0.2444(8) 0.3356(8) 0.0997(9) 0.029(4) Uani 0.32(2) 1 d . U P C 1
H13A H 0.2593 0.3124 0.0653 0.035 Uiso 0.32(2) 1 calc R U P C 1
C14A C 0.2831(8) 0.3462(8) 0.1512(8) 0.032(4) Uani 0.32(2) 1 d . U P C 1
H14A H 0.3211 0.3273 0.1539 0.039 Uiso 0.32(2) 1 calc R U P C 1
C11A C 0.1691(7) 0.3910(7) 0.1445(7) 0.029(4) Uani 0.32(2) 1 d . U P C 1
H11A H 0.1284 0.4046 0.1434 0.034 Uiso 0.32(2) 1 calc R U P C 1
C12A C 0.2061(8) 0.4080(8) 0.1960(10) 0.037(4) Uani 0.32(2) 1 d . . P C 1
H12A H 0.1922 0.4340 0.2280 0.044 Uiso 0.32(2) 1 calc R U P C 1
C13B C 0.2291(7) 0.3191(5) 0.1166(9) 0.091(6) Uani 0.68(2) 1 d . . P C 2
H13B H 0.2361 0.2848 0.0940 0.109 Uiso 0.68(2) 1 calc R U P C 2
C14B C 0.2635(9) 0.3315(6) 0.1761(10) 0.140(9) Uani 0.68(2) 1 d . . P C 2
H14B H 0.2840 0.3022 0.1988 0.168 Uiso 0.68(2) 1 calc R U P C 2
C11B C 0.1883(6) 0.4044(4) 0.1201(7) 0.076(4) Uani 0.68(2) 1 d . . P C 2
H11B H 0.1592 0.4307 0.1045 0.091 Uiso 0.68(2) 1 calc R U P C 2
C12B C 0.2280(7) 0.4218(5) 0.1696(8) 0.080(5) Uani 0.68(2) 1 d . . P C 2
H12B H 0.2283 0.4599 0.1828 0.096 Uiso 0.68(2) 1 calc R U P C 2
C8A C 0.3028(11) 0.2999(6) -0.1280(10) 0.063(5) Uani 0.64(5) 1 d D U P D 1
H8A H 0.2914 0.3340 -0.1074 0.075 Uiso 0.64(5) 1 calc R U P D 1
C7A C 0.3478(11) 0.3004(6) -0.1760(12) 0.067(5) Uani 0.64(5) 1 d D U P D 1
H7A H 0.3667 0.3347 -0.1879 0.081 Uiso 0.64(5) 1 calc R U P D 1
C8B C 0.2847(18) 0.2973(11) -0.1481(19) 0.071(8) Uani 0.36(5) 1 d D U P D 2
H8B H 0.2607 0.3298 -0.1411 0.086 Uiso 0.36(5) 1 calc R U P D 2
C7B C 0.3293(17) 0.2980(11) -0.1966(19) 0.064(7) Uani 0.36(5) 1 d D U P D 2
H7B H 0.3354 0.3308 -0.2224 0.077 Uiso 0.36(5) 1 calc R U P D 2
C3A C -0.0085(11) 0.2978(7) -0.1725(11) 0.074(5) Uani 0.59(4) 1 d D U P E 1
H3A H 0.0142 0.3308 -0.1636 0.089 Uiso 0.59(4) 1 calc R U P E 1
C2A C -0.0526(11) 0.2991(7) -0.2219(12) 0.076(5) Uani 0.59(4) 1 d D U P E 1
H2A H -0.0601 0.3329 -0.2452 0.091 Uiso 0.59(4) 1 calc R U P E 1
C3B C -0.0291(12) 0.2987(7) -0.1507(13) 0.050(6) Uani 0.41(4) 1 d D U P E 2
H3B H -0.0204 0.3323 -0.1276 0.060 Uiso 0.41(4) 1 calc R U P E 2
C2B C -0.0751(14) 0.2988(8) -0.1997(13) 0.063(6) Uani 0.41(4) 1 d D U P E 2
H2B H -0.0983 0.3318 -0.2073 0.076 Uiso 0.41(4) 1 calc R U P E 2
C18 C 0.38234(18) 0.4034(2) 0.3284(2) 0.0473(11) Uani 1 1 d . . . . .
