# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_(NiL)2
_database_code_depnum_ccdc_archive 'CCDC 1957997'
loop_
_audit_author_name
_audit_author_address
'Carine Duhayon'
;LCC CNRS
France
;
_audit_update_record             
;
2019-10-08 deposited with the CCDC.	2019-12-16 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105 107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   22.4352(6)
_cell_length_b                   16.10382(18)
_cell_length_c                   15.4417(4)
_cell_angle_alpha                90
_cell_angle_beta                 133.251(5)
_cell_angle_gamma                90
_cell_volume                     4063.5(4)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1 '
_symmetry_space_group_name_Hall  '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z+1/2
x,-y,z+1/2
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.3331 0.5567 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni -3.0029 0.5091 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

_chemical_formula_sum            'C46 H38 N10 Ni2 O4'
_chemical_formula_moiety         'C46 H38 N10 Ni2 O4'
_chemical_compound_source        ?
_chemical_formula_weight         912.24


_cell_measurement_reflns_used    11556
_cell_measurement_theta_min      4
_cell_measurement_theta_max      60
_cell_measurement_temperature    180

_exptl_crystal_description       planar
_exptl_crystal_colour            red
_exptl_crystal_size_min          0.020
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.300

_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1888
_exptl_absorpt_coefficient_mu    1.637

# Sheldrick geometric approximatio 0.78 0.97 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, acta cryst. (1995), a51, 33-38'
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_T_max  0.97
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      180
_diffrn_reflns_number            18728
_reflns_number_total             3025
_diffrn_reflns_av_R_equivalents  0.030
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 3025 
# Theoretical number of reflections is about 6050 


_diffrn_reflns_theta_min         3.854
_diffrn_reflns_theta_max         60.096
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        60.096
_diffrn_measured_fraction_theta_full 0.999


_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_reflns_limit_h_min              -25
_reflns_limit_h_max              18
_reflns_limit_k_min              0
_reflns_limit_k_max              18
_reflns_limit_l_min              0
_reflns_limit_l_max              17

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.28
_refine_diff_density_max         0.29


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>1.5\s(I)
_refine_ls_number_reflns         2813
_refine_ls_number_restraints     0
_refine_ls_number_parameters     280
_oxford_refine_ls_R_factor_ref   0.0278
_refine_ls_wR_factor_ref         0.0267
_refine_ls_goodness_of_fit_ref   1.1471
_refine_ls_shift/su_max          0.0011589
_refine_ls_shift/su_mean         0.0000479


# The values computed from all data 
_oxford_reflns_number_all        3007
_refine_ls_R_factor_all          0.0305
_refine_ls_wR_factor_all         0.0283

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                2769
_refine_ls_R_factor_gt           0.0271
_refine_ls_wR_factor_gt          0.0266

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 4.99 -1.37 3.32 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
N1 N 0.40342(7) 0.34045(8) 0.70696(11) 0.0194 1.0000 Uani . . . . . .
N2 N 0.50466(7) 0.46306(8) 0.85329(10) 0.0188 1.0000 Uani . . . . . .
N3 N 0.56191(7) 0.52566(8) 0.91836(11) 0.0217 1.0000 Uani . . . . . .
N4 N 0.45891(7) 0.17954(8) 0.57343(11) 0.0196 1.0000 Uani . . . . . .
N5 N 0.42792(7) 0.23165(7) 0.60580(10) 0.0176 1.0000 Uani . . . . . .
C1 C 0.36204(9) 0.26738(9) 0.66766(13) 0.0198 1.0000 Uani . . . . . .
C2 C 0.29344(10) 0.25577(11) 0.65146(14) 0.0258 1.0000 Uani . . . . . .
C3 C 0.26354(10) 0.32269(11) 0.66756(14) 0.0303 1.0000 Uani . . . . . .
C4 C 0.30339(9) 0.39816(11) 0.70343(14) 0.0275 1.0000 Uani . . . . . .
C5 C 0.37520(9) 0.40473(10) 0.72712(13) 0.0209 1.0000 Uani . . . . . .
C6 C 0.42812(9) 0.47907(9) 0.78576(13) 0.0215 1.0000 Uani . . . . . .
C7 C 0.39508(10) 0.56352(11) 0.77368(16) 0.0355 1.0000 Uani . . . . . .
C8 C 0.63587(9) 0.49157(9) 0.99697(13) 0.0193 1.0000 Uani . . . . . .
C9 C 0.49043(8) 0.22676(9) 0.54181(12) 0.0179 1.0000 Uani . . . . . .
C10 C 0.39062(9) 0.20239(10) 0.63558(13) 0.0204 1.0000 Uani . . . . . .
C11 C 0.37460(11) 0.11267(10) 0.63513(16) 0.0301 1.0000 Uani . . . . . .
C12 C 0.70491(9) 0.55150(10) 1.07324(13) 0.0209 1.0000 Uani . . . . . .
C13 C 0.78033(9) 0.52620(10) 1.18045(13) 0.0230 1.0000 Uani . . . . . .
C14 C 0.84379(9) 0.58310(11) 1.25203(14) 0.0277 1.0000 Uani . . . . . .
C15 C 0.83233(10) 0.66517(11) 1.21773(14) 0.0283 1.0000 Uani . . . . . .
C16 C 0.75758(11) 0.69092(11) 1.11108(15) 0.0318 1.0000 Uani . . . . . .
C17 C 0.69462(10) 0.63415(10) 1.03909(14) 0.0282 1.0000 Uani . . . . . .
C18 C 0.53065(9) 0.18184(9) 0.50918(13) 0.0193 1.0000 Uani . . . . . .
C19 C 0.54589(10) 0.22434(10) 0.44738(14) 0.0257 1.0000 Uani . . . . . .
C20 C 0.58123(11) 0.18328(11) 0.41312(16) 0.0321 1.0000 Uani . . . . . .
C21 C 0.60340(11) 0.10081(11) 0.44206(16) 0.0334 1.0000 Uani . . . . . .
C22 C 0.58958(11) 0.05839(10) 0.50495(16) 0.0317 1.0000 Uani . . . . . .
C23 C 0.55302(9) 0.09868(10) 0.53794(14) 0.0246 1.0000 Uani . . . . . .
O2 O 0.48897(6) 0.30582(6) 0.53756(9) 0.0216 1.0000 Uani . . . . . .
O1 O 0.65192(6) 0.41359(6) 1.01295(9) 0.0220 1.0000 Uani . . . . . .
Ni1 Ni 0.547596(14) 0.350387(14) 0.88290(2) 0.0176 1.0000 Uani . . . . . .
H21 H 0.2667 0.2023 0.6272 0.0320 1.0000 Uiso R . . . . .
H31 H 0.2142 0.3169 0.6529 0.0376 1.0000 Uiso R . . . . .
H41 H 0.2834 0.4455 0.7149 0.0346 1.0000 Uiso R . . . . .
H72 H 0.3373 0.5659 0.7046 0.0548 1.0000 Uiso R . . . . .
H71 H 0.4067 0.5764 0.8462 0.0555 1.0000 Uiso R . . . . .
H73 H 0.4228 0.6035 0.7639 0.0550 1.0000 Uiso R . . . . .
H112 H 0.3885 0.0992 0.7075 0.0490 1.0000 Uiso R . . . . .
H113 H 0.4110 0.0796 0.6356 0.0503 1.0000 Uiso R . . . . .
H111 H 0.3172 0.0996 0.5669 0.0500 1.0000 Uiso R . . . . .
H131 H 0.7883 0.4691 1.2054 0.0285 1.0000 Uiso R . . . . .
H141 H 0.8958 0.5656 1.3269 0.0345 1.0000 Uiso R . . . . .
H151 H 0.8773 0.7042 1.2700 0.0358 1.0000 Uiso R . . . . .
H161 H 0.7485 0.7478 1.0849 0.0388 1.0000 Uiso R . . . . .
H171 H 0.6435 0.6516 0.9658 0.0355 1.0000 Uiso R . . . . .
H191 H 0.5314 0.2823 0.4292 0.0314 1.0000 Uiso R . . . . .
H201 H 0.5900 0.2119 0.3673 0.0407 1.0000 Uiso R . . . . .
H211 H 0.6286 0.0734 0.4177 0.0414 1.0000 Uiso R . . . . .
H221 H 0.6052 0.0011 0.5268 0.0380 1.0000 Uiso R . . . . .
H231 H 0.5430 0.0693 0.5806 0.0302 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
N1 . Ni1 5_656 2.2911(12) yes
N1 . C1 . 1.357(2) yes
N1 . C5 . 1.356(2) yes
N1 . Ni1 . 2.4139(12) yes
N2 . N3 . 1.3810(18) yes
N2 . C6 . 1.284(2) yes
N2 . Ni1 . 1.9559(12) yes
N3 . C8 . 1.330(2) yes
N4 . N5 . 1.3834(17) yes
N4 . C9 . 1.3377(19) yes
N5 . Ni1 5_656 1.9639(12) yes
N5 . C10 . 1.2890(19) yes
C1 . C2 . 1.392(2) yes
C1 . C10 . 1.479(2) yes
C2 . C3 . 1.379(2) yes
C2 . H21 . 0.966 no
C3 . C4 . 1.380(3) yes
C3 . H31 . 0.970 no
C4 . C5 . 1.390(2) yes
C4 . H41 . 0.960 no
C5 . C6 . 1.480(2) yes
C6 . C7 . 1.498(2) yes
C7 . H72 . 0.961 no
C7 . H71 . 0.982 no
C7 . H73 . 0.977 no
C8 . C12 . 1.489(2) yes
C8 . O1 . 1.2828(19) yes
C9 . C18 . 1.488(2) yes
C9 . O2 . 1.2741(19) yes
C10 . C11 . 1.488(2) yes
C11 . H112 . 0.958 no
C11 . H113 . 0.971 no
C11 . H111 . 0.977 no
C12 . C13 . 1.390(2) yes
C12 . C17 . 1.392(2) yes
C13 . C14 . 1.390(2) yes
C13 . H131 . 0.965 no
C14 . C15 . 1.381(2) yes
C14 . H141 . 0.964 no
C15 . C16 . 1.383(2) yes
C15 . H151 . 0.973 no
C16 . C17 . 1.384(2) yes
C16 . H161 . 0.965 no
C17 . H171 . 0.947 no
C18 . C19 . 1.394(2) yes
C18 . C23 . 1.392(2) yes
C19 . C20 . 1.386(2) yes
C19 . H191 . 0.965 no
C20 . C21 . 1.381(3) yes
C20 . H201 . 0.972 no
C21 . C22 . 1.385(3) yes
C21 . H211 . 0.974 no
C22 . C23 . 1.388(2) yes
C22 . H221 . 0.962 no
C23 . H231 . 0.955 no
O2 . Ni1 5_656 2.0193(10) yes
O1 . Ni1 . 2.0263(10) yes
Ni1 . Ni1 5_656 3.0651(5) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Ni1 5_656 N1 . C1 . 104.76(9) yes
Ni1 5_656 N1 . C5 . 125.36(10) yes
C1 . N1 . C5 . 118.72(12) yes
Ni1 5_656 N1 . Ni1 . 81.26(4) yes
C1 . N1 . Ni1 . 122.63(9) yes
C5 . N1 . Ni1 . 99.63(9) yes
N3 . N2 . C6 . 120.25(12) yes
N3 . N2 . Ni1 . 116.33(9) yes
C6 . N2 . Ni1 . 123.13(10) yes
N2 . N3 . C8 . 108.63(12) yes
N5 . N4 . C9 . 108.02(12) yes
N4 . N5 . Ni1 5_656 116.33(9) yes
N4 . N5 . C10 . 121.14(12) yes
Ni1 5_656 N5 . C10 . 122.33(10) yes
N1 . C1 . C2 . 122.00(14) yes
N1 . C1 . C10 . 116.27(13) yes
C2 . C1 . C10 . 121.62(14) yes
C1 . C2 . C3 . 118.49(15) yes
C1 . C2 . H21 . 120.3 no
C3 . C2 . H21 . 121.1 no
C2 . C3 . C4 . 119.95(14) yes
C2 . C3 . H31 . 120.1 no
C4 . C3 . H31 . 120.0 no
C3 . C4 . C5 . 119.20(15) yes
C3 . C4 . H41 . 121.1 no
C5 . C4 . H41 . 119.7 no
C4 . C5 . N1 . 121.36(14) yes
C4 . C5 . C6 . 121.45(14) yes
N1 . C5 . C6 . 116.95(13) yes
C5 . C6 . N2 . 113.59(13) yes
C5 . C6 . C7 . 122.49(13) yes
N2 . C6 . C7 . 123.76(14) yes
C6 . C7 . H72 . 110.5 no
C6 . C7 . H71 . 109.1 no
H72 . C7 . H71 . 111.1 no
C6 . C7 . H73 . 107.7 no
H72 . C7 . H73 . 108.6 no
H71 . C7 . H73 . 109.7 no
N3 . C8 . C12 . 115.18(13) yes
N3 . C8 . O1 . 126.16(13) yes
C12 . C8 . O1 . 118.65(13) yes
N4 . C9 . C18 . 116.24(13) yes
N4 . C9 . O2 . 125.83(13) yes
C18 . C9 . O2 . 117.93(13) yes
C1 . C10 . N5 . 113.41(13) yes
C1 . C10 . C11 . 122.01(13) yes
N5 . C10 . C11 . 124.56(14) yes
C10 . C11 . H112 . 109.3 no
C10 . C11 . H113 . 109.5 no
H112 . C11 . H113 . 105.6 no
C10 . C11 . H111 . 110.5 no
H112 . C11 . H111 . 110.1 no
H113 . C11 . H111 . 111.8 no
C8 . C12 . C13 . 120.65(14) yes
C8 . C12 . C17 . 120.51(14) yes
C13 . C12 . C17 . 118.83(14) yes
C12 . C13 . C14 . 120.12(15) yes
C12 . C13 . H131 . 119.7 no
C14 . C13 . H131 . 120.2 no
C13 . C14 . C15 . 120.39(15) yes
C13 . C14 . H141 . 120.0 no
C15 . C14 . H141 . 119.6 no
C14 . C15 . C16 . 119.93(15) yes
C14 . C15 . H151 . 119.0 no
C16 . C15 . H151 . 121.1 no
C15 . C16 . C17 . 119.74(16) yes
C15 . C16 . H161 . 121.3 no
C17 . C16 . H161 . 119.0 no
C12 . C17 . C16 . 120.96(15) yes
C12 . C17 . H171 . 119.2 no
C16 . C17 . H171 . 119.8 no
C9 . C18 . C19 . 118.90(14) yes
C9 . C18 . C23 . 121.97(13) yes
C19 . C18 . C23 . 119.13(14) yes
C18 . C19 . C20 . 120.00(15) yes
C18 . C19 . H191 . 118.8 no
C20 . C19 . H191 . 121.2 no
C19 . C20 . C21 . 120.59(15) yes
C19 . C20 . H201 . 120.4 no
C21 . C20 . H201 . 119.0 no
C20 . C21 . C22 . 119.81(15) yes
C20 . C21 . H211 . 119.1 no
C22 . C21 . H211 . 121.0 no
C21 . C22 . C23 . 119.97(16) yes
C21 . C22 . H221 . 121.0 no
C23 . C22 . H221 . 119.0 no
C18 . C23 . C22 . 120.48(15) yes
C18 . C23 . H231 . 119.5 no
C22 . C23 . H231 . 120.0 no
C9 . O2 . Ni1 5_656 109.31(9) yes
C8 . O1 . Ni1 . 108.64(9) yes
N1 . Ni1 . N1 5_656 98.20(4) yes
N1 . Ni1 . Ni1 5_656 47.63(3) yes
N1 5_656 Ni1 . Ni1 5_656 51.11(3) yes
N1 . Ni1 . O1 . 153.62(4) yes
N1 5_656 Ni1 . O1 . 85.85(4) yes
Ni1 5_656 Ni1 . O1 . 126.79(3) yes
N1 . Ni1 . O2 5_656 82.61(4) yes
N1 5_656 Ni1 . O2 5_656 155.09(4) yes
Ni1 5_656 Ni1 . O2 5_656 127.87(3) yes
O1 . Ni1 . O2 5_656 104.51(4) yes
N1 . Ni1 . N5 5_656 96.48(5) yes
N1 5_656 Ni1 . N5 5_656 76.39(5) yes
Ni1 5_656 Ni1 . N5 5_656 90.85(3) yes
O1 . Ni1 . N5 5_656 109.77(5) yes
O2 5_656 Ni1 . N5 5_656 78.78(4) yes
N1 . Ni1 . N2 . 74.51(5) yes
N1 5_656 Ni1 . N2 . 106.68(5) yes
Ni1 5_656 Ni1 . N2 . 84.68(4) yes
O1 . Ni1 . N2 . 79.35(5) yes
O2 5_656 Ni1 . N2 . 97.56(5) yes
N5 5_656 Ni1 . N2 . 170.72(5) yes
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cpd3
_database_code_depnum_ccdc_archive 'CCDC 1957999'
loop_
_audit_author_name
_audit_author_address
'Carine Duhayon'
;LCC CNRS
France
;
_audit_update_record             
;
2019-10-08 deposited with the CCDC.	2019-12-16 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          'disorderd ligand'
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   11.5125(3)
_cell_length_b                   16.4374(3)
_cell_length_c                   19.5359(4)
_cell_angle_alpha                90
_cell_angle_beta                 106.980(2)
_cell_angle_gamma                90
_cell_volume                     3535.72(15)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n '
_symmetry_space_group_name_Hall  '-P 2yn '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,-y+1/2,z+1/2
-x+1/2,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cr 0.3209 0.6236 10.6406 6.1038 7.3537 0.3920 3.3240 20.2626 1.4922 98.7399
1.1832 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C73 H63 Cr2 N21 Ni1 O6 
# Dc =      1.40 Fooo =   1544.00 Mu =      6.34 M =   1493.14
# Found Formula = C73 H38 Cr2 N21 Ni1 O6 
# Dc =      1.38 FOOO =   1494.00 Mu =      6.34 M =   1467.94