C17 C 0.3484(2) 0.45277(18) 0.3345(2) 0.0469(10) Uani 1 1 d . . . . .
C16 C 0.30768(19) 0.40263(17) 0.2545(2) 0.0504(11) Uani 1 1 d . . . . .
C10 C 0.2228(2) 0.2500 -0.0563(2) 0.0284(10) Uani 1 2 d S T P D .
C5 C 0.0507(2) 0.2500 -0.0796(3) 0.0368(12) Uani 1 2 d S T P E .
C9 C 0.2740(3) 0.2500 -0.1093(3) 0.0403(13) Uani 1 2 d DS T P . .
C4 C 0.0037(3) 0.2500 -0.1356(3) 0.0413(13) Uani 1 2 d DS T P . .
C15 C 0.26664(19) 0.38458(18) 0.1994(2) 0.0490(11) Uani 1 1 d . . . . .
C6 C 0.3658(3) 0.2500 -0.2078(4) 0.0591(19) Uani 1 2 d DS T P . .
C1 C -0.0865(3) 0.2500 -0.2373(4) 0.062(2) Uani 1 2 d DS T P . .
C34 C 0.35501(18) 0.50285(18) 0.3777(2) 0.0436(10) Uani 1 1 d . . . . .
C35 C 0.43847(19) 0.38417(18) 0.3643(2) 0.0450(10) Uani 1 1 d . . . . .
N2 N 0.35554(16) 0.37182(16) 0.2780(2) 0.0571(11) Uani 1 1 d . . . . .
H2 H 0.3672 0.3387 0.2642 0.068 Uiso 1 1 calc R U . . .
N3 N 0.30107(17) 0.45099(16) 0.2872(2) 0.0574(11) Uani 1 1 d . . . . .
N1 N 0.18802(14) 0.35482(13) 0.09353(14) 0.0337(7) Uani 1 1 d . . . . .
N5 N 0.36631(13) 0.59877(13) 0.45997(15) 0.0312(7) Uani 1 1 d . . . . .
N4 N 0.54761(13) 0.35162(13) 0.43147(15) 0.0345(7) Uani 1 1 d . . . . .
O1 O 0.12202(12) 0.2500 0.06613(14) 0.0173(6) Uani 1 2 d S T P . .
O2 O 0.20382(12) 0.29756(12) -0.03726(14) 0.0402(7) Uani 1 1 d . . . . .
O3 O 0.06859(13) 0.29730(11) -0.05845(14) 0.0421(7) Uani 1 1 d . . . . .
F4 F 0.3875(3) 0.2500 0.2426(3) 0.1122(19) Uiso 1 2 d DS . P . .
F5 F 0.4386(5) 0.3201(4) 0.1777(5) 0.373(8) Uiso 1 1 d D . . . .
F3 F 0.3819(6) 0.2500 0.1197(9) 0.318(9) Uiso 1 2 d DS . P . .
F1 F 0.4969(5) 0.2500 0.2332(6) 0.327(8) Uiso 1 2 d DS . P . .
F2 F 0.4911(6) 0.2500 0.1160(7) 0.377(11) Uiso 1 2 d DS . P . .
Si1 Si 0.4383(5) 0.2500 0.1807(5) 0.293(5) Uiso 1 2 d DS . P . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
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 O1 1.9943(14) . ?
Ni1 O3 2.039(2) . ?
Ni1 O2 2.052(2) . ?
Ni1 N4 2.105(3) 6_556 ?
Ni1 N5 2.132(3) 2_564 ?
Ni1 N1 2.147(3) . ?
C25A C26A 1.367(11) . ?
C25A C35 1.377(9) . ?
C25A H25A 0.9300 . ?
C26A N4 1.339(8) . ?
C26A H26A 0.9300 . ?
C24A N4 1.360(9) . ?
C24A C23A 1.373(13) . ?
C24A H24A 0.9300 . ?
C23A C35 1.388(11) . ?
C23A H23A 0.9300 . ?
C25B C26B 1.350(10) . ?
C25B C35 1.406(9) . ?
C25B H25B 0.9300 . ?
C26B N4 1.391(7) . ?
C26B H26B 0.9300 . ?
C24B N4 1.323(8) . ?
C24B C23B 1.383(11) . ?
C24B H24B 0.9300 . ?
C23B C35 1.361(9) . ?
C23B H23B 0.9300 . ?
C19A C20A 1.386(10) . ?
C19A C34 1.445(10) . ?
C19A H19A 0.9300 . ?
C20A N5 1.302(8) . ?
C20A H20A 0.9300 . ?
C22A N5 1.274(8) . ?
C22A C21A 1.391(11) . ?
C22A H22A 0.9300 . ?
C21A C34 1.420(9) . ?
C21A H21A 0.9300 . ?
C19B C20B 1.342(12) . ?
C19B C34 1.388(10) . ?
C19B H19B 0.9300 . ?
C20B N5 1.360(9) . ?
C20B H20B 0.9300 . ?
C22B N5 1.294(11) . ?
C22B C21B 1.422(12) . ?
C22B H22B 0.9300 . ?
C21B C34 1.372(10) . ?
C21B H21B 0.9300 . ?
C13A N1 1.298(19) . ?
C13A C14A 1.34(3) . ?
C13A H13A 0.9300 . ?
C14A C15 1.360(19) . ?
C14A H14A 0.9300 . ?
C11A C12A 1.36(2) . ?
C11A N1 1.382(15) . ?
C11A H11A 0.9300 . ?
C12A C15 1.413(19) . ?
C12A H12A 0.9300 . ?
C13B N1 1.300(10) . ?
C13B C14B 1.425(14) . ?
C13B H13B 0.9300 . ?
C14B C15 1.326(12) . ?
C14B H14B 0.9300 . ?
C11B N1 1.274(8) . ?
C11B C12B 1.365(12) . ?
C11B H11B 0.9300 . ?
C12B C15 1.340(11) . ?
C12B H12B 0.9300 . ?
C8A C7A 1.358(11) . ?
C8A C9 1.372(11) . ?
C8A H8A 0.9300 . ?
C7A C6 1.391(11) . ?
C7A H7A 0.9300 . ?
C8B C7B 1.361(18) . ?
C8B C9 1.367(17) . ?
C8B H8B 0.9300 . ?
C7B C6 1.388(18) . ?
C7B H7B 0.9300 . ?
C3A C4 1.361(13) . ?
C3A C2A 1.365(13) . ?
C3A H3A 0.9300 . ?
C2A C1 1.395(13) . ?
C2A H2A 0.9300 . ?
C3B C4 1.373(14) . ?
C3B C2B 1.386(15) . ?
C3B H3B 0.9300 . ?
C2B C1 1.388(15) . ?
C2B H2B 0.9300 . ?
C18 C17 1.371(6) . ?
C18 N2 1.372(5) . ?
C18 C35 1.472(5) . ?
C17 N3 1.386(5) . ?
C17 C34 1.459(5) . ?
C16 N3 1.312(5) . ?
C16 N2 1.340(5) . ?
C16 C15 1.469(5) . ?
C10 O2 1.243(3) 7_565 ?
C10 O2 1.244(3) . ?
C10 C9 1.523(7) . ?
C5 O3 1.244(3) 7_565 ?
C5 O3 1.244(3) . ?
C5 C4 1.502(7) . ?
C9 C8B 1.367(17) 7_565 ?
C9 C8A 1.372(11) 7_565 ?
C4 C3A 1.361(13) 7_565 ?
C4 C3B 1.373(14) 7_565 ?
C6 C7B 1.388(18) 7_565 ?
C6 C7A 1.391(11) 7_565 ?
C6 C1 1.496(8) 6_655 ?
C1 C2B 1.388(15) 7_565 ?
C1 C2A 1.395(13) 7_565 ?
C1 C6 1.496(8) 6 ?
N2 H2 0.8600 . ?
N5 Ni1 2.132(3) 2_565 ?
N4 Ni1 2.105(3) 6_656 ?
O1 Ni1 1.9942(14) 7_565 ?