_chemical_formula_sum            'C73 H63 Cr2 N21 Ni1 O6'
_chemical_formula_moiety         'C73 H59 Cr2 N21 Ni O4, 2(H2 O)'
_chemical_compound_source        .
_chemical_formula_weight         1493.14


_cell_measurement_reflns_used    9926
_cell_measurement_theta_min      2
_cell_measurement_theta_max      28
_cell_measurement_temperature    100

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.15
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_max          0.2

_exptl_crystal_density_diffrn    1.40
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1494
_exptl_absorpt_coefficient_mu    0.634

# Sheldrick geometric approximatio 1.00 1.00 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  1.00
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      100
_diffrn_reflns_number            104637
_reflns_number_total             11367
_diffrn_reflns_av_R_equivalents  0.114
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 11367 
# Theoretical number of reflections is about 24036 


_diffrn_reflns_theta_min         1.650
_diffrn_reflns_theta_max         31.810
_diffrn_measured_fraction_theta_max 0.942

_diffrn_reflns_theta_full        27.356
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_reflns_limit_h_min              -16
_reflns_limit_h_max              15
_reflns_limit_k_min              0
_reflns_limit_k_max              24
_reflns_limit_l_min              0
_reflns_limit_l_max              28


_atom_sites_solution_primary     other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.52
_refine_diff_density_max         2.09


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_refine_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_restraints     0
_refine_ls_number_parameters     418
_refine_ls_number_reflns         8067
_oxford_refine_ls_R_factor_ref   0.1013
_refine_ls_wR_factor_ref         0.1109
_refine_ls_goodness_of_fit_ref   1.0486
_refine_ls_shift/su_max          0.0005441
_refine_ls_shift/su_mean         0.0000385


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        8067
_refine_ls_R_factor_all          0.1013
_refine_ls_wR_factor_all         0.1109

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                8067
_refine_ls_R_factor_gt           0.1013
_refine_ls_wR_factor_gt          0.1109


_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 5.23 4.67 4.16 1.15 0.993E-01 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cr1 Cr 0.90360(5) 0.86923(4) 0.65631(3) 0.0235 1.0000 Uani . . . . . .
Ni1 Ni 0.5000 1.0000 0.5000 0.0593 1.0000 Uani S . . . . .
C1 C 0.7621(3) 0.9352(2) 0.59063(19) 0.0257 1.0000 Uani . . . . . .
C2 C 1.0566(4) 0.8063(3) 0.7162(2) 0.0324 1.0000 Uani . . . . . .
C3 C 1.0653(3) 1.0362(2) 0.6882(2) 0.0277 1.0000 Uani . . . . . .
C4 C 1.1450(4) 1.0990(3) 0.6824(2) 0.0330 1.0000 Uani . . . . . .
C5 C 1.1985(4) 1.0930(3) 0.6273(3) 0.0369 1.0000 Uani . . . . . .
C6 C 1.1746(3) 1.0272(3) 0.5810(2) 0.0353 1.0000 Uani . . . . . .
C7 C 1.0952(3) 0.9668(3) 0.5917(2) 0.0289 1.0000 Uani . . . . . .
C8 C 1.0548(3) 0.8953(3) 0.5464(2) 0.0286 1.0000 Uani . . . . . .
C9 C 1.1037(4) 0.8746(3) 0.4854(2) 0.0379 1.0000 Uani . . . . . .
C10 C 0.8466(4) 0.7499(3) 0.5486(2) 0.0308 1.0000 Uani . . . . . .
C11 C 0.8003(3) 0.8949(2) 0.76891(18) 0.0246 1.0000 Uani . . . . . .
C12 C 0.9965(3) 1.0344(2) 0.7404(2) 0.0280 1.0000 Uani . . . . . .
C13 C 1.0053(4) 1.1020(3) 0.7928(2) 0.0380 1.0000 Uani . . . . . .
C14 C 0.7739(4) 0.6821(3) 0.5095(2) 0.0369 1.0000 Uani . . . . . .
C15 C 0.7698(6) 0.6645(4) 0.4383(3) 0.0532 1.0000 Uani . . . . . .
C16 C 0.6955(7) 0.6018(4) 0.4024(3) 0.0644 1.0000 Uani . . . . . .
C17 C 0.6254(7) 0.5577(4) 0.4360(3) 0.0661 1.0000 Uani . . . . . .
C18 C 0.6309(6) 0.5740(4) 0.5069(3) 0.0600 1.0000 Uani . . . . . .
C19 C 0.7040(5) 0.6368(3) 0.5425(3) 0.0492 1.0000 Uani . . . . . .
C20 C 0.7199(4) 0.8742(3) 0.8139(2) 0.0314 1.0000 Uani . . . . . .
C21 C 0.6640(4) 0.7990(3) 0.8063(2) 0.0421 1.0000 Uani . . . . . .
C22 C 0.5934(5) 0.7778(4) 0.8509(3) 0.0550 1.0000 Uani . . . . . .
C23 C 0.5786(5) 0.8312(4) 0.9015(3) 0.0545 1.0000 Uani . . . . . .
C24 C 0.6333(5) 0.9062(4) 0.9086(3) 0.0533 1.0000 Uani . . . . . .
C25 C 0.7038(5) 0.9282(3) 0.8650(3) 0.0427 1.0000 Uani . . . . . .
N1 N 0.6764(4) 0.9646(3) 0.5530(2) 0.0501 1.0000 Uani . . . . . .
N2 N 1.1408(4) 0.7677(3) 0.7455(2) 0.0511 1.0000 Uani . . . . . .
N3 N 1.0426(3) 0.9729(2) 0.64433(17) 0.0262 1.0000 Uani . . . . . .
N4 N 0.9724(3) 0.8529(2) 0.56336(17) 0.0267 1.0000 Uani . . . . . .
N5 N 0.9222(3) 0.7875(2) 0.51999(18) 0.0303 1.0000 Uani . . . . . .
N6 N 0.8589(3) 0.9645(2) 0.78176(17) 0.0281 1.0000 Uani . . . . . .
N7 N 0.9288(3) 0.97046(19) 0.73527(16) 0.0248 1.0000 Uani . . . . . .
O1 O 0.8305(3) 0.76950(19) 0.60977(15) 0.0330 1.0000 Uani . . . . . .
O2 O 0.8083(2) 0.84270(18) 0.72178(14) 0.0291 1.0000 Uani . . . . . .
C100 C 0.5338(7) 1.0098(3) 0.3446(3) 0.0401(19) 0.5000 Uiso G . . . . .
C101 C 0.5705(8) 1.0474(4) 0.2906(3) 0.057(4) 0.5000 Uiso G . . . . .
C102 C 0.6131(8) 1.1271(4) 0.2992(3) 0.047(2) 0.5000 Uiso G . . . . .
C103 C 0.6191(6) 1.1692(3) 0.3620(3) 0.055(3) 0.5000 Uiso G . . . . .
C104 C 0.5824(5) 1.1316(3) 0.4160(2) 0.0530(12) 1.0000 Uiso G . . . . .
C105 C 0.5746(11) 1.1708(8) 0.4838(7) 0.055(3) 0.5000 Uiso . . . . . .
C106 C 0.6173(7) 1.2579(5) 0.4960(4) 0.0752(19) 1.0000 Uiso . . . . . .
C107 C 0.5169(7) 1.2401(5) 0.6165(4) 0.078(2) 1.0000 Uiso . . . . . .
C108 C 0.4997(9) 1.0868(4) 0.6358(5) 0.050(3) 0.5000 Uiso G . . . . .
C109 C 0.5257(13) 1.1044(7) 0.7082(6) 0.105(7) 0.5000 Uiso G . . . . .
C110 C 0.4769(15) 1.0373(8) 0.7303(5) 0.131(8) 0.5000 Uiso G . . . . .
C111 C 0.4235(13) 0.9502(7) 0.6934(6) 0.098(7) 0.5000 Uiso G . . . . .
C112 C 0.4445(9) 0.9553(4) 0.6317(5) 0.055(3) 0.5000 Uiso G . . . . .
C114 C 0.3748(10) 0.8050(7) 0.6111(6) 0.051(2) 0.5000 Uiso . . . . . .
C115 C 0.364(2) 0.8249(15) 0.6788(13) 0.117(7) 0.5000 Uiso . . . . . .
C116 C 0.391(2) 0.9035(16) 0.7213(13) 0.116(7) 0.5000 Uiso . . . . . .
C117 C 0.3546(10) 0.7335(7) 0.5634(6) 0.048(2) 0.5000 Uiso . . . . . .
C119 C 0.4275(9) 0.8234(6) 0.4813(6) 0.0388(19) 0.5000 Uiso . . . . . .
C121 C 0.4929(8) 0.9340(6) 0.3438(5) 0.0342(18) 0.5000 Uiso . . . . . .
C122 C 0.4308(12) 0.8965(8) 0.2706(7) 0.052(3) 0.5000 Uiso . . . . . .
N8 N 0.5397(5) 1.0519(3) 0.4074(3) 0.0409(17) 0.5000 Uiso G . . . . .
N9 N 0.5441(10) 1.1233(7) 0.5273(6) 0.058(2) 0.5000 Uiso . . . . . .
N10 N 0.5309(12) 1.1349(9) 0.5955(7) 0.066(3) 0.5000 Uiso . . . . . .
N11 N 0.4741(8) 1.0114(5) 0.6051(4) 0.070(3) 0.5000 Uiso G . . . . .
N12 N 0.4366(7) 0.8819(5) 0.5229(4) 0.0415(17) 0.5000 Uiso . . . . . .
N13 N 0.4491(6) 0.8296(4) 0.4138(3) 0.0243(12) 0.5000 Uiso . . . . . .
N14 N 0.4816(7) 0.9083(5) 0.4014(4) 0.0344(15) 0.5000 Uiso . . . . . .
O3 O 0.6997(13) 0.8298(9) 0.1383(8) 0.047(3) 0.2500 Uiso . . . . . .
O4 O 0.6823(9) 0.8769(6) 0.1654(5) 0.051(2) 0.4000 Uiso . . . . . .
O5 O 0.5903(10) 0.8944(7) 0.1041(6) 0.050(2) 0.3500 Uiso . . . . . .
H41 H 1.1603 1.1438 0.7139 0.0420 1.0000 Uiso R . . . . .
H51 H 1.2502 1.1343 0.6207 0.0472 1.0000 Uiso R . . . . .
H61 H 1.2111 1.0230 0.5432 0.0451 1.0000 Uiso R . . . . .
H93 H 1.0361 0.8643 0.4429 0.0612 1.0000 Uiso R . . . . .
H92 H 1.1537 0.8263 0.4965 0.0611 1.0000 Uiso R . . . . .
H91 H 1.1522 0.9193 0.4753 0.0613 1.0000 Uiso R . . . . .
H133 H 0.9528 1.0903 0.8221 0.0601 1.0000 Uiso R . . . . .
H132 H 1.0882 1.1056 0.8219 0.0603 1.0000 Uiso R . . . . .
H131 H 0.9820 1.1524 0.7668 0.0600 1.0000 Uiso R . . . . .
H151 H 0.8170 0.6963 0.4156 0.0681 1.0000 Uiso R . . . . .
H161 H 0.6920 0.5894 0.3544 0.0822 1.0000 Uiso R . . . . .
H171 H 0.5745 0.5156 0.4112 0.0842 1.0000 Uiso R . . . . .
H181 H 0.5862 0.5430 0.5311 0.0780 1.0000 Uiso R . . . . .
H191 H 0.7067 0.6491 0.5900 0.0611 1.0000 Uiso R . . . . .
H211 H 0.6722 0.7627 0.7705 0.0552 1.0000 Uiso R . . . . .
H221 H 0.5541 0.7269 0.8455 0.0682 1.0000 Uiso R . . . . .
H231 H 0.5325 0.8156 0.9320 0.0710 1.0000 Uiso R . . . . .
H241 H 0.6248 0.9431 0.9437 0.0702 1.0000 Uiso R . . . . .
H251 H 0.7424 0.9793 0.8701 0.0552 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None

loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cr1 . C1 . 2.063(4) yes
Cr1 . C2 . 2.082(4) yes
Cr1 . N3 . 2.396(3) yes
Cr1 . N4 . 2.200(3) yes
Cr1 . N7 . 2.230(3) yes
Cr1 . O1 . 1.943(3) yes
Cr1 . O2 . 1.962(3) yes
Ni1 . N14 2_676 2.406(8) yes
Ni1 . N11 2_676 2.167(7) yes
Ni1 . N8 2_676 2.167(4) yes
Ni1 . N12 2_676 2.166(9) yes
Ni1 . N9 2_676 2.119(11) yes
Ni1 . N1 2_676 2.075(4) yes
Ni1 . N10 2_676 2.852(14) yes
Ni1 . N1 . 2.075(4) yes
Ni1 . N8 . 2.167(4) yes
Ni1 . N9 . 2.119(11) yes
Ni1 . N10 . 2.852(14) yes
Ni1 . N11 . 2.167(7) yes
Ni1 . N12 . 2.166(9) yes
Ni1 . N14 . 2.406(8) yes
C1 . N1 . 1.151(6) yes
C2 . N2 . 1.160(6) yes
C3 . C4 . 1.408(5) yes
C3 . C12 . 1.463(5) yes
C3 . N3 . 1.324(5) yes
C4 . C5 . 1.391(6) yes
C4 . H41 . 0.944 no
C5 . C6 . 1.385(7) yes
C5 . H51 . 0.936 no
C6 . C7 . 1.406(5) yes
C6 . H61 . 0.951 no
C7 . C8 . 1.463(6) yes
C7 . N3 . 1.342(5) yes
C8 . C9 . 1.498(5) yes
C8 . N4 . 1.295(5) yes
C9 . H93 . 0.973 no
C9 . H92 . 0.967 no
C9 . H91 . 0.977 no
C10 . C14 . 1.468(6) yes
C10 . N5 . 1.318(5) yes
C10 . O1 . 1.301(5) yes
C11 . C20 . 1.489(5) yes
C11 . N6 . 1.314(5) yes
C11 . O2 . 1.282(5) yes
C12 . C13 . 1.493(6) yes
C12 . N7 . 1.295(5) yes
C13 . H133 . 0.965 no
C13 . H132 . 0.960 no
C13 . H131 . 0.968 no
C14 . C15 . 1.408(7) yes
C14 . C19 . 1.385(7) yes
C15 . C16 . 1.391(8) yes
C15 . H151 . 0.951 no
C16 . C17 . 1.384(9) yes
C16 . H161 . 0.950 no
C17 . C18 . 1.393(9) yes
C17 . H171 . 0.944 no
C18 . C19 . 1.384(7) yes
C18 . H181 . 0.944 no
C19 . H191 . 0.941 no
C20 . C21 . 1.382(6) yes
C20 . C25 . 1.387(6) yes
C21 . C22 . 1.397(6) yes
C21 . H211 . 0.946 no
C22 . C23 . 1.370(8) yes
C22 . H221 . 0.943 no
C23 . C24 . 1.372(9) yes
C23 . H231 . 0.941 no
C24 . C25 . 1.386(6) yes
C24 . H241 . 0.941 no
C25 . H251 . 0.942 no
N4 . N5 . 1.386(5) yes
N6 . N7 . 1.382(4) yes
C100 . C110 2_676 1.629(8) yes
C100 . C108 2_676 1.703(9) yes
C100 . C111 2_676 1.20(1) yes
C100 . N11 2_676 1.070(9) yes
C100 . C101 . 1.391 yes
C100 . C121 . 1.331(11) yes
C100 . N8 . 1.392 yes
C101 . C110 2_676 1.508(15) yes
C101 . C112 2_676 1.577(10) yes
C101 . C116 2_676 0.98(3) yes
C101 . C102 . 1.392 yes
C102 . C111 2_676 1.359(12) yes
C102 . C115 2_676 0.90(2) yes
C102 . C103 . 1.392 yes
C103 . C115 2_676 0.88(2) yes
C103 . C104 . 1.391 yes
C104 . C112 2_676 1.685(8) yes
C104 . C114 2_676 1.328(13) yes
C104 . N12 2_676 1.294(9) yes
C104 . C105 . 1.498(14) yes
C104 . N8 . 1.391 yes
C105 . N12 2_676 0.880(13) yes
C105 . C106 . 1.510(15) yes
C105 . N9 . 1.278(17) yes
C106 . C119 2_676 1.543(13) yes
C106 . C117 2_676 1.301(13) yes
C107 . N13 2_676 1.397(10) yes
C107 . N10 . 1.796(17) yes
C108 . C122 2_676 1.789(17) yes
C108 . N14 2_676 0.820(11) yes
C108 . C109 . 1.388 yes
C108 . N10 . 1.241(16) yes
C108 . N11 . 1.371 yes
C109 . C121 2_676 1.161(12) yes
C109 . C110 . 1.363 yes
C110 . C122 2_676 1.52(2) yes
C110 . C121 2_676 1.652(12) yes
C110 . C111 . 1.640 yes
C111 . C112 . 1.299 yes
C111 . C116 . 1.07(2) yes
C112 . N8 2_676 0.844(10) yes
C112 . N11 . 1.157 yes
C114 . C115 . 1.40(3) yes
C114 . C117 . 1.476(16) yes
C115 . C116 . 1.52(3) yes
C119 . N10 2_676 1.836(17) yes
C119 . N9 2_676 0.968(13) yes
C119 . N12 . 1.244(13) yes
C119 . N13 . 1.415(12) yes
C121 . N10 2_676 1.719(17) yes
C121 . N11 2_676 1.315(12) yes
C121 . C122 . 1.528(16) yes
C121 . N14 . 1.244(12) yes
N8 . N12 2_676 1.702(10) yes
N8 . N11 2_676 1.070(9) yes
N9 . N14 2_676 1.593(13) yes
N9 . N13 2_676 1.370(12) yes
N9 . N12 2_676 1.070(12) yes
N9 . N10 . 1.397(16) yes
N11 . N14 2_676 1.434(12) yes
N13 . N14 . 1.388(10) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 . Cr1 . C2 . 174.40(15) yes
C1 . Cr1 . N3 . 89.67(13) yes
C2 . Cr1 . N3 . 85.90(14) yes
C1 . Cr1 . N4 . 87.72(12) yes
C2 . Cr1 . N4 . 87.35(14) yes
N3 . Cr1 . N4 . 66.07(12) yes
C1 . Cr1 . N7 . 87.59(13) yes
C2 . Cr1 . N7 . 93.66(14) yes
N3 . Cr1 . N7 . 65.22(11) yes
N4 . Cr1 . N7 . 131.06(12) yes
C1 . Cr1 . O1 . 89.81(14) yes
C2 . Cr1 . O1 . 91.36(15) yes
N3 . Cr1 . O1 . 139.89(12) yes
N4 . Cr1 . O1 . 73.84(12) yes
N7 . Cr1 . O1 . 154.76(12) yes
C1 . Cr1 . O2 . 91.83(12) yes
C2 . Cr1 . O2 . 93.76(14) yes
N3 . Cr1 . O2 . 137.60(12) yes
N4 . Cr1 . O2 . 156.33(13) yes
N7 . Cr1 . O2 . 72.51(11) yes
O1 . Cr1 . O2 . 82.50(12) yes
N14 2_676 Ni1 . N11 2_676 143.9(3) yes
N14 2_676 Ni1 . N8 2_676 64.4(2) yes
N11 2_676 Ni1 . N8 2_676 151.4(2) yes
N14 2_676 Ni1 . N12 2_676 69.4(3) yes
N11 2_676 Ni1 . N12 2_676 74.6(3) yes
N8 2_676 Ni1 . N12 2_676 133.7(3) yes
N14 2_676 Ni1 . N9 2_676 139.4(4) yes
N11 2_676 Ni1 . N9 2_676 76.6(4) yes
N8 2_676 Ni1 . N9 2_676 74.9(3) yes
N12 2_676 Ni1 . N9 2_676 151.1(3) yes
N14 2_676 Ni1 . N1 2_676 93.9(2) yes
N11 2_676 Ni1 . N1 2_676 86.4(3) yes
N8 2_676 Ni1 . N1 2_676 96.46(19) yes
N12 2_676 Ni1 . N1 2_676 89.2(3) yes
N9 2_676 Ni1 . N1 2_676 90.9(3) yes
N14 2_676 Ni1 . N10 2_676 167.3(3) yes
N8 2_676 Ni1 . N10 2_676 102.9(3) yes
N12 2_676 Ni1 . N10 2_676 123.2(4) yes
N14 2_676 Ni1 . N1 . 86.1(2) yes
N11 2_676 Ni1 . N1 . 93.6(3) yes
N8 2_676 Ni1 . N1 . 83.54(19) yes
N12 2_676 Ni1 . N1 . 90.8(3) yes
N9 2_676 Ni1 . N1 . 89.1(3) yes
N14 2_676 Ni1 . N8 . 115.6(2) yes
N8 2_676 Ni1 . N8 . 179.99 yes
N9 2_676 Ni1 . N8 . 105.1(3) yes
N11 2_676 Ni1 . N9 . 103.4(4) yes
N8 2_676 Ni1 . N9 . 105.1(3) yes
N9 2_676 Ni1 . N9 . 179.99 yes
N11 2_676 Ni1 . N10 . 131.4(4) yes
N8 2_676 Ni1 . N10 . 77.1(3) yes
N9 2_676 Ni1 . N10 . 152.0(4) yes
N11 2_676 Ni1 . N11 . 179.99 yes
N12 2_676 Ni1 . N11 . 105.4(3) yes
N9 2_676 Ni1 . N11 . 103.4(4) yes
N14 2_676 Ni1 . N12 . 110.6(3) yes
N11 2_676 Ni1 . N12 . 105.4(3) yes
N12 2_676 Ni1 . N12 . 179.99 yes
N14 2_676 Ni1 . N14 . 180.00 yes
N8 2_676 Ni1 . N14 . 115.6(2) yes
N12 2_676 Ni1 . N14 . 110.6(3) yes
N1 2_676 Ni1 . N10 2_676 88.5(3) yes
N1 2_676 Ni1 . N1 . 179.99 yes
N10 2_676 Ni1 . N1 . 91.5(3) yes
N1 2_676 Ni1 . N8 . 83.54(19) yes
N10 2_676 Ni1 . N8 . 77.1(3) yes
N1 . Ni1 . N8 . 96.46(19) yes
N1 2_676 Ni1 . N9 . 89.1(3) yes
N10 2_676 Ni1 . N9 . 152.0(4) yes
N1 . Ni1 . N9 . 90.9(3) yes
N8 . Ni1 . N9 . 74.9(3) yes
N1 2_676 Ni1 . N10 . 91.5(3) yes
N10 2_676 Ni1 . N10 . 180.00 yes
N1 . Ni1 . N10 . 88.5(3) yes
N8 . Ni1 . N10 . 102.9(3) yes
N1 2_676 Ni1 . N11 . 93.6(3) yes
N10 2_676 Ni1 . N11 . 131.4(4) yes
N1 . Ni1 . N11 . 86.4(3) yes
N8 . Ni1 . N11 . 151.4(2) yes
N9 . Ni1 . N11 . 76.6(4) yes
N1 2_676 Ni1 . N12 . 90.8(3) yes
N10 2_676 Ni1 . N12 . 56.8(4) yes
N1 . Ni1 . N12 . 89.2(3) yes
N8 . Ni1 . N12 . 133.7(3) yes
N9 . Ni1 . N12 . 151.1(3) yes
N1 2_676 Ni1 . N14 . 86.1(2) yes
N10 2_676 Ni1 . N14 . 12.7(3) yes
N1 . Ni1 . N14 . 93.9(2) yes
N8 . Ni1 . N14 . 64.4(2) yes
N9 . Ni1 . N14 . 139.4(4) yes
N10 . Ni1 . N12 . 123.2(4) yes
N11 . Ni1 . N12 . 74.6(3) yes
N10 . Ni1 . N14 . 167.3(3) yes
N11 . Ni1 . N14 . 143.9(3) yes
N12 . Ni1 . N14 . 69.4(3) yes
Cr1 . C1 . N1 . 173.0(4) yes
Cr1 . C2 . N2 . 175.2(4) yes
C4 . C3 . C12 . 124.7(4) yes
C4 . C3 . N3 . 122.2(4) yes
C12 . C3 . N3 . 113.0(3) yes
C3 . C4 . C5 . 117.2(4) yes
C3 . C4 . H41 . 121.4 no
C5 . C4 . H41 . 121.3 no
C4 . C5 . C6 . 120.8(4) yes
C4 . C5 . H51 . 119.9 no
C6 . C5 . H51 . 119.3 no
C5 . C6 . C7 . 117.9(4) yes
C5 . C6 . H61 . 120.9 no
C7 . C6 . H61 . 121.2 no
C6 . C7 . C8 . 125.7(4) yes
C6 . C7 . N3 . 121.3(4) yes
C8 . C7 . N3 . 112.9(3) yes
C7 . C8 . C9 . 122.4(4) yes
C7 . C8 . N4 . 113.9(3) yes
C9 . C8 . N4 . 123.7(4) yes
C8 . C9 . H93 . 109.1 no
C8 . C9 . H92 . 110.2 no
H93 . C9 . H92 . 108.9 no
C8 . C9 . H91 . 111.1 no
H93 . C9 . H91 . 108.7 no
H92 . C9 . H91 . 108.9 no
C14 . C10 . N5 . 118.8(4) yes
C14 . C10 . O1 . 117.0(4) yes
N5 . C10 . O1 . 124.3(4) yes
C20 . C11 . N6 . 117.3(3) yes
C20 . C11 . O2 . 117.3(3) yes
N6 . C11 . O2 . 125.4(3) yes
C3 . C12 . C13 . 121.4(3) yes
C3 . C12 . N7 . 113.5(4) yes
C13 . C12 . N7 . 125.2(4) yes
C12 . C13 . H133 . 109.2 no
C12 . C13 . H132 . 107.9 no
H133 . C13 . H132 . 110.4 no
C12 . C13 . H131 . 109.0 no
H133 . C13 . H131 . 110.9 no
H132 . C13 . H131 . 109.4 no
C10 . C14 . C15 . 121.3(4) yes
C10 . C14 . C19 . 119.1(4) yes
C15 . C14 . C19 . 119.5(5) yes
C14 . C15 . C16 . 119.2(6) yes
C14 . C15 . H151 . 119.2 no
C16 . C15 . H151 . 121.6 no
C15 . C16 . C17 . 120.5(5) yes
C15 . C16 . H161 . 119.9 no
C17 . C16 . H161 . 119.6 no
C16 . C17 . C18 . 120.4(5) yes
C16 . C17 . H171 . 120.0 no
C18 . C17 . H171 . 119.6 no
C17 . C18 . C19 . 119.2(6) yes
C17 . C18 . H181 . 121.4 no
C19 . C18 . H181 . 119.4 no
C14 . C19 . C18 . 121.2(5) yes
C14 . C19 . H191 . 119.1 no
C18 . C19 . H191 . 119.8 no
C11 . C20 . C21 . 119.5(4) yes
C11 . C20 . C25 . 121.0(4) yes
C21 . C20 . C25 . 119.5(4) yes
C20 . C21 . C22 . 119.6(5) yes
C20 . C21 . H211 . 119.9 no
C22 . C21 . H211 . 120.4 no
C21 . C22 . C23 . 120.5(5) yes
C21 . C22 . H221 . 119.9 no
C23 . C22 . H221 . 119.6 no
C22 . C23 . C24 . 119.9(4) yes
C22 . C23 . H231 . 119.6 no
C24 . C23 . H231 . 120.5 no
C23 . C24 . C25 . 120.4(5) yes
C23 . C24 . H241 . 120.7 no
C25 . C24 . H241 . 118.9 no
C20 . C25 . C24 . 120.1(5) yes
C20 . C25 . H251 . 119.3 no
C24 . C25 . H251 . 120.6 no
Ni1 . N1 . C1 . 165.5(4) yes
Cr1 . N3 . C7 . 119.0(3) yes
Cr1 . N3 . C3 . 120.4(2) yes
C7 . N3 . C3 . 120.5(3) yes
Cr1 . N4 . C8 . 127.8(3) yes
Cr1 . N4 . N5 . 114.4(2) yes
C8 . N4 . N5 . 117.8(3) yes
N4 . N5 . C10 . 108.2(3) yes
C11 . N6 . N7 . 107.5(3) yes
Cr1 . N7 . N6 . 114.7(2) yes
Cr1 . N7 . C12 . 127.8(3) yes
N6 . N7 . C12 . 117.4(3) yes
C10 . O1 . Cr1 . 118.7(3) yes
Cr1 . O2 . C11 . 119.4(2) yes
C110 2_676 C100 . C108 2_676 78.2(3) yes
C110 2_676 C100 . C111 2_676 68.9(4) yes
C108 2_676 C100 . C111 2_676 144.1(7) yes
C110 2_676 C100 . N11 2_676 131.7(7) yes
C108 2_676 C100 . N11 2_676 53.5(4) yes
C111 2_676 C100 . N11 2_676 155.0(9) yes
C110 2_676 C100 . C101 . 59.3(6) yes
C108 2_676 C100 . C101 . 136.3(5) yes
N11 2_676 C100 . C101 . 165.2(6) yes
C110 2_676 C100 . C121 . 67.0(6) yes
C111 2_676 C100 . C121 . 135.4(8) yes
N11 2_676 C100 . C121 . 65.3(7) yes
C101 . C100 . C121 . 126.2(6) yes
C110 2_676 C100 . N8 . 178.0(8) yes
C108 2_676 C100 . N8 . 102.9(5) yes
C111 2_676 C100 . N8 . 110.5(6) yes
C101 . C100 . N8 . 120.00 yes
C121 . C100 . N8 . 113.8(6) yes
C110 2_676 C101 . C112 2_676 95.8(6) yes
C110 2_676 C101 . C100 . 68.2(5) yes
C110 2_676 C101 . C116 2_676 148.2(16) yes
C112 2_676 C101 . C116 2_676 115.7(15) yes
C100 . C101 . C116 2_676 143.3(15) yes
C110 2_676 C101 . C102 . 171.5(5) yes
C112 2_676 C101 . C102 . 92.5(3) yes
C100 . C101 . C102 . 120.00 yes
C101 . C102 . C115 2_676 158.1(15) yes
C111 2_676 C102 . C115 2_676 145.8(16) yes
C101 . C102 . C103 . 120.00 yes
C111 2_676 C102 . C103 . 108.0(5) yes
C102 . C103 . C104 . 120.00 yes
C115 2_676 C103 . C104 . 159.2(16) yes
C112 2_676 C104 . C103 . 90.2(3) yes
C112 2_676 C104 . C114 2_676 118.3(6) yes
C112 2_676 C104 . N12 2_676 108.2(6) yes
C103 . C104 . N12 2_676 161.2(5) yes
C114 2_676 C104 . N12 2_676 133.3(7) yes
C112 2_676 C104 . C105 . 143.7(7) yes
C103 . C104 . C105 . 126.1(6) yes
C114 2_676 C104 . C105 . 98.1(8) yes
C103 . C104 . N8 . 120.00 yes
C114 2_676 C104 . N8 . 148.1(5) yes
N12 2_676 C104 . N8 . 78.6(5) yes
C105 . C104 . N8 . 113.7(6) yes
C104 . C105 . N12 2_676 59.3(10) yes
C104 . C105 . C106 . 116.6(9) yes
N12 2_676 C105 . C106 . 169.7(15) yes
C104 . C105 . N9 . 115.1(11) yes
N12 2_676 C105 . N9 . 55.9(10) yes
C106 . C105 . N9 . 127.9(12) yes
C119 2_676 C106 . C117 2_676 122.8(9) yes
C105 . C106 . C117 2_676 96.6(9) yes
C100 2_676 C108 . C122 2_676 88.7(7) yes
C100 2_676 C108 . N14 2_676 115.2(10) yes
C122 2_676 C108 . N14 2_676 137.3(11) yes
C100 2_676 C108 . C109 . 87.8(3) yes
N14 2_676 C108 . C109 . 148.0(10) yes
C100 2_676 C108 . N10 . 149.6(10) yes
C122 2_676 C108 . N10 . 115.1(9) yes
C109 . C108 . N10 . 119.9(10) yes
C122 2_676 C108 . N11 . 124.1(7) yes
N14 2_676 C108 . N11 . 77.3(9) yes
C109 . C108 . N11 . 126.14 yes
N10 . C108 . N11 . 111.3(10) yes
C108 . C109 . C110 . 99.62 yes
C121 2_676 C109 . C110 . 81.3(6) yes
C122 2_676 C110 . C101 2_676 148.7(11) yes
C122 2_676 C110 . C100 2_676 101.5(9) yes
C101 2_676 C110 . C100 2_676 52.5(3) yes
C122 2_676 C110 . C121 2_676 57.3(7) yes
C101 2_676 C110 . C121 2_676 100.3(5) yes
C101 2_676 C110 . C109 . 144.3(4) yes
C100 2_676 C110 . C109 . 91.8(3) yes
C122 2_676 C110 . C111 . 142.3(8) yes
C121 2_676 C110 . C111 . 90.7(4) yes
C109 . C110 . C111 . 134.74 yes
C110 . C111 . C102 2_676 149.1(8) yes
C110 . C111 . C100 2_676 68.0(4) yes
C102 2_676 C111 . C100 2_676 140.6(11) yes
C110 . C111 . C112 . 101.74 yes
C102 2_676 C111 . C112 . 107.8(8) yes
C110 . C111 . C116 . 123.1(18) yes
C100 2_676 C111 . C116 . 167(2) yes
C112 . C111 . C116 . 134.8(18) yes
C101 2_676 C112 . C104 2_676 117.1(5) yes
C104 2_676 C112 . C111 . 113.9(6) yes
C101 2_676 C112 . N8 2_676 168.6(11) yes
C104 2_676 C112 . N8 2_676 55.4(4) yes
C111 . C112 . N8 2_676 168.1(7) yes
C101 2_676 C112 . N11 . 125.7(5) yes
C104 2_676 C112 . N11 . 117.2(6) yes
C111 . C112 . N11 . 128.85 yes
N8 2_676 C112 . N11 . 62.3(7) yes
C104 2_676 C114 . C115 . 109.9(13) yes
C104 2_676 C114 . C117 . 112.4(9) yes
C115 . C114 . C117 . 137.6(14) yes
C114 . C115 . C102 2_676 124(2) yes
C102 2_676 C115 . C103 2_676 103(2) yes
C114 . C115 . C116 . 131(2) yes
C103 2_676 C115 . C116 . 109(2) yes
C115 . C116 . C111 . 113(2) yes
C115 . C116 . C101 2_676 128(2) yes
C114 . C117 . C106 2_676 116.3(10) yes
C106 2_676 C119 . N10 2_676 138.4(9) yes
C106 2_676 C119 . N9 2_676 173.2(13) yes
C106 2_676 C119 . N12 . 117.0(9) yes
N10 2_676 C119 . N12 . 104.6(9) yes
N9 2_676 C119 . N12 . 56.2(9) yes
C106 2_676 C119 . N13 . 119.6(8) yes
N9 2_676 C119 . N13 . 67.2(9) yes
N12 . C119 . N13 . 123.3(9) yes
C110 2_676 C121 . N10 2_676 155.4(8) yes
C110 2_676 C121 . C100 . 65.2(6) yes
N10 2_676 C121 . C100 . 137.3(8) yes
C110 2_676 C121 . N11 2_676 112.5(8) yes
N10 2_676 C121 . N11 2_676 89.7(7) yes
C110 2_676 C121 . C109 2_676 54.6(5) yes
N10 2_676 C121 . C109 2_676 102.8(9) yes
C100 . C121 . C109 2_676 119.6(10) yes
N11 2_676 C121 . C109 2_676 167.1(11) yes
C110 2_676 C121 . C122 . 57.1(8) yes
N10 2_676 C121 . C122 . 104.8(8) yes
C100 . C121 . C122 . 117.2(9) yes
N11 2_676 C121 . C122 . 159.8(10) yes
C110 2_676 C121 . N14 . 173.5(10) yes
C100 . C121 . N14 . 115.8(8) yes
N11 2_676 C121 . N14 . 68.1(7) yes
C109 2_676 C121 . N14 . 124.5(10) yes
C122 . C121 . N14 . 124.4(9) yes
C121 . C122 . C110 2_676 65.6(7) yes
C110 2_676 C122 . C108 2_676 78.3(7) yes
C100 . N8 . C104 . 120.00 yes
C100 . N8 . N12 2_676 168.0(4) yes
C100 . N8 . Ni1 . 124.8(3) yes
C104 . N8 . Ni1 . 115.0(3) yes
N12 2_676 N8 . Ni1 . 66.8(3) yes
C104 . N8 . N11 2_676 165.2(6) yes
N12 2_676 N8 . N11 2_676 141.5(6) yes
Ni1 . N8 . N11 2_676 75.7(4) yes
C104 . N8 . C112 2_676 94.7(5) yes
N12 2_676 N8 . C112 2_676 142.1(7) yes
Ni1 . N8 . C112 2_676 148.7(6) yes
N11 2_676 N8 . C112 2_676 73.4(6) yes
N14 2_676 N9 . N13 2_676 55.2(5) yes
N14 2_676 N9 . Ni1 . 79.4(5) yes
N13 2_676 N9 . Ni1 . 134.7(7) yes
N14 2_676 N9 . C105 . 159.9(11) yes
N13 2_676 N9 . C105 . 104.7(10) yes
Ni1 . N9 . C105 . 120.6(9) yes
N14 2_676 N9 . N12 2_676 156.4(11) yes
N13 2_676 N9 . N12 2_676 146.9(12) yes
Ni1 . N9 . N12 2_676 78.0(8) yes
N14 2_676 N9 . C119 2_676 127.3(12) yes
N13 2_676 N9 . C119 2_676 72.2(10) yes
Ni1 . N9 . C119 2_676 153.0(11) yes
N12 2_676 N9 . C119 2_676 75.0(11) yes
Ni1 . N9 . N10 . 106.6(9) yes
C105 . N9 . N10 . 132.8(13) yes
N12 2_676 N9 . N10 . 173.6(13) yes
C119 2_676 N9 . N10 . 100.3(13) yes
N9 . N10 . C121 2_676 130.7(11) yes
N9 . N10 . C107 . 113.0(11) yes
C121 2_676 N10 . C107 . 115.7(8) yes
C121 2_676 N10 . C119 2_676 160.5(10) yes
C107 . N10 . C119 2_676 83.6(8) yes
N9 . N10 . C108 . 130.6(14) yes
C107 . N10 . C108 . 114.0(10) yes
C119 2_676 N10 . C108 . 161.8(12) yes
C121 2_676 N10 . Ni1 . 85.7(6) yes
C107 . N10 . Ni1 . 153.6(7) yes
C119 2_676 N10 . Ni1 . 76.6(5) yes
C108 . N10 . Ni1 . 85.2(9) yes
N14 2_676 N11 . Ni1 . 81.1(4) yes
C108 . N11 . Ni1 . 114.9(5) yes
N14 2_676 N11 . C121 2_676 53.6(6) yes
Ni1 . N11 . C121 2_676 133.6(7) yes
N14 2_676 N11 . C112 . 158.7(5) yes
C108 . N11 . C112 . 125.22 yes
Ni1 . N11 . C112 . 119.8(5) yes
C121 2_676 N11 . C112 . 105.1(5) yes
N14 2_676 N11 . C100 2_676 120.5(6) yes
C108 . N11 . C100 2_676 87.6(4) yes
Ni1 . N11 . C100 2_676 155.9(7) yes
C121 2_676 N11 . C100 2_676 66.9(6) yes
N14 2_676 N11 . N8 2_676 155.2(7) yes
C108 . N11 . N8 2_676 167.8(6) yes
Ni1 . N11 . N8 2_676 75.7(4) yes
C121 2_676 N11 . N8 2_676 146.0(8) yes
C100 2_676 N11 . N8 2_676 81.1(6) yes
N8 2_676 N12 . Ni1 . 66.9(3) yes
Ni1 . N12 . C104 2_676 120.1(6) yes
N8 2_676 N12 . C119 . 168.7(9) yes
Ni1 . N12 . C119 . 121.8(7) yes
C104 2_676 N12 . C119 . 117.7(9) yes
N8 2_676 N12 . N9 2_676 139.2(9) yes
Ni1 . N12 . N9 2_676 73.1(8) yes
C104 2_676 N12 . N9 2_676 165.5(11) yes
N8 2_676 N12 . C105 2_676 136.9(13) yes
Ni1 . N12 . C105 2_676 153.6(12) yes
C104 2_676 N12 . C105 2_676 84.9(12) yes
N9 2_676 N12 . C105 2_676 81.2(13) yes
C119 . N13 . C107 2_676 118.8(7) yes
C107 2_676 N13 . N9 2_676 149.9(8) yes
C119 . N13 . N14 . 111.1(7) yes
C107 2_676 N13 . N14 . 124.6(7) yes
N9 2_676 N13 . N14 . 70.6(6) yes
Ni1 . N14 . N9 2_676 60.0(5) yes
Ni1 . N14 . N11 2_676 62.9(4) yes
N9 2_676 N14 . N11 2_676 122.6(7) yes
Ni1 . N14 . N13 . 114.1(5) yes
N11 2_676 N14 . N13 . 174.0(7) yes
Ni1 . N14 . C121 . 120.3(7) yes
N9 2_676 N14 . C121 . 175.5(8) yes
N11 2_676 N14 . C121 . 58.3(6) yes
N13 . N14 . C121 . 125.4(8) yes
Ni1 . N14 . C108 2_676 131.6(9) yes
N9 2_676 N14 . C108 2_676 166.1(11) yes
N11 2_676 N14 . C108 2_676 68.8(7) yes
N13 . N14 . C108 2_676 113.6(10) yes