F4 Si1 1.646(10) . ?
F5 Si1 1.641(9) . ?
F3 Si1 1.714(12) . ?
F1 Si1 1.634(12) . ?
F2 Si1 1.714(12) . ?
Si1 F5 1.641(9) 7_565 ?
 
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 Ni1 O3 93.80(10) . . ?
O1 Ni1 O2 92.52(11) . . ?
O3 Ni1 O2 91.71(11) . . ?
O1 Ni1 N4 88.61(11) . 6_556 ?
O3 Ni1 N4 87.32(12) . 6_556 ?
O2 Ni1 N4 178.55(12) . 6_556 ?
O1 Ni1 N5 178.29(11) . 2_564 ?
O3 Ni1 N5 85.35(11) . 2_564 ?
O2 Ni1 N5 86.03(11) . 2_564 ?
N4 Ni1 N5 92.83(11) 6_556 2_564 ?
O1 Ni1 N1 88.18(11) . . ?
O3 Ni1 N1 177.87(11) . . ?
O2 Ni1 N1 88.99(11) . . ?
N4 Ni1 N1 91.95(12) 6_556 . ?
N5 Ni1 N1 92.69(11) 2_564 . ?
C26A C25A C35 120.8(7) . . ?
C26A C25A H25A 119.6 . . ?
C35 C25A H25A 119.6 . . ?
N4 C26A C25A 123.1(7) . . ?
N4 C26A H26A 118.5 . . ?
C25A C26A H26A 118.5 . . ?
N4 C24A C23A 121.4(8) . . ?
N4 C24A H24A 119.3 . . ?
C23A C24A H24A 119.3 . . ?
C24A C23A C35 121.3(8) . . ?
C24A C23A H23A 119.3 . . ?
C35 C23A H23A 119.3 . . ?
C26B C25B C35 120.8(7) . . ?
C26B C25B H25B 119.6 . . ?
C35 C25B H25B 119.6 . . ?
C25B C26B N4 121.7(6) . . ?
C25B C26B H26B 119.2 . . ?
N4 C26B H26B 119.2 . . ?
N4 C24B C23B 122.5(7) . . ?
N4 C24B H24B 118.7 . . ?
C23B C24B H24B 118.7 . . ?
C35 C23B C24B 121.4(7) . . ?
C35 C23B H23B 119.3 . . ?
C24B C23B H23B 119.3 . . ?
C20A C19A C34 117.1(7) . . ?
C20A C19A H19A 121.4 . . ?
C34 C19A H19A 121.4 . . ?
N5 C20A C19A 124.2(7) . . ?
N5 C20A H20A 117.9 . . ?
C19A C20A H20A 117.9 . . ?
N5 C22A C21A 124.0(7) . . ?
N5 C22A H22A 118.0 . . ?
C21A C22A H22A 118.0 . . ?
C22A C21A C34 118.4(7) . . ?
C22A C21A H21A 120.8 . . ?
C34 C21A H21A 120.8 . . ?
C20B C19B C34 119.2(7) . . ?
C20B C19B H19B 120.4 . . ?
C34 C19B H19B 120.4 . . ?
C19B C20B N5 124.3(8) . . ?
C19B C20B H20B 117.9 . . ?
N5 C20B H20B 117.9 . . ?
N5 C22B C21B 126.6(7) . . ?
N5 C22B H22B 116.7 . . ?
C21B C22B H22B 116.7 . . ?
C34 C21B C22B 115.2(8) . . ?
C34 C21B H21B 122.4 . . ?
C22B C21B H21B 122.4 . . ?
N1 C13A C14A 125.9(17) . . ?
N1 C13A H13A 117.0 . . ?
C14A C13A H13A 117.0 . . ?
C13A C14A C15 119.9(16) . . ?
C13A C14A H14A 120.1 . . ?
C15 C14A H14A 120.1 . . ?
C12A C11A N1 124.1(14) . . ?
C12A C11A H11A 118.0 . . ?
N1 C11A H11A 118.0 . . ?
C11A C12A C15 117.5(14) . . ?
C11A C12A H12A 121.2 . . ?
C15 C12A H12A 121.2 . . ?