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C6 . H61 . N1 2_776 171 0.95 2.58 3.526(11) yes
C13 . H132 . O3 2_776 154 0.96 2.57 3.454(11) yes
C13 . H132 . O4 2_776 151 0.96 2.60 3.465(11) yes


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cpd2
_database_code_depnum_ccdc_archive 'CCDC 1958000'
loop_
_audit_author_name
_audit_author_address
'Carine Duhayon'
;LCC CNRS
France
;
_audit_update_record             
;
2019-10-08 deposited with the CCDC.	2019-12-16 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          'disorderd ligand'
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   10.2821(5)
_cell_length_b                   17.4266(7)
_cell_length_c                   14.9144(6)
_cell_angle_alpha                90
_cell_angle_beta                 102.068(2)
_cell_angle_gamma                90
_cell_volume                     2613.3(2)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n '
_symmetry_space_group_name_Hall  '-P 2yn '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,-y+1/2,z+1/2
-x+1/2,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cr 0.3209 0.6236 10.6406 6.1038 7.3537 0.3920 3.3240 20.2626 1.4922 98.7399
1.1832 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543
1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C27 H22 N11 Ni2 O0.50 
# Dc =      1.59 Fooo =   1284.00 Mu =     14.84 M =    625.97
# Found Formula = C27 H21.00 N11 Ni2 O0.50 
# Dc =      1.59 FOOO =   1280.00 Mu =     14.84 M =    624.96

_chemical_formula_sum            'C27 H22.00 N11 Ni2 O0.50'
_chemical_formula_moiety         'C27 H21 N11 Ni2, 0.5(H2 O)'
_chemical_compound_source        ?
_chemical_formula_weight         625.97


_cell_measurement_reflns_used    9959
_cell_measurement_theta_min      3
_cell_measurement_theta_max      27
_cell_measurement_temperature    100

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.150
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1280
_exptl_absorpt_coefficient_mu    1.484

# Sheldrick geometric approximatio 0.74 0.80 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_T_max  0.80
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      100
_diffrn_reflns_number            55318
_reflns_number_total             6471
_diffrn_reflns_av_R_equivalents  0.059
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 6471 
# Theoretical number of reflections is about 12986 


_diffrn_reflns_theta_min         1.821
_diffrn_reflns_theta_max         28.300
_diffrn_measured_fraction_theta_max 0.997

_diffrn_reflns_theta_full        28.300
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_reflns_limit_h_min              -13
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              23
_reflns_limit_l_min              0
_reflns_limit_l_max              19


_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.93
_refine_diff_density_max         2.15


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns         4536
_refine_ls_number_restraints     154
_refine_ls_number_parameters     321
_oxford_refine_ls_R_factor_ref   0.0721
_refine_ls_wR_factor_ref         0.0761
_refine_ls_goodness_of_fit_ref   1.0477
_refine_ls_shift/su_max          0.0022115
_refine_ls_shift/su_mean         0.0001671


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        6458
_refine_ls_R_factor_all          0.0968
_refine_ls_wR_factor_all         0.1131

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4894
_refine_ls_R_factor_gt           0.0763
_refine_ls_wR_factor_gt          0.0793

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.318 0.311 0.103 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ni1 Ni 0.95634(6) 0.25403(3) 0.23395(4) 0.0246 1.0000 Uani . . . . . .
Ni2 Ni 0.70618(7) 0.20441(4) 0.48263(4) 0.0307 1.0000 Uani . . . . . .
C1 C 0.8626(5) 0.2241(3) 0.3219(3) 0.0279 1.0000 Uani . . . . . .
C2 C 0.5476(5) 0.2180(3) 0.6436(3) 0.0272 1.0000 Uani . . . . . .
C3 C 0.9540(7) 0.1544(4) 0.1826(4) 0.0497 0.3000 Uani . . . . . .
C30 C 0.9038(7) 0.1654(4) 0.1679(4) 0.0331 0.7000 Uani . . . . . .
C4 C 0.9738(7) 0.3495(4) 0.2903(4) 0.0350 0.5000 Uani . . . . . .
C40 C 1.0120(7) 0.3435(4) 0.3022(4) 0.0300 0.5000 Uani . . . . . .
N3 N 0.9391(10) 0.0978(4) 0.1393(5) 0.0699 0.3000 Uani . . . . . .
N30 N 0.8672(10) 0.1111(4) 0.1264(5) 0.0648 0.7000 Uani . . . . . .
N4 N 0.9845(10) 0.4066(4) 0.3293(5) 0.0644 0.5000 Uani . . . . . .
N40 N 1.0453(10) 0.3973(4) 0.3456(5) 0.0526 0.5000 Uani . . . . . .
C5 C 0.6326(8) 0.3696(4) 0.4444(7) 0.0398(17) 0.5000 Uiso D . . . . .
C6 C 0.5675(9) 0.4403(4) 0.4170(8) 0.055(2) 0.5000 Uiso D . . . . .
C7 C 0.4473(11) 0.4317(4) 0.3685(14) 0.096(2) 0.5000 Uiso D . . . . .
C8 C 0.3866(8) 0.3600(5) 0.3431(8) 0.051(2) 0.5000 Uiso D . . . . .
C9 C 0.4632(7) 0.2891(4) 0.3729(7) 0.0423(18) 0.5000 Uiso D . . . . .
C10 C 0.4201(6) 0.2120(4) 0.3559(7) 0.044(3) 0.5000 Uiso D . . . . .
C11 C 0.2757(11) 0.2060(5) 0.3127(13) 0.095(6) 0.5000 Uiso D . . . . .
C12 C 0.4072(13) 0.0508(5) 0.2924(9) 0.085(5) 0.5000 Uiso D . . . . .
C13 C 0.6051(6) 0.0430(3) 0.4279(5) 0.0267(18) 0.5000 Uiso D . . . . .
C14 C 0.5987(8) -0.0354(4) 0.4221(6) 0.042(2) 0.5000 Uiso D . . . . .
C15 C 0.7076(8) -0.0741(3) 0.4763(7) 0.044(2) 0.5000 Uiso D . . . . .
C16 C 0.8135(7) -0.0322(3) 0.5317(6) 0.039(2) 0.5000 Uiso D . . . . .
C17 C 0.7983(7) 0.0476(3) 0.5274(6) 0.030(2) 0.5000 Uiso D . . . . .
C18 C 0.9002(6) 0.0969(3) 0.5797(6) 0.035(2) 0.5000 Uiso D . . . . .
C19 C 1.0128(7) 0.0610(3) 0.6317(7) 0.049(3) 0.5000 Uiso D . . . . .
C20 C 1.0273(8) -0.0175(4) 0.6389(7) 0.048(3) 0.5000 Uiso D . . . . .
C21 C 0.9287(10) -0.0634(3) 0.5870(9) 0.063(4) 0.5000 Uiso D . . . . .
C22 C 1.1100(9) 0.1192(4) 0.6788(8) 0.060(3) 0.5000 Uiso D . . . . .
C23 C 1.0917(9) 0.1957(4) 0.6660(8) 0.057(3) 0.5000 Uiso D . . . . .
C24 C 0.9713(7) 0.2244(3) 0.6082(7) 0.041(3) 0.5000 Uiso D . . . . .
C25 C 1.047(6) 0.360(3) 0.652(4) 0.17(2) 0.3000 Uiso . . . . . .
C26 C 0.7644(7) 0.3777(3) 0.5022(6) 0.0417(17) 0.5000 Uiso D . . . . .
C27 C 0.8288(15) 0.4555(6) 0.5327(17) 0.093(10) 0.3000 Uiso D . . . . .
C50 C 0.5873(8) 0.3559(3) 0.4279(7) 0.0398(17) 0.5000 Uiso D . . . . .
C60 C 0.5126(10) 0.4203(3) 0.3858(8) 0.055(2) 0.5000 Uiso D . . . . .
C70 C 0.4024(8) 0.4010(4) 0.3292(7) 0.042(2) 0.5000 Uiso D . . . . .
C80 C 0.3593(8) 0.3240(4) 0.3101(7) 0.051(2) 0.5000 Uiso D . . . . .
C90 C 0.4457(7) 0.2607(4) 0.3540(6) 0.0423(18) 0.5000 Uiso D . . . . .
C100 C 0.4220(5) 0.1800(3) 0.3425(5) 0.0295(19) 0.5000 Uiso D . . . . .
C110 C 0.2840(9) 0.1619(4) 0.2909(8) 0.050(3) 0.5000 Uiso D . . . . .
C120 C 0.4368(10) 0.0118(5) 0.3166(8) 0.062(3) 0.5000 Uiso D . . . . .
C130 C 0.6421(7) 0.0294(3) 0.4456(6) 0.039(2) 0.5000 Uiso D . . . . .
C140 C 0.6545(7) -0.0486(3) 0.4500(6) 0.033(2) 0.5000 Uiso D . . . . .
C150 C 0.7696(7) -0.0753(3) 0.5097(6) 0.035(2) 0.5000 Uiso D . . . . .
C160 C 0.8631(6) -0.0223(3) 0.5620(5) 0.0270(18) 0.5000 Uiso D . . . . .
C170 C 0.8290(6) 0.0554(2) 0.5476(5) 0.0262(19) 0.5000 Uiso D . . . . .
C180 C 0.9194(6) 0.1152(2) 0.5925(5) 0.0248(18) 0.5000 Uiso D . . . . .
C190 C 1.0332(5) 0.0911(3) 0.6537(5) 0.0251(17) 0.5000 Uiso D . . . . .
C200 C 1.0662(7) 0.0142(4) 0.6708(6) 0.036(2) 0.5000 Uiso D . . . . .
C210 C 0.9812(7) -0.0414(3) 0.6233(6) 0.0286(18) 0.5000 Uiso D . . . . .
C220 C 1.1153(6) 0.1577(3) 0.6923(5) 0.0261(17) 0.5000 Uiso D . . . . .
C230 C 1.0787(6) 0.2310(3) 0.6711(5) 0.0299(19) 0.5000 Uiso D . . . . .
C240 C 0.9560(5) 0.2472(3) 0.6063(5) 0.0247(18) 0.5000 Uiso D . . . . .
C250 C 1.0153(8) 0.3750(5) 0.5710(8) 0.048(3) 0.5000 Uiso D . . . . .
C251 C 1.0635(11) 0.3457(8) 0.5722(16) 0.076(11) 0.2000 Uiso D . . . . .
C260 C 0.7099(8) 0.3761(3) 0.4907(6) 0.0417(17) 0.5000 Uiso D . . . . .
C270 C 0.7484(10) 0.4592(5) 0.5216(9) 0.062(3) 0.5000 Uiso D . . . . .
C271 C 0.872(5) 0.453(3) 0.496(3) 0.077(11) 0.2000 Uiso . . . . . .
N1 N 0.8026(4) 0.2085(2) 0.3758(3) 0.0306(8) 1.0000 Uiso . . . . . .
N2 N 0.6053(4) 0.2045(2) 0.5886(3) 0.0298(8) 1.0000 Uiso . . . . . .
N5 N 0.5839(10) 0.3014(6) 0.4258(7) 0.0354(14) 0.5000 Uiso . . . . . .
N6 N 0.5065(6) 0.1612(4) 0.3826(5) 0.0339(13) 0.5000 Uiso D . . . . .
N7 N 0.4966(6) 0.0857(3) 0.3716(4) 0.037(2) 0.5000 Uiso D . . . . .
N8 N 0.6958(7) 0.0842(3) 0.4764(6) 0.0290(10) 0.5000 Uiso D . . . . .
N9 N 0.8807(6) 0.1728(3) 0.5702(6) 0.0309(10) 0.5000 Uiso D . . . . .
N10 N 0.9414(6) 0.3026(3) 0.5867(5) 0.0410(14) 0.5000 Uiso D . . . . .
N11 N 0.8153(7) 0.3138(3) 0.5338(7) 0.0395(13) 0.5000 Uiso D . . . . .
N50 N 0.5569(10) 0.2814(5) 0.4110(7) 0.0354(14) 0.5000 Uiso . . . . . .
N60 N 0.5182(6) 0.1357(3) 0.3831(5) 0.0339(13) 0.5000 Uiso D . . . . .
N70 N 0.5234(5) 0.0597(3) 0.3858(4) 0.0365(19) 0.5000 Uiso D . . . . .
N80 N 0.7213(7) 0.0808(2) 0.4909(6) 0.0290(10) 0.5000 Uiso D . . . . .
N90 N 0.8814(6) 0.1885(3) 0.5741(6) 0.0309(10) 0.5000 Uiso D . . . . .
N100 N 0.9054(5) 0.3199(3) 0.5800(4) 0.0410(14) 0.5000 Uiso D . . . . .
N110 N 0.7821(7) 0.3183(3) 0.5199(6) 0.0395(13) 0.5000 Uiso D . . . . .
O1 O 0.2120(15) 0.2742(9) 0.4846(10) 0.109(5) 0.5000 Uiso . . . . . .
H141 H 0.5255 -0.0619 0.3844 0.0485 0.5000 Uiso . . . . . .
H151 H 0.7082 -0.1298 0.4751 0.0490 0.5000 Uiso . . . . . .
H1401 H 0.5901 -0.0821 0.4164 0.0383 0.5000 Uiso . . . . . .
H1201 H 0.3631 0.0408 0.2855 0.0766 0.5000 Uiso . . . . . .
H1202 H 0.4016 -0.0307 0.3473 0.0766 0.5000 Uiso . . . . . .
H1203 H 0.4836 -0.0092 0.2746 0.0766 0.5000 Uiso . . . . . .
H121 H 0.3388 0.0863 0.2654 0.1018 0.5000 Uiso . . . . . .
H122 H 0.4508 0.0318 0.2489 0.1018 0.5000 Uiso . . . . . .
H123 H 0.3587 0.0072 0.3141 0.1018 0.5000 Uiso . . . . . .
H1101 H 0.2394 0.2010 0.2643 0.0729 0.5000 Uiso . . . . . .
H1102 H 0.2392 0.1280 0.3238 0.0729 0.5000 Uiso . . . . . .
H1103 H 0.2971 0.1247 0.2358 0.0729 0.5000 Uiso . . . . . .
H111 H 0.2379 0.2498 0.2898 0.0963 0.5000 Uiso . . . . . .
H112 H 0.2287 0.1714 0.3375 0.0963 0.5000 Uiso . . . . . .
H113 H 0.2757 0.1748 0.2453 0.0963 0.5000 Uiso . . . . . .
H1501 H 0.7856 -0.1300 0.5153 0.0385 0.5000 Uiso . . . . . .
H211 H 0.9398 -0.1185 0.5909 0.0722 0.5000 Uiso . . . . . .
H2101 H 1.0065 -0.0944 0.6335 0.0348 0.5000 Uiso . . . . . .
H2001 H 1.1466 -0.0010 0.7128 0.0422 0.5000 Uiso . . . . . .
H221 H 1.1889 0.1037 0.7234 0.0687 0.5000 Uiso . . . . . .
H2201 H 1.1986 0.1513 0.7361 0.0329 0.5000 Uiso . . . . . .
H2301 H 1.1328 0.2737 0.6980 0.0392 0.5000 Uiso . . . . . .
H231 H 1.1567 0.2319 0.6971 0.0705 0.5000 Uiso . . . . . .
H201 H 1.1032 -0.0415 0.6777 0.0580 0.5000 Uiso . . . . . .
H2501 H 0.9869 0.4250 0.5537 0.0622 0.5000 Uiso . . . . . .
H2502 H 1.0797 0.3792 0.6306 0.0622 0.5000 Uiso . . . . . .
H2503 H 1.0689 0.3564 0.5288 0.0622 0.5000 Uiso . . . . . .
H2511 H 1.0523 0.3972 0.5610 0.0975 0.2000 Uiso . . . . . .
H2512 H 1.1358 0.3420 0.6321 0.0975 0.2000 Uiso . . . . . .
H2513 H 1.1069 0.3213 0.5287 0.0975 0.2000 Uiso . . . . . .
H2701 H 0.6705 0.4935 0.4822 0.0852 0.5000 Uiso . . . . . .
H2702 H 0.7459 0.4695 0.5794 0.0852 0.5000 Uiso . . . . . .
H2703 H 0.8221 0.4773 0.5004 0.0852 0.5000 Uiso . . . . . .
H271 H 0.7615 0.4971 0.4990 0.0868 0.3000 Uiso . . . . . .
H272 H 0.8234 0.4670 0.5965 0.0868 0.3000 Uiso . . . . . .
H273 H 0.9057 0.4654 0.5204 0.0868 0.3000 Uiso . . . . . .
H2711 H 0.8143 0.4995 0.4821 0.1064 0.2000 Uiso . . . . . .
H2712 H 0.9096 0.4668 0.5682 0.1064 0.2000 Uiso . . . . . .
H2713 H 0.9314 0.4466 0.4711 0.1064 0.2000 Uiso . . . . . .
H801 H 0.2738 0.3162 0.2656 0.0649 0.5000 Uiso . . . . . .
H701 H 0.3495 0.4416 0.3039 0.0571 0.5000 Uiso . . . . . .
H71 H 0.4045 0.4781 0.3509 0.1218 0.5000 Uiso . . . . . .
H61 H 0.6131 0.4927 0.4342 0.0648 0.5000 Uiso . . . . . .
H601 H 0.5415 0.4753 0.3994 0.0648 0.5000 Uiso . . . . . .
H81 H 0.2961 0.3614 0.3045 0.0649 0.5000 Uiso . . . . . .
H251 H 1.0220 0.4098 0.6378 0.1916 0.3000 Uiso . . . . . .
H252 H 1.1310 0.3471 0.6459 0.1916 0.3000 Uiso . . . . . .
H253 H 1.0370 0.3486 0.7148 0.1916 0.3000 Uiso . . . . . .