N1 C13B C14B 120.9(8) . . ?
N1 C13B H13B 119.5 . . ?
C14B C13B H13B 119.5 . . ?
C15 C14B C13B 120.4(9) . . ?
C15 C14B H14B 119.8 . . ?
C13B C14B H14B 119.8 . . ?
N1 C11B C12B 124.9(7) . . ?
N1 C11B H11B 117.5 . . ?
C12B C11B H11B 117.5 . . ?
C15 C12B C11B 120.8(9) . . ?
C15 C12B H12B 119.6 . . ?
C11B C12B H12B 119.6 . . ?
C7A C8A C9 121.3(13) . . ?
C7A C8A H8A 119.4 . . ?
C9 C8A H8A 119.4 . . ?
C8A C7A C6 120.7(13) . . ?
C8A C7A H7A 119.7 . . ?
C6 C7A H7A 119.7 . . ?
C7B C8B C9 122(3) . . ?
C7B C8B H8B 119.0 . . ?
C9 C8B H8B 119.0 . . ?
C8B C7B C6 120(3) . . ?
C8B C7B H7B 120.0 . . ?
C6 C7B H7B 120.0 . . ?
C4 C3A C2A 122.7(15) . . ?
C4 C3A H3A 118.6 . . ?
C2A C3A H3A 118.6 . . ?
C3A C2A C1 120.1(14) . . ?
C3A C2A H2A 119.9 . . ?
C1 C2A H2A 119.9 . . ?
C4 C3B C2B 121.4(14) . . ?
C4 C3B H3B 119.3 . . ?
C2B C3B H3B 119.3 . . ?
C3B C2B C1 120.2(15) . . ?
C3B C2B H2B 119.9 . . ?
C1 C2B H2B 119.9 . . ?
C17 C18 N2 107.1(3) . . ?
C17 C18 C35 130.6(4) . . ?
N2 C18 C35 122.2(4) . . ?
C18 C17 N3 107.7(3) . . ?
C18 C17 C34 132.5(4) . . ?
N3 C17 C34 119.7(3) . . ?
N3 C16 N2 112.0(3) . . ?
N3 C16 C15 123.5(3) . . ?
N2 C16 C15 124.5(4) . . ?
O2 C10 O2 126.9(4) 7_565 . ?
O2 C10 C9 116.6(2) 7_565 . ?
O2 C10 C9 116.6(2) . . ?
O3 C5 O3 125.5(5) 7_565 . ?
O3 C5 C4 117.3(2) 7_565 . ?
O3 C5 C4 117.3(2) . . ?
C8B C9 C8B 108(3) 7_565 . ?
C8A C9 C8A 116.4(15) 7_565 . ?
C8B C9 C10 120.7(13) 7_565 . ?
C8B C9 C10 120.7(13) . . ?
C8A C9 C10 120.9(7) 7_565 . ?
C8A C9 C10 120.9(7) . . ?
C3A C4 C3A 110.2(18) . 7_565 ?
C3B C4 C3B 112.1(18) . 7_565 ?
C3A C4 C5 121.9(7) . . ?
C3A C4 C5 121.9(7) 7_565 . ?
C3B C4 C5 120.5(7) . . ?
C3B C4 C5 120.5(7) 7_565 . ?
C14B C15 C12B 115.0(7) . . ?
C14A C15 C12A 117.5(11) . . ?
C14B C15 C16 124.0(5) . . ?
C12B C15 C16 121.0(5) . . ?
C14A C15 C16 124.0(9) . . ?
C12A C15 C16 118.4(8) . . ?
C7B C6 C7B 108(3) 7_565 . ?
C7A C6 C7A 115.7(15) . 7_565 ?
C7B C6 C1 120.2(13) 7_565 6_655 ?
C7B C6 C1 120.2(13) . 6_655 ?
C7A C6 C1 121.4(7) . 6_655 ?
C7A C6 C1 121.4(7) 7_565 6_655 ?
C2B C1 C2B 111(2) . 7_565 ?
C2A C1 C2A 110.9(17) . 7_565 ?
C2B C1 C6 121.0(8) . 6 ?