_refine_ls_extinction_method     None

loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 . C2 3_554 1.861(4) yes
Ni1 . C1 . 1.858(4) yes
Ni1 . C3 . 1.896(6) yes
Ni1 . C30 . 1.850(6) yes
Ni1 . C4 . 1.855(6) yes
Ni1 . C40 . 1.885(6) yes
Ni2 . N1 . 2.046(4) yes
Ni2 . N2 . 2.063(4) yes
Ni2 . N5 . 2.172(10) yes
Ni2 . N6 . 2.393(5) yes
Ni2 . N8 . 2.098(4) yes
Ni2 . N9 . 2.061(5) yes
Ni2 . N11 . 2.261(5) yes
Ni2 . N50 . 2.147(10) yes
Ni2 . N60 . 2.485(5) yes
Ni2 . N80 . 2.161(4) yes
Ni2 . N90 . 2.038(4) yes
Ni2 . N110 . 2.163(5) yes
C1 . N1 . 1.143(6) yes
C2 . N2 . 1.134(6) yes
C3 . N3 . 1.171(8) yes
C30 . N30 . 1.150(8) yes
C4 . N4 . 1.146(8) yes
C40 . N40 . 1.149(8) yes
C5 . C6 . 1.421(8) yes
C5 . C26 . 1.453(7) yes
C5 . N5 . 1.296(11) yes
C6 . C7 . 1.304(8) yes
C6 . H61 . 1.033 no
C7 . C8 . 1.412(8) yes
C7 . H71 . 0.931 no
C8 . C9 . 1.483(8) yes
C8 . H81 . 0.987 no
C9 . C10 . 1.421(7) yes
C9 . N5 . 1.341(11) yes
C10 . C11 . 1.494(9) yes
C10 . N6 . 1.258(7) yes
C11 . H111 . 0.891 no
C11 . H112 . 0.899 no
C11 . H113 . 1.142 no
C12 . N7 . 1.468(9) yes
C12 . H121 . 0.960 no
C12 . H122 . 0.923 no
C12 . H123 . 0.998 no
C13 . C14 . 1.369(6) yes
C13 . N7 . 1.453(6) yes
C13 . N8 . 1.275(6) yes
C14 . C15 . 1.409(7) yes
C14 . H141 . 0.959 no
C15 . C16 . 1.423(6) yes
C15 . H151 . 0.972 no
C16 . C17 . 1.399(6) yes
C16 . C21 . 1.403(7) yes
C17 . C18 . 1.450(6) yes
C17 . N8 . 1.327(6) yes
C18 . C19 . 1.399(6) yes
C18 . N9 . 1.341(6) yes
C19 . C20 . 1.378(7) yes
C19 . C22 . 1.492(7) yes
C20 . C21 . 1.392(7) yes
C20 . H201 . 0.965 no
C21 . C210 . 0.780(8) yes
C21 . H211 . 0.969 no
C22 . C23 . 1.355(7) yes
C22 . H221 . 0.974 no
C23 . C24 . 1.442(7) yes
C23 . H231 . 0.965 no
C24 . N9 . 1.333(6) yes
C24 . N10 . 1.419(7) yes
C24 . N100 . 1.814(8) yes
C25 . N10 . 1.64(6) yes
C25 . H251 . 0.924 no
C25 . H252 . 0.910 no
C25 . H253 . 0.984 no
C26 . C27 . 1.535(10) yes
C26 . C271 . 1.73(5) yes
C26 . N11 . 1.278(7) yes
C27 . H271 . 1.054 no
C27 . H272 . 0.986 no
C27 . H273 . 0.866 no
C50 . C60 . 1.428(7) yes
C50 . C260 . 1.447(7) yes
C50 . N50 . 1.348(11) yes
C60 . C70 . 1.307(7) yes
C60 . H601 . 1.011 no
C70 . C80 . 1.423(7) yes
C70 . H701 . 0.925 no
C80 . C90 . 1.480(7) yes
C80 . H801 . 0.993 no
C90 . C100 . 1.431(7) yes
C90 . N50 . 1.325(11) yes
C100 . C110 . 1.499(8) yes
C100 . N60 . 1.300(7) yes
C110 . H1101 . 0.870 no
C110 . H1102 . 0.946 no
C110 . H1103 . 1.077 no
C120 . N70 . 1.474(8) yes
C120 . H1201 . 0.947 no
C120 . H1202 . 0.980 no
C120 . H1203 . 0.940 no
C130 . C140 . 1.365(6) yes
C130 . N70 . 1.452(6) yes
C130 . N80 . 1.302(6) yes
C140 . C150 . 1.404(6) yes
C140 . H1401 . 0.945 no
C150 . C160 . 1.440(6) yes
C150 . H1501 . 0.967 no
C160 . C170 . 1.405(5) yes
C160 . C210 . 1.399(6) yes
C170 . C180 . 1.462(5) yes
C170 . N80 . 1.321(6) yes
C180 . C190 . 1.391(5) yes
C180 . N90 . 1.348(6) yes
C190 . C200 . 1.393(6) yes
C190 . C220 . 1.480(6) yes
C200 . C210 . 1.395(6) yes
C200 . H2001 . 0.964 no
C210 . H2101 . 0.962 no
C220 . C230 . 1.351(6) yes
C220 . H2201 . 0.969 no
C230 . C240 . 1.448(6) yes
C230 . H2301 . 0.965 no
C240 . N90 . 1.307(6) yes
C240 . N100 . 1.394(6) yes
C250 . N100 . 1.511(8) yes
C250 . H2501 . 0.937 no
C250 . H2502 . 0.994 no
C250 . H2503 . 0.975 no
C251 . N10 . 1.517(10) yes
C251 . H2511 . 0.915 no
C251 . H2512 . 1.038 no
C251 . H2513 . 0.960 no
C260 . C270 . 1.546(8) yes
C260 . N110 . 1.272(7) yes
C270 . H2701 . 1.072 no
C270 . H2702 . 0.885 no
C270 . H2703 . 0.935 no
C271 . H2711 . 1.001 no
C271 . H2712 . 1.099 no
C271 . H2713 . 0.785 no
N6 . N7 . 1.328(7) yes
N10 . N11 . 1.383(7) yes
N60 . N70 . 1.324(7) yes
N100 . N110 . 1.392(7) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 3_554 Ni1 . C1 . 178.4(2) yes
C2 3_554 Ni1 . C3 . 85.0(2) yes
C1 . Ni1 . C3 . 93.7(2) yes
C2 3_554 Ni1 . C30 . 88.2(2) yes
C1 . Ni1 . C30 . 90.3(2) yes
C3 . Ni1 . C30 . 16.85(6) yes
C2 3_554 Ni1 . C4 . 94.4(2) yes
C1 . Ni1 . C4 . 87.0(2) yes
C3 . Ni1 . C4 . 174.8(3) yes
C30 . Ni1 . C4 . 168.3(3) yes
C2 3_554 Ni1 . C40 . 91.8(2) yes
C1 . Ni1 . C40 . 89.7(2) yes
C3 . Ni1 . C40 . 162.3(3) yes
C30 . Ni1 . C40 . 179.2(3) yes
C4 . Ni1 . C40 . 12.52(4) yes
N1 . Ni2 . N2 . 177.64(16) yes
N1 . Ni2 . N5 . 90.2(3) yes
N2 . Ni2 . N5 . 87.5(3) yes
N1 . Ni2 . N6 . 91.0(2) yes
N2 . Ni2 . N6 . 88.5(2) yes
N5 . Ni2 . N6 . 69.5(3) yes
N1 . Ni2 . N8 . 91.7(3) yes
N2 . Ni2 . N8 . 90.3(3) yes
N5 . Ni2 . N8 . 137.7(3) yes
N6 . Ni2 . N8 . 68.2(2) yes
N1 . Ni2 . N9 . 90.2(3) yes
N2 . Ni2 . N9 . 91.4(3) yes
N5 . Ni2 . N9 . 144.3(3) yes
N6 . Ni2 . N9 . 146.2(2) yes
N8 . Ni2 . N9 . 77.9(2) yes
N1 . Ni2 . N11 . 86.9(3) yes
N2 . Ni2 . N11 . 92.0(3) yes
N5 . Ni2 . N11 . 71.4(3) yes
N6 . Ni2 . N11 . 140.9(2) yes
N8 . Ni2 . N11 . 150.8(2) yes
N1 . Ni2 . N50 . 90.2(3) yes
N2 . Ni2 . N50 . 87.6(3) yes
N5 . Ni2 . N50 . 12.5(3) yes
N6 . Ni2 . N50 . 57.0(3) yes
N8 . Ni2 . N50 . 125.2(3) yes
N1 . Ni2 . N60 . 89.7(2) yes
N2 . Ni2 . N60 . 90.3(2) yes
N5 . Ni2 . N60 . 80.1(3) yes
N6 . Ni2 . N60 . 10.63(19) yes
N8 . Ni2 . N60 . 57.7(2) yes
N1 . Ni2 . N80 . 92.2(3) yes
N2 . Ni2 . N80 . 90.0(3) yes
N5 . Ni2 . N80 . 145.8(3) yes
N6 . Ni2 . N80 . 76.4(2) yes
N8 . Ni2 . N80 . 8.1(2) yes
N1 . Ni2 . N90 . 91.2(3) yes
N2 . Ni2 . N90 . 90.2(3) yes
N5 . Ni2 . N90 . 136.5(3) yes
N6 . Ni2 . N90 . 153.8(2) yes
N8 . Ni2 . N90 . 85.6(2) yes
N1 . Ni2 . N110 . 87.7(3) yes
N2 . Ni2 . N110 . 90.8(3) yes
N5 . Ni2 . N110 . 62.2(3) yes
N6 . Ni2 . N110 . 131.7(2) yes
N8 . Ni2 . N110 . 160.0(2) yes
N9 . Ni2 . N11 . 72.9(2) yes
N9 . Ni2 . N50 . 156.8(3) yes
N11 . Ni2 . N50 . 83.9(3) yes
N9 . Ni2 . N60 . 135.7(2) yes
N11 . Ni2 . N60 . 151.3(2) yes
N50 . Ni2 . N60 . 67.5(3) yes
N9 . Ni2 . N80 . 69.8(2) yes
N11 . Ni2 . N80 . 142.7(2) yes
N50 . Ni2 . N80 . 133.3(3) yes
N60 . Ni2 . N80 . 65.88(19) yes
N9 . Ni2 . N90 . 7.8(3) yes
N11 . Ni2 . N90 . 65.3(2) yes
N50 . Ni2 . N90 . 149.0(3) yes
N60 . Ni2 . N90 . 143.4(2) yes
N80 . Ni2 . N90 . 77.5(2) yes
N9 . Ni2 . N110 . 82.1(2) yes
N11 . Ni2 . N110 . 9.2(2) yes
N50 . Ni2 . N110 . 74.7(3) yes
N60 . Ni2 . N110 . 142.2(2) yes
N80 . Ni2 . N110 . 151.9(2) yes
N90 . Ni2 . N110 . 74.4(2) yes
Ni1 . C1 . N1 . 177.3(4) yes
Ni1 3_455 C2 . N2 . 176.7(4) yes
Ni1 . C3 . N3 . 169.5(7) yes
Ni1 . C30 . N30 . 177.9(8) yes
Ni1 . C4 . N4 . 176.5(6) yes
Ni1 . C40 . N40 . 178.4(6) yes
C6 . C5 . C26 . 114.27(9) yes
C6 . C5 . N5 . 126.5(6) yes
C26 . C5 . N5 . 119.2(6) yes
C5 . C6 . C7 . 113.30(9) yes
C5 . C6 . H61 . 122.2 no
C7 . C6 . H61 . 124.5 no
C6 . C7 . C8 . 124.33(9) yes
C6 . C7 . H71 . 113.2 no
C8 . C7 . H71 . 122.4 no
C7 . C8 . C9 . 118.67(9) yes
C7 . C8 . H81 . 116.4 no
C9 . C8 . H81 . 124.9 no
C8 . C9 . C10 . 127.45(9) yes
C8 . C9 . N5 . 114.3(5) yes
C10 . C9 . N5 . 118.2(6) yes
C9 . C10 . C11 . 112.86(9) yes
C9 . C10 . N6 . 115.81(8) yes
C11 . C10 . N6 . 131.25(9) yes
C10 . C11 . H111 . 114.8 no
C10 . C11 . H112 . 116.1 no
H111 . C11 . H112 . 120.2 no
C10 . C11 . H113 . 103.3 no
H111 . C11 . H113 . 98.7 no
H112 . C11 . H113 . 98.2 no
N7 . C12 . H121 . 110.6 no
N7 . C12 . H122 . 113.5 no
H121 . C12 . H122 . 110.9 no
N7 . C12 . H123 . 109.0 no
H121 . C12 . H123 . 104.8 no
H122 . C12 . H123 . 107.6 no
C14 . C13 . N7 . 116.87(8) yes
C14 . C13 . N8 . 128.16(7) yes
N7 . C13 . N8 . 114.96(8) yes
C13 . C14 . C15 . 114.76(8) yes
C13 . C14 . H141 . 122.7 no
C15 . C14 . H141 . 122.5 no
C14 . C15 . C16 . 120.53(8) yes
C14 . C15 . H151 . 118.4 no
C16 . C15 . H151 . 121.1 no
C15 . C16 . C17 . 114.71(7) yes
C15 . C16 . C21 . 126.33(8) yes
C17 . C16 . C21 . 118.96(7) yes
C16 . C17 . C18 . 120.20(7) yes
C16 . C17 . N8 . 124.88(7) yes
C18 . C17 . N8 . 114.91(7) yes
C17 . C18 . C19 . 116.98(8) yes
C17 . C18 . N9 . 116.91(8) yes
C19 . C18 . N9 . 126.02(8) yes
C18 . C19 . C20 . 123.45(8) yes
C18 . C19 . C22 . 110.62(8) yes
C20 . C19 . C22 . 125.91(8) yes
C19 . C20 . C21 . 118.17(9) yes
C19 . C20 . H201 . 122.5 no
C21 . C20 . H201 . 119.3 no
C16 . C21 . C20 . 122.12(9) yes
C16 . C21 . C210 . 126.6(6) yes
C16 . C21 . H211 . 119.6 no
C20 . C21 . H211 . 118.3 no
C210 . C21 . H211 . 112.9 no
C19 . C22 . C23 . 122.87(9) yes
C19 . C22 . H221 . 121.0 no
C23 . C22 . H221 . 116.1 no
C22 . C23 . C24 . 120.14(9) yes
C22 . C23 . H231 . 120.9 no
C24 . C23 . H231 . 118.9 no
C23 . C24 . N9 . 117.20(7) yes
C23 . C24 . N10 . 125.91(8) yes
N9 . C24 . N10 . 116.88(8) yes
C23 . C24 . N100 . 133.6(3) yes
N9 . C24 . N100 . 109.0(3) yes
N10 . C25 . H251 . 108.6 no
N10 . C25 . H252 . 108.7 no
H251 . C25 . H252 . 115.5 no
N10 . C25 . H253 . 104.9 no
H251 . C25 . H253 . 108.7 no
H252 . C25 . H253 . 109.8 no
C5 . C26 . C27 . 123.55(9) yes
C5 . C26 . C271 . 124.6(16) yes
C5 . C26 . N11 . 113.14(9) yes
C27 . C26 . N11 . 122.85(9) yes
C271 . C26 . N11 . 117.6(15) yes
C26 . C27 . H271 . 105.5 no
C26 . C27 . H272 . 111.0 no
H271 . C27 . H272 . 99.0 no
C26 . C27 . H273 . 118.1 no
H271 . C27 . H273 . 107.4 no
H272 . C27 . H273 . 113.7 no
C60 . C50 . C260 . 114.21(9) yes
C60 . C50 . N50 . 126.3(5) yes
C260 . C50 . N50 . 119.4(5) yes
C50 . C60 . C70 . 113.32(9) yes
C50 . C60 . H601 . 123.1 no
C70 . C60 . H601 . 123.6 no
C60 . C70 . C80 . 124.34(9) yes
C60 . C70 . H701 . 115.0 no
C80 . C70 . H701 . 120.6 no
C70 . C80 . C90 . 118.72(9) yes
C70 . C80 . H801 . 117.2 no
C90 . C80 . H801 . 124.0 no
C80 . C90 . C100 . 127.43(9) yes
C80 . C90 . N50 . 116.1(5) yes
C100 . C90 . N50 . 116.5(5) yes
C90 . C100 . C110 . 112.79(9) yes
C90 . C100 . N60 . 115.73(8) yes
C110 . C100 . N60 . 131.27(9) yes
C100 . C110 . H1101 . 114.9 no
C100 . C110 . H1102 . 112.1 no
H1101 . C110 . H1102 . 117.3 no
C100 . C110 . H1103 . 105.2 no
H1101 . C110 . H1103 . 105.1 no
H1102 . C110 . H1103 . 99.9 no
N70 . C120 . H1201 . 110.2 no
N70 . C120 . H1202 . 109.2 no
H1201 . C120 . H1202 . 107.2 no
N70 . C120 . H1203 . 111.7 no
H1201 . C120 . H1203 . 110.6 no
H1202 . C120 . H1203 . 107.8 no
C140 . C130 . N70 . 116.79(8) yes
C140 . C130 . N80 . 128.17(8) yes
N70 . C130 . N80 . 115.00(8) yes
C130 . C140 . C150 . 114.81(8) yes
C130 . C140 . H1401 . 122.8 no
C150 . C140 . H1401 . 122.3 no
C140 . C150 . C160 . 120.62(8) yes
C140 . C150 . H1501 . 119.2 no
C160 . C150 . H1501 . 120.2 no
C150 . C160 . C170 . 114.75(7) yes
C150 . C160 . C210 . 126.25(8) yes
C170 . C160 . C210 . 119.00(7) yes
C160 . C170 . C180 . 120.16(8) yes
C160 . C170 . N80 . 124.77(8) yes
C180 . C170 . N80 . 114.96(8) yes
C170 . C180 . C190 . 116.92(7) yes
C170 . C180 . N90 . 116.94(7) yes
C190 . C180 . N90 . 126.06(8) yes
C180 . C190 . C200 . 123.41(7) yes
C180 . C190 . C220 . 110.62(8) yes
C200 . C190 . C220 . 125.89(8) yes
C190 . C200 . C210 . 118.21(8) yes
C190 . C200 . H2001 . 121.8 no
C210 . C200 . H2001 . 120.0 no
C160 . C210 . C200 . 122.16(8) yes
C200 . C210 . C21 . 164.2(9) yes
C160 . C210 . H2101 . 120.0 no
C200 . C210 . H2101 . 117.8 no
C190 . C220 . C230 . 122.83(9) yes
C190 . C220 . H2201 . 121.6 no
C230 . C220 . H2201 . 115.6 no
C220 . C230 . C240 . 120.13(9) yes
C220 . C230 . H2301 . 121.6 no
C240 . C230 . H2301 . 118.3 no
C230 . C240 . N90 . 117.12(8) yes
C230 . C240 . N100 . 125.86(8) yes
N90 . C240 . N100 . 116.85(8) yes
N100 . C250 . H2501 . 114.8 no
N100 . C250 . H2502 . 109.7 no
H2501 . C250 . H2502 . 106.9 no
N100 . C250 . H2503 . 112.3 no
H2501 . C250 . H2503 . 108.5 no
H2502 . C250 . H2503 . 104.0 no
N10 . C251 . H2511 . 115.8 no
N10 . C251 . H2512 . 108.1 no
H2511 . C251 . H2512 . 105.0 no
N10 . C251 . H2513 . 113.1 no
H2511 . C251 . H2513 . 111.7 no
H2512 . C251 . H2513 . 101.8 no
C50 . C260 . C270 . 123.68(8) yes
C50 . C260 . N110 . 113.37(8) yes
C270 . C260 . N110 . 122.93(8) yes
C260 . C270 . H2701 . 104.1 no
C260 . C270 . H2702 . 115.0 no
H2701 . C270 . H2702 . 104.5 no
C260 . C270 . H2703 . 112.9 no
H2701 . C270 . H2703 . 101.0 no
H2702 . C270 . H2703 . 116.9 no
C26 . C271 . H2711 . 105.8 no
C26 . C271 . H2712 . 102.3 no
H2711 . C271 . H2712 . 95.1 no
C26 . C271 . H2713 . 119.6 no
H2711 . C271 . H2713 . 120.1 no
H2712 . C271 . H2713 . 109.7 no
Ni2 . N1 . C1 . 167.4(4) yes
Ni2 . N2 . C2 . 167.9(4) yes
Ni2 . N5 . C9 . 119.6(7) yes
Ni2 . N5 . C5 . 117.6(7) yes
C9 . N5 . C5 . 122.8(9) yes
Ni2 . N6 . C10 . 115.7(3) yes
Ni2 . N6 . N7 . 114.97(19) yes
C10 . N6 . N7 . 128.87(9) yes
C12 . N7 . C13 . 121.99(10) yes
C12 . N7 . N6 . 121.90(10) yes
C13 . N7 . N6 . 113.95(9) yes
C17 . N8 . Ni2 . 115.30(19) yes
C17 . N8 . C13 . 116.95(8) yes
Ni2 . N8 . C13 . 127.7(2) yes
C18 . N9 . C24 . 122.96(9) yes
C18 . N9 . Ni2 . 114.9(2) yes
C24 . N9 . Ni2 . 121.9(2) yes
C251 . N10 . C25 . 47(2) yes
C251 . N10 . C24 . 111.16(10) yes
C25 . N10 . C24 . 111(2) yes
C251 . N10 . N11 . 123.58(10) yes
C25 . N10 . N11 . 133(2) yes
C24 . N10 . N11 . 113.40(9) yes
Ni2 . N11 . N10 . 114.4(2) yes
Ni2 . N11 . C26 . 118.3(2) yes
N10 . N11 . C26 . 126.56(9) yes
C50 . N50 . Ni2 . 113.3(6) yes
C50 . N50 . C90 . 121.1(9) yes
Ni2 . N50 . C90 . 125.5(7) yes
Ni2 . N60 . C100 . 114.4(2) yes
Ni2 . N60 . N70 . 116.21(18) yes
C100 . N60 . N70 . 129.04(9) yes
C120 . N70 . C130 . 122.04(10) yes
C120 . N70 . N60 . 121.99(10) yes
C130 . N70 . N60 . 113.98(9) yes
Ni2 . N80 . C170 . 114.27(18) yes
Ni2 . N80 . C130 . 128.81(19) yes
C170 . N80 . C130 . 116.87(8) yes
C180 . N90 . C240 . 122.94(8) yes
C180 . N90 . Ni2 . 116.3(2) yes
C240 . N90 . Ni2 . 120.6(2) yes
C250 . N100 . C240 . 111.17(10) yes
C250 . N100 . C24 . 110.7(4) yes
C250 . N100 . N110 . 123.55(10) yes
C240 . N100 . N110 . 113.52(9) yes
C24 . N100 . N110 . 112.2(3) yes
N100 . N110 . Ni2 . 114.5(2) yes
N100 . N110 . C260 . 126.37(9) yes
Ni2 . N110 . C260 . 119.0(2) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C120 . H1201 . C110 . 137 0.95 2.27 3.033(14) yes
C120 . H1203 . N4 4_645 154 0.94 2.21 3.080(14) yes
C120 . H1203 . N40 4_645 140 0.94 2.39 3.170(14) yes
C12 . H121 . C11 . 132 0.96 2.34 3.067(14) yes
C12 . H121 . C110 . 137 0.96 1.51 2.311(14) yes
C150 . H1501 . O1 2_656 170 0.97 2.51 3.470(14) yes
C250 . H2501 . C27 . 125 0.94 1.68 2.348(14) yes
C250 . H2501 . C270 . 121 0.94 2.47 3.062(14) yes
C250 . H2501 . C271 . 132 0.94 1.40 2.141(14) yes
C250 . H2503 . O1 1_655 153 0.98 2.25 3.151(14) yes
C251 . H2511 . C27 . 121 0.91 2.47 3.039(14) yes
C251 . H2511 . C271 . 126 0.91 2.14 2.780(14) yes
C25 . H2512 . N30 3_555 142 1.06 2.53 3.428(14) yes
C251 . H2513 . O1 1_655 162 0.96 1.60 2.535(14) yes
C270 . H2701 . N30 4_655 141 1.07 2.59 3.494(14) yes
C271 . H2713 . N4 . 143 0.79 2.40 3.058(14) yes
C271 . H2713 . N40 . 155 0.79 2.56 3.287(14) yes
C6 . H61 . N3 4_655 125 1.03 2.15 2.867(14) yes
C6 . H61 . N30 4_655 141 1.03 2.28 3.149(14) yes
C60 . H601 . N3 4_655 153 1.01 2.23 3.168(14) yes
C25 . H251 . C27 . 128 0.92 2.40 3.055(14) yes
C25 . H251 . C271 . 125 0.92 2.46 3.093(14) yes
C25 . H253 . C100 3_555 158 0.98 2.49 3.426(14) yes
C25 . H253 . N6 3_555 173 0.98 2.59 3.570(14) yes
C25 . H253 . N60 3_555 163 0.98 2.57 3.523(14) yes


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cpd4
_database_code_depnum_ccdc_archive 'CCDC 1957998'
loop_
_audit_author_name
_audit_author_address
'Carine Duhayon'
;LCC CNRS
France
;
_audit_update_record             
;
2019-10-08 deposited with the CCDC.	2019-12-16 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          SQUEEZE
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   28.0208(17)
_cell_length_b                   20.6609(10)
_cell_length_c                   20.2346(11)
_cell_angle_alpha                90
_cell_angle_beta                 96.273(2)
_cell_angle_gamma                90
_cell_volume                     11644.4(11)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c '
_symmetry_space_group_name_Hall  '-C 2yc '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
x,-y,z+1/2
-x,y,-z+1/2
x+1/2,-y+1/2,z+1/2
-x+1/2,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mo -1.6832 0.6857 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584
4.3875 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cr 0.3209 0.6236 10.6406 6.1038 7.3537 0.3920 3.3240 20.2626 1.4922 98.7399
1.1832 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            8

# Given Formula = C51 H47 Cl1 Cr1 N15 Ni1 O7 
# Dc =      1.29 Fooo =   4664.00 Mu =      6.16 M =   1128.19
# Found Formula = C51 H47 Cl1 Cr1 N15 Ni1 O7 
# Dc =      1.29 FOOO =   4664.00 Mu =      6.16 M =   1128.19

_chemical_formula_sum            'C51 H47 Cl1 Cr1 N15 Ni1 O7'
_chemical_formula_moiety         'C48 H40 Cr N14 Ni O2, Cl O4, C3 H7 N O '
_chemical_compound_source        ?
_chemical_formula_weight         1128.19


_cell_measurement_reflns_used    9701
_cell_measurement_theta_min      2
_cell_measurement_theta_max      27
_cell_measurement_temperature    100

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.060
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_max          0.180

_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             4664
_exptl_absorpt_coefficient_mu    0.616

# Sheldrick geometric approximatio 0.90 0.96 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_T_max  0.96
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      100
_diffrn_reflns_number            148165
_reflns_number_total             13403
_diffrn_reflns_av_R_equivalents  0.074
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 13403 
# Theoretical number of reflections is about 26935 


_diffrn_reflns_theta_min         1.227
_diffrn_reflns_theta_max         27.568
_diffrn_measured_fraction_theta_max 0.994

_diffrn_reflns_theta_full        27.017
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       26
_reflns_limit_h_min              -36
_reflns_limit_h_max              36
_reflns_limit_k_min              0
_reflns_limit_k_max              26
_reflns_limit_l_min              0
_reflns_limit_l_max              26


_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.27
_refine_diff_density_max         1.44


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns         9260
_refine_ls_number_restraints     0
_refine_ls_number_parameters     676
_oxford_refine_ls_R_factor_ref   0.0692
_refine_ls_wR_factor_ref         0.0728
_refine_ls_goodness_of_fit_ref   1.0417
_refine_ls_shift/su_max          0.0018655
_refine_ls_shift/su_mean         0.0000409


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        13375
_refine_ls_R_factor_all          0.0962
_refine_ls_wR_factor_all         0.1180

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                10099
_refine_ls_R_factor_gt           0.0740
_refine_ls_wR_factor_gt          0.0767