C2B C1 C6 121.0(8) 7_565 6 ?
C2A C1 C6 121.2(7) . 6 ?
C2A C1 C6 121.2(7) 7_565 6 ?
C21B C34 C19B 119.6(6) . . ?
C21A C34 C19A 116.1(5) . . ?
C21B C34 C17 119.7(5) . . ?
C19B C34 C17 120.7(5) . . ?
C21A C34 C17 123.0(5) . . ?
C19A C34 C17 120.9(4) . . ?
C25A C35 C23A 116.1(6) . . ?
C23B C35 C25B 116.2(5) . . ?
C23B C35 C18 122.6(4) . . ?
C25A C35 C18 119.9(5) . . ?
C23A C35 C18 124.0(5) . . ?
C25B C35 C18 121.2(5) . . ?
C16 N2 C18 106.7(3) . . ?
C16 N2 H2 126.7 . . ?
C18 N2 H2 126.7 . . ?
C16 N3 C17 106.4(3) . . ?
C11B N1 C13B 115.9(6) . . ?
C13A N1 C11A 114.7(11) . . ?
C11B N1 Ni1 127.4(4) . . ?
C13A N1 Ni1 121.3(9) . . ?
C13B N1 Ni1 116.7(4) . . ?
C11A N1 Ni1 123.6(6) . . ?
C22A N5 C20A 119.9(5) . . ?
C22B N5 C20B 115.1(5) . . ?
C22A N5 Ni1 120.5(4) . 2_565 ?
C22B N5 Ni1 127.1(4) . 2_565 ?
C20A N5 Ni1 118.9(4) . 2_565 ?
C20B N5 Ni1 117.8(4) . 2_565 ?
C26A N4 C24A 117.3(6) . . ?
C24B N4 C26B 116.9(5) . . ?
C24B N4 Ni1 121.7(4) . 6_656 ?
C26A N4 Ni1 124.3(4) . 6_656 ?
C24A N4 Ni1 118.4(4) . 6_656 ?
C26B N4 Ni1 120.7(3) . 6_656 ?
Ni1 O1 Ni1 119.71(14) 7_565 . ?
C10 O2 Ni1 133.4(3) . . ?
C5 O3 Ni1 134.9(3) . . ?
F1 Si1 F5 91.2(4) . 7_565 ?
F1 Si1 F5 91.2(4) . . ?
F5 Si1 F5 175.8(8) 7_565 . ?
F1 Si1 F4 91.9(6) . . ?
F5 Si1 F4 91.7(4) 7_565 . ?
F5 Si1 F4 91.7(4) . . ?
F1 Si1 F2 88.3(6) . . ?
F5 Si1 F2 88.3(4) 7_565 . ?
F5 Si1 F2 88.3(4) . . ?
F4 Si1 F2 179.8(8) . . ?
F1 Si1 F3 174.7(9) . . ?
F5 Si1 F3 88.7(4) 7_565 . ?
F5 Si1 F3 88.7(4) . . ?
F4 Si1 F3 93.4(8) . . ?
F2 Si1 F3 86.3(6) . . ?
 
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
C35 C25A C26A N4 0.5(13) . . . . ?
N4 C24A C23A C35 -1.3(19) . . . . ?
C35 C25B C26B N4 6.1(12) . . . . ?
N4 C24B C23B C35 -0.6(14) . . . . ?
C34 C19A C20A N5 -4.0(12) . . . . ?
N5 C22A C21A C34 3.7(12) . . . . ?
C34 C19B C20B N5 0.1(15) . . . . ?
N5 C22B C21B C34 -0.1(12) . . . . ?
N1 C13A C14A C15 -7(2) . . . . ?
N1 C11A C12A C15 -4(2) . . . . ?
N1 C13B C14B C15 -17(3) . . . . ?
N1 C11B C12B C15 -7(2) . . . . ?
C9 C8A C7A C6 0.1(18) . . . . ?
C9 C8B C7B C6 0(2) . . . . ?
C4 C3A C2A C1 -1.3(18) . . . . ?
C4 C3B C2B C1 -4(2) . . . . ?
N2 C18 C17 N3 -0.4(6) . . . . ?
C35 C18 C17 N3 177.7(5) . . . . ?
N2 C18 C17 C34 -178.3(5) . . . . ?
C35 C18 C17 C34 -0.2(9) . . . . ?
C7B C8B C9 C8B -34(4) . . . 7_565 ?
C7B C8B C9 C10 -178.7(13) . . . . ?
C7A C8A C9 C8A 16(3) . . . 7_565 ?
C7A C8A C9 C10 -178.7(9) . . . . ?
O2 C10 C9 C8B 20(2) 7_565 . . 7_565 ?
O2 C10 C9 C8B -160(2) . . . 7_565 ?
O2 C10 C9 C8B 160(2) 7_565 . . . ?
O2 C10 C9 C8B -20(2) . . . . ?
O2 C10 C9 C8A -8.1(15) 7_565 . . 7_565 ?
O2 C10 C9 C8A 172.6(14) . . . 7_565 ?
O2 C10 C9 C8A -172.6(14) 7_565 . . . ?
O2 C10 C9 C8A 8.1(15) . . . . ?
C2A C3A C4 C3A 29(3) . . . 7_565 ?
C2A C3A C4 C5 -177.6(10) . . . . ?
C2B C3B C4 C3B -25(3) . . . 7_565 ?
C2B C3B C4 C5 -176.5(11) . . . . ?
O3 C5 C4 C3A -165.0(16) 7_565 . . . ?
O3 C5 C4 C3A 14.9(17) . . . . ?
O3 C5 C4 C3A -14.9(17) 7_565 . . 7_565 ?
O3 C5 C4 C3A 165.0(16) . . . 7_565 ?
O3 C5 C4 C3B 164.3(17) 7_565 . . . ?
O3 C5 C4 C3B -15.8(18) . . . . ?
O3 C5 C4 C3B 15.8(18) 7_565 . . 7_565 ?
O3 C5 C4 C3B -164.3(17) . . . 7_565 ?
C13B C14B C15 C12B 10(2) . . . . ?
C13B C14B C15 C16 -171.3(12) . . . . ?
C11B C12B C15 C14B 1.2(17) . . . . ?
C11B C12B C15 C16 -177.5(9) . . . . ?
C13A C14A C15 C12A 5.8(18) . . . . ?
C13A C14A C15 C16 -174.8(10) . . . . ?
C11A C12A C15 C14A -0.9(18) . . . . ?
C11A C12A C15 C16 179.6(10) . . . . ?
N3 C16 C15 C14B -164.2(15) . . . . ?
N2 C16 C15 C14B 14.9(16) . . . . ?
N3 C16 C15 C12B 14.4(13) . . . . ?
N2 C16 C15 C12B -166.5(11) . . . . ?
N3 C16 C15 C14A 157.3(9) . . . . ?
N2 C16 C15 C14A -23.6(10) . . . . ?
N3 C16 C15 C12A -23.3(11) . . . . ?
N2 C16 C15 C12A 155.9(10) . . . . ?
C8B C7B C6 C7B 35(4) . . . 7_565 ?
C8B C7B C6 C1 177.9(13) . . . 6_655 ?
C8A C7A C6 C7A -16(3) . . . 7_565 ?
C8A C7A C6 C1 177.6(10) . . . 6_655 ?
C3B C2B C1 C2B 32(3) . . . 7_565 ?
C3B C2B C1 C6 -177.6(11) . . . 6 ?
C3A C2A C1 C2A -27(3) . . . 7_565 ?
C3A C2A C1 C6 -178.7(10) . . . 6 ?
C22B C21B C34 C19B -0.4(10) . . . . ?
C22B C21B C34 C17 -179.3(6) . . . . ?
C20B C19B C34 C21B 0.3(13) . . . . ?
C20B C19B C34 C17 179.3(8) . . . . ?
C22A C21A C34 C19A -1.4(10) . . . . ?
C22A C21A C34 C17 178.0(6) . . . . ?
C20A C19A C34 C21A 1.6(11) . . . . ?
C20A C19A C34 C17 -177.9(6) . . . . ?
C18 C17 C34 C21B -43.2(9) . . . . ?
N3 C17 C34 C21B 139.1(6) . . . . ?
C18 C17 C34 C19B 137.8(7) . . . . ?
N3 C17 C34 C19B -39.9(8) . . . . ?
C18 C17 C34 C21A 41.4(9) . . . . ?
N3 C17 C34 C21A -136.3(6) . . . . ?
C18 C17 C34 C19A -139.2(7) . . . . ?
N3 C17 C34 C19A 43.1(8) . . . . ?
C24B C23B C35 C25B -2.6(12) . . . . ?
C24B C23B C35 C18 177.6(7) . . . . ?
C26A C25A C35 C23A -1.1(12) . . . . ?
C26A C25A C35 C18 -179.5(7) . . . . ?
C24A C23A C35 C25A 1.5(16) . . . . ?
C24A C23A C35 C18 179.9(9) . . . . ?
C26B C25B C35 C23B -0.2(11) . . . . ?
C26B C25B C35 C18 179.6(6) . . . . ?
C17 C18 C35 C23B -147.8(7) . . . . ?
N2 C18 C35 C23B 30.1(8) . . . . ?
C17 C18 C35 C25A -35.8(9) . . . . ?
N2 C18 C35 C25A 142.0(6) . . . . ?
C17 C18 C35 C23A 145.9(9) . . . . ?
N2 C18 C35 C23A -36.3(10) . . . . ?
C17 C18 C35 C25B 32.4(9) . . . . ?
N2 C18 C35 C25B -149.7(6) . . . . ?
N3 C16 N2 C18 -1.4(6) . . . . ?
C15 C16 N2 C18 179.3(4) . . . . ?
C17 C18 N2 C16 1.1(6) . . . . ?
C35 C18 N2 C16 -177.2(4) . . . . ?
N2 C16 N3 C17 1.2(6) . . . . ?
C15 C16 N3 C17 -179.6(4) . . . . ?
C18 C17 N3 C16 -0.4(6) . . . . ?
C34 C17 N3 C16 177.8(4) . . . . ?
C12B C11B N1 C13B 0.3(17) . . . . ?
C12B C11B N1 Ni1 179.7(9) . . . . ?
C14A C13A N1 C11A 2.6(18) . . . . ?
C14A C13A N1 Ni1 -170.4(11) . . . . ?
C14B C13B N1 C11B 11(2) . . . . ?
C14B C13B N1 Ni1 -168.1(13) . . . . ?
C12A C11A N1 C13A 2.8(17) . . . . ?
C12A C11A N1 Ni1 175.6(10) . . . . ?
C21A C22A N5 C20A -6.0(11) . . . . ?
C21A C22A N5 Ni1 -176.6(6) . . . 2_565 ?
C21B C22B N5 C20B 0.5(11) . . . . ?
C21B C22B N5 Ni1 179.7(6) . . . 2_565 ?
C19A C20A N5 C22A 6.3(11) . . . . ?
C19A C20A N5 Ni1 177.0(7) . . . 2_565 ?
C19B C20B N5 C22B -0.5(13) . . . . ?
C19B C20B N5 Ni1 -179.8(8) . . . 2_565 ?
C23B C24B N4 C26B 6.2(11) . . . . ?
C23B C24B N4 Ni1 177.0(7) . . . 6_656 ?
C25A C26A N4 C24A -0.3(12) . . . . ?
C25A C26A N4 Ni1 -178.6(6) . . . 6_656 ?
C23A C24A N4 C26A 0.7(15) . . . . ?
C23A C24A N4 Ni1 179.1(9) . . . 6_656 ?
C25B C26B N4 C24B -9.0(10) . . . . ?
C25B C26B N4 Ni1 -179.8(6) . . . 6_656 ?
O2 C10 O2 Ni1 -13.5(8) 7_565 . . . ?
C9 C10 O2 Ni1 165.7(3) . . . . ?
O3 C5 O3 Ni1 -2.7(9) 7_565 . . . ?
C4 C5 O3 Ni1 177.4(3) . . . . ?
 
_refine_diff_density_max    0.669
_refine_diff_density_min   -1.475
_refine_diff_density_rms    0.113