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.376 0.409 0.130 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C33 C 0.11615(19) 0.5538(3) 0.5841(3) 0.0529 1.0000 Uani . . . . . .
C34 C 0.15081(15) 0.4439(2) 0.56907(17) 0.0321 1.0000 Uani . . . . . .
C35 C 0.10560(18) 0.4158(3) 0.5521(2) 0.0475 1.0000 Uani . . . . . .
C36 C 0.10204(17) 0.3500(3) 0.5468(2) 0.0453 1.0000 Uani . . . . . .
C37 C 0.14273(15) 0.3106(2) 0.55730(18) 0.0340 1.0000 Uani . . . . . .
C38 C 0.18635(14) 0.34310(18) 0.57207(16) 0.0277 1.0000 Uani . . . . . .
C39 C 0.23006(13) 0.30671(16) 0.58141(15) 0.0219 1.0000 Uani . . . . . .
C40 C 0.23012(16) 0.23910(17) 0.57686(16) 0.0299 1.0000 Uani . . . . . .
C41 C 0.18546(17) 0.20688(19) 0.56324(18) 0.0369 1.0000 Uani . . . . . .
C42 C 0.14376(16) 0.2415(2) 0.55332(19) 0.0375 1.0000 Uani . . . . . .
C43 C 0.27598(16) 0.20956(18) 0.58546(17) 0.0310 1.0000 Uani . . . . . .
C44 C 0.31673(16) 0.24547(17) 0.59680(17) 0.0304 1.0000 Uani . . . . . .
C45 C 0.31297(14) 0.31421(17) 0.60097(16) 0.0262 1.0000 Uani . . . . . .
C46 C 0.39881(18) 0.3316(2) 0.6409(3) 0.0482 1.0000 Uani . . . . . .
C47 C 0.36955(16) 0.4684(2) 0.61052(19) 0.0347 1.0000 Uani . . . . . .
C48 C 0.42138(19) 0.4676(3) 0.6004(3) 0.0542 1.0000 Uani . . . . . .
C49 C 0.1626(3) 0.3234(4) 0.7354(3) 0.0338 0.6000 Uani . . . . . .
C50 C 0.0740(4) 0.3210(6) 0.7178(5) 0.0726 0.6000 Uani . . . . . .
C51 C 0.1494(7) 0.3468(8) 0.7321(8) 0.0613 0.4000 Uani . . . . . .
C52 C 0.0646(7) 0.3741(11) 0.7186(10) 0.0937 0.4000 Uani . . . . . .
C53 C 0.1143(5) 0.4204(6) 0.7175(5) 0.0566 0.6000 Uani . . . . . .
C54 C 0.1287(6) 0.4502(8) 0.7253(7) 0.0556 0.4000 Uani . . . . . .
N10 N 0.15724(13) 0.51100(17) 0.57635(16) 0.0363 1.0000 Uani . . . . . .
N11 N 0.19031(12) 0.40809(15) 0.57828(13) 0.0271 1.0000 Uani . . . . . .
N12 N 0.27083(11) 0.34182(13) 0.59356(13) 0.0230 1.0000 Uani . . . . . .
N13 N 0.35215(12) 0.35557(15) 0.60992(15) 0.0271 1.0000 Uani . . . . . .
N14 N 0.34022(12) 0.42016(15) 0.61161(14) 0.0278 1.0000 Uani . . . . . .
N15 N 0.1187(3) 0.3583(4) 0.7223(3) 0.0479 0.6000 Uani . . . . . .
N16 N 0.1177(5) 0.3944(8) 0.7250(7) 0.0596 0.4000 Uani . . . . . .
O1 O 0.19526(10) 0.54002(12) 0.35728(11) 0.0274 1.0000 Uani . . . . . .
O2 O 0.21620(9) 0.43081(11) 0.30705(11) 0.0248 1.0000 Uani . . . . . .
O3 O 0.0468(2) 0.1359(2) 0.5112(3) 0.1062 1.0000 Uani . . . . . .
O4 O -0.0177(3) 0.1998(4) 0.4784(5) 0.1683 1.0000 Uani . . . . . .
O5 O 0.02775(16) 0.2165(2) 0.5794(3) 0.1000 1.0000 Uani . . . . . .
O6 O -0.0207(3) 0.1279(4) 0.5598(4) 0.1557 1.0000 Uani . . . . . .
O7 O 0.0812(3) 0.4545(5) 0.7068(4) 0.0819 0.6000 Uani . . . . . .
O8 O 0.0995(5) 0.4947(7) 0.7224(6) 0.0795 0.4000 Uani . . . . . .
N1 N 0.26490(12) 0.44916(14) 0.49654(14) 0.0263 1.0000 Uani . . . . . .
N2 N 0.26198(12) 0.44406(14) 0.69956(14) 0.0286 1.0000 Uani . . . . . .
N3 N 0.34061(12) 0.52395(15) 0.37393(15) 0.0292 1.0000 Uani . . . . . .
N4 N 0.27186(12) 0.59561(14) 0.39713(14) 0.0270 1.0000 Uani . . . . . .
N5 N 0.23128(13) 0.62966(14) 0.40891(14) 0.0308 1.0000 Uani . . . . . .
N6 N 0.28233(12) 0.37107(14) 0.28678(14) 0.0272 1.0000 Uani . . . . . .
N7 N 0.30559(12) 0.42367(14) 0.31765(13) 0.0257 1.0000 Uani . . . . . .
N8 N 0.29746(13) 0.53290(15) 0.60646(14) 0.0295 1.0000 Uani . . . . . .
N9 N 0.20329(13) 0.52906(15) 0.59113(15) 0.0318 1.0000 Uani . . . . . .
C1 C 0.26167(12) 0.46312(14) 0.44109(15) 0.0179 1.0000 Uani . . . . . .
C2 C 0.26044(13) 0.45894(15) 0.75384(15) 0.0198 1.0000 Uani . . . . . .
C3 C 0.37337(15) 0.4802(2) 0.36180(19) 0.0340 1.0000 Uani . . . . . .
C4 C 0.42140(18) 0.4885(3) 0.3828(3) 0.0522 1.0000 Uani . . . . . .
C5 C 0.4354(2) 0.5447(3) 0.4177(3) 0.0610 1.0000 Uani . . . . . .
C6 C 0.40097(19) 0.5901(2) 0.4307(3) 0.0495 1.0000 Uani . . . . . .
C7 C 0.35383(16) 0.57759(18) 0.40741(18) 0.0325 1.0000 Uani . . . . . .
C8 C 0.31284(16) 0.61932(17) 0.41957(17) 0.0303 1.0000 Uani . . . . . .
C9 C 0.32043(19) 0.68211(19) 0.4561(2) 0.0406 1.0000 Uani . . . . . .
C10 C 0.19321(16) 0.59550(17) 0.38663(16) 0.0294 1.0000 Uani . . . . . .
C11 C 0.23619(14) 0.38019(16) 0.28442(15) 0.0236 1.0000 Uani . . . . . .
C12 C 0.35195(16) 0.42256(18) 0.32734(19) 0.0329 1.0000 Uani . . . . . .
C13 C 0.38260(17) 0.3684(2) 0.3078(2) 0.0411 1.0000 Uani . . . . . .
C14 C 0.14508(17) 0.62059(19) 0.39649(19) 0.0353 1.0000 Uani . . . . . .
C15 C 0.13916(18) 0.6841(2) 0.41796(19) 0.0380 1.0000 Uani . . . . . .
C16 C 0.0938(2) 0.7067(2) 0.4275(2) 0.0478 1.0000 Uani . . . . . .
C17 C 0.0551(2) 0.6667(3) 0.4165(3) 0.0627 1.0000 Uani . . . . . .
C18 C 0.0605(2) 0.6029(3) 0.3944(3) 0.0695 1.0000 Uani . . . . . .
C19 C 0.1055(2) 0.5811(2) 0.3839(3) 0.0545 1.0000 Uani . . . . . .
C20 C 0.20404(15) 0.32846(17) 0.25490(16) 0.0282 1.0000 Uani . . . . . .
C21 C 0.15534(16) 0.33983(19) 0.24048(19) 0.0343 1.0000 Uani . . . . . .
C22 C 0.12511(19) 0.2906(2) 0.2155(2) 0.0456 1.0000 Uani . . . . . .
C23 C 0.1433(2) 0.2285(2) 0.2067(2) 0.0473 1.0000 Uani . . . . . .
C24 C 0.1916(2) 0.2169(2) 0.22111(19) 0.0434 1.0000 Uani . . . . . .
C25 C 0.22236(17) 0.26639(18) 0.24499(17) 0.0331 1.0000 Uani . . . . . .
C26 C 0.34562(16) 0.53163(19) 0.61585(18) 0.0328 1.0000 Uani . . . . . .
C27 C 0.37199(19) 0.5885(2) 0.6307(2) 0.0443 1.0000 Uani . . . . . .
C28 C 0.3470(2) 0.6456(2) 0.6361(2) 0.0488 1.0000 Uani . . . . . .
C29 C 0.29793(19) 0.64666(18) 0.6244(2) 0.0400 1.0000 Uani . . . . . .
C30 C 0.27346(17) 0.58883(17) 0.60857(17) 0.0328 1.0000 Uani . . . . . .
C31 C 0.22032(17) 0.58612(18) 0.59200(16) 0.0325 1.0000 Uani . . . . . .
C32 C 0.1962(2) 0.6500(2) 0.5726(2) 0.0477 1.0000 Uani . . . . . .
Ni1 Ni 0.265911(17) 0.43871(2) 0.598124(19) 0.0209 1.0000 Uani . . . . . .
Cr1 Cr 0.25726(2) 0.50059(3) 0.34652(2) 0.0216 1.0000 Uani . . . . . .
Cl1 Cl 0.00909(6) 0.16821(9) 0.53278(13) 0.0974 1.0000 Uani . . . . . .
H331 H 0.1265 0.5882 0.6157 0.0848 1.0000 Uiso R . . . . .
H332 H 0.0904 0.5305 0.6016 0.0850 1.0000 Uiso R . . . . .
H333 H 0.1046 0.5736 0.5429 0.0852 1.0000 Uiso R . . . . .
H351 H 0.0784 0.4422 0.5437 0.0583 1.0000 Uiso R . . . . .
H361 H 0.0716 0.3304 0.5366 0.0561 1.0000 Uiso R . . . . .
H411 H 0.1842 0.1611 0.5617 0.0462 1.0000 Uiso R . . . . .
H421 H 0.1150 0.2194 0.5434 0.0473 1.0000 Uiso R . . . . .
H431 H 0.2783 0.1650 0.5822 0.0368 1.0000 Uiso R . . . . .
H441 H 0.3473 0.2260 0.6021 0.0374 1.0000 Uiso R . . . . .
H463 H 0.4115 0.3617 0.6758 0.0778 1.0000 Uiso R . . . . .
H462 H 0.3934 0.2890 0.6594 0.0780 1.0000 Uiso R . . . . .
H461 H 0.4205 0.3278 0.6074 0.0781 1.0000 Uiso R . . . . .
H481 H 0.4300 0.5086 0.5810 0.0870 1.0000 Uiso R . . . . .
H482 H 0.4404 0.4606 0.6429 0.0871 1.0000 Uiso R . . . . .
H483 H 0.4267 0.4326 0.5700 0.0870 1.0000 Uiso R . . . . .
H41 H 0.4439 0.4569 0.3746 0.0653 1.0000 Uiso R . . . . .
H51 H 0.4682 0.5524 0.4325 0.0730 1.0000 Uiso R . . . . .
H61 H 0.4093 0.6281 0.4547 0.0591 1.0000 Uiso R . . . . .
H92 H 0.2907 0.7046 0.4559 0.0630 1.0000 Uiso R . . . . .
H93 H 0.3339 0.6735 0.5004 0.0632 1.0000 Uiso R . . . . .
H91 H 0.3428 0.7077 0.4352 0.0627 1.0000 Uiso R . . . . .
H132 H 0.3630 0.3354 0.2851 0.0651 1.0000 Uiso R . . . . .
H131 H 0.3996 0.3509 0.3477 0.0650 1.0000 Uiso R . . . . .
H133 H 0.4050 0.3851 0.2792 0.0649 1.0000 Uiso R . . . . .
H151 H 0.1661 0.7113 0.4260 0.0485 1.0000 Uiso R . . . . .
H161 H 0.0900 0.7494 0.4420 0.0580 1.0000 Uiso R . . . . .
H171 H 0.0243 0.6817 0.4235 0.0760 1.0000 Uiso R . . . . .
H181 H 0.0334 0.5756 0.3873 0.0841 1.0000 Uiso R . . . . .
H191 H 0.1102 0.5390 0.3700 0.0649 1.0000 Uiso R . . . . .
H211 H 0.1433 0.3814 0.2470 0.0441 1.0000 Uiso R . . . . .
H221 H 0.0922 0.2985 0.2039 0.0571 1.0000 Uiso R . . . . .
H231 H 0.1227 0.1951 0.1906 0.0592 1.0000 Uiso R . . . . .
H241 H 0.2040 0.1754 0.2158 0.0542 1.0000 Uiso R . . . . .
H251 H 0.2552 0.2585 0.2545 0.0430 1.0000 Uiso R . . . . .
H271 H 0.4056 0.5872 0.6376 0.0569 1.0000 Uiso R . . . . .
H281 H 0.3636 0.6846 0.6483 0.0600 1.0000 Uiso R . . . . .
H291 H 0.2810 0.6856 0.6270 0.0521 1.0000 Uiso R . . . . .
H322 H 0.1653 0.6423 0.5463 0.0782 1.0000 Uiso R . . . . .
H321 H 0.1905 0.6718 0.6131 0.0781 1.0000 Uiso R . . . . .
H323 H 0.2167 0.6759 0.5483 0.0782 1.0000 Uiso R . . . . .
H501 H 0.0470 0.3488 0.7092 0.0893 0.6000 Uiso R . . . . .
H502 H 0.0722 0.2989 0.7586 0.0893 0.6000 Uiso R . . . . .
H503 H 0.0741 0.2904 0.6828 0.0893 0.6000 Uiso R . . . . .
H521 H 0.0429 0.4095 0.7130 0.1146 0.4000 Uiso R . . . . .
H522 H 0.0593 0.3508 0.7576 0.1146 0.4000 Uiso R . . . . .
H523 H 0.0597 0.3463 0.6811 0.1146 0.4000 Uiso R . . . . .
H491 H 0.1890 0.3523 0.7373 0.0428 0.6000 Uiso R . . . . .
H492 H 0.1630 0.3013 0.7767 0.0428 0.6000 Uiso R . . . . .
H493 H 0.1649 0.2928 0.7008 0.0428 0.6000 Uiso R . . . . .
H511 H 0.1815 0.3625 0.7364 0.0757 0.4000 Uiso R . . . . .
H512 H 0.1439 0.3235 0.7710 0.0757 0.4000 Uiso R . . . . .
H513 H 0.1444 0.3191 0.6945 0.0757 0.4000 Uiso R . . . . .
H531 H 0.1438 0.4435 0.7226 0.0701 0.6000 Uiso R . . . . .
H541 H 0.1619 0.4605 0.7281 0.0689 0.4000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.02038(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C33 . N10 . 1.474(5) yes
C33 . H331 . 0.978 no
C33 . H332 . 0.965 no
C33 . H333 . 0.954 no
C34 . C35 . 1.402(7) yes
C34 . N10 . 1.403(5) yes
C34 . N11 . 1.328(5) yes
C35 . C36 . 1.367(7) yes
C35 . H351 . 0.937 no
C36 . C37 . 1.398(7) yes
C36 . H361 . 0.947 no
C37 . C38 . 1.398(6) yes
C37 . C42 . 1.432(6) yes
C38 . C39 . 1.432(5) yes
C38 . N11 . 1.352(5) yes
C39 . C40 . 1.400(5) yes
C39 . N12 . 1.353(5) yes
C40 . C41 . 1.417(6) yes
C40 . C43 . 1.416(6) yes
C41 . C42 . 1.366(6) yes
C41 . H411 . 0.946 no
C42 . H421 . 0.928 no
C43 . C44 . 1.360(6) yes
C43 . H431 . 0.925 no
C44 . C45 . 1.427(5) yes
C44 . H441 . 0.943 no
C45 . N12 . 1.305(5) yes
C45 . N13 . 1.387(5) yes
C46 . N13 . 1.472(6) yes
C46 . H463 . 0.978 no
C46 . H462 . 0.975 no
C46 . H461 . 0.962 no
C47 . C48 . 1.489(7) yes
C47 . N14 . 1.294(5) yes
C47 . C26 . 1.478(6) yes
C48 . H481 . 0.973 no
C48 . H482 . 0.972 no
C48 . H483 . 0.972 no
C49 . N15 . 1.426(10) yes
C49 . H491 . 0.950 no
C49 . H492 . 0.950 no
C49 . H493 . 0.950 no
C50 . N15 . 1.465(14) yes
C50 . H501 . 0.950 no
C50 . H502 . 0.950 no
C50 . H503 . 0.950 no
C51 . C53 . 1.818(19) yes
C51 . N16 . 1.32(2) yes
C51 . H511 . 0.950 no
C51 . H512 . 0.950 no
C51 . H513 . 0.950 no
C52 . N16 . 1.54(3) yes
C52 . H521 . 0.950 no
C52 . H522 . 0.950 no
C52 . H523 . 0.950 no
C53 . N15 . 1.292(13) yes
C53 . O7 . 1.164(13) yes
C53 . H531 . 0.950 no
C54 . N16 . 1.19(2) yes
C54 . O8 . 1.229(17) yes
C54 . H541 . 0.950 no
N10 . N9 . 1.345(5) yes
N11 . Ni1 . 2.205(3) yes
N12 . Ni1 . 2.009(3) yes
N13 . N14 . 1.377(4) yes
N14 . Ni1 . 2.105(3) yes
O1 . C10 . 1.295(4) yes
O1 . Cr1 . 1.952(3) yes
O2 . C11 . 1.293(4) yes
O2 . Cr1 . 1.959(2) yes
O3 . Cl1 . 1.361(5) yes
O4 . Cl1 . 1.421(7) yes
O5 . Cl1 . 1.432(5) yes
O6 . Cl1 . 1.337(6) yes
N1 . C1 . 1.152(4) yes
N1 . Ni1 . 2.064(3) yes
N2 . C2 . 1.146(4) yes
N2 . Ni1 . 2.070(3) yes
N3 . C3 . 1.330(5) yes
N3 . C7 . 1.330(5) yes
N3 . Cr1 . 2.390(3) yes
N4 . N5 . 1.380(5) yes
N4 . C8 . 1.285(5) yes
N4 . Cr1 . 2.231(3) yes
N5 . C10 . 1.317(5) yes
N6 . N7 . 1.381(4) yes
N6 . C11 . 1.302(5) yes
N7 . C12 . 1.293(5) yes
N7 . Cr1 . 2.208(3) yes
N8 . C26 . 1.342(6) yes
N8 . C30 . 1.340(5) yes
N8 . Ni1 . 2.137(3) yes
N9 . C31 . 1.271(5) yes
N9 . Ni1 . 2.555(3) yes
C1 . Cr1 . 2.056(3) yes
C2 . Cr1 5_565 2.064(3) yes
C3 . C4 . 1.377(7) yes
C3 . C12 . 1.475(6) yes
C4 . C5 . 1.393(7) yes
C4 . H41 . 0.937 no
C5 . C6 . 1.391(8) yes
C5 . H51 . 0.949 no
C6 . C7 . 1.377(7) yes
C6 . H61 . 0.939 no
C7 . C8 . 1.478(6) yes
C8 . C9 . 1.497(5) yes
C9 . H92 . 0.952 no
C9 . H93 . 0.950 no
C9 . H91 . 0.953 no
C10 . C14 . 1.479(6) yes
C11 . C20 . 1.481(5) yes
C12 . C13 . 1.490(6) yes
C13 . H132 . 0.960 no
C13 . H131 . 0.961 no
C13 . H133 . 0.963 no
C14 . C15 . 1.397(5) yes
C14 . C19 . 1.378(7) yes
C15 . C16 . 1.389(7) yes
C15 . H151 . 0.942 no
C16 . C17 . 1.362(8) yes
C16 . H161 . 0.939 no
C17 . C18 . 1.405(8) yes
C17 . H171 . 0.942 no
C18 . C19 . 1.379(8) yes
C18 . H181 . 0.944 no
C19 . H191 . 0.927 no
C20 . C21 . 1.384(6) yes
C20 . C25 . 1.404(5) yes
C21 . C22 . 1.384(6) yes
C21 . H211 . 0.937 no
C22 . C23 . 1.399(7) yes
C22 . H221 . 0.939 no
C23 . C24 . 1.374(7) yes
C23 . H231 . 0.937 no
C24 . C25 . 1.389(6) yes
C24 . H241 . 0.937 no
C25 . H251 . 0.934 no
C26 . C27 . 1.402(6) yes
C27 . C28 . 1.384(7) yes
C27 . H271 . 0.937 no
C28 . C29 . 1.370(7) yes
C28 . H281 . 0.948 no
C29 . C30 . 1.397(6) yes
C29 . H291 . 0.938 no
C30 . C31 . 1.491(6) yes
C31 . C32 . 1.515(5) yes
C32 . H322 . 0.977 no
C32 . H321 . 0.965 no
C32 . H323 . 0.959 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N10 . C33 . H331 . 109.0 no
N10 . C33 . H332 . 111.3 no
H331 . C33 . H332 . 107.7 no
N10 . C33 . H333 . 111.0 no
H331 . C33 . H333 . 108.0 no
H332 . C33 . H333 . 109.7 no
C35 . C34 . N10 . 122.5(4) yes
C35 . C34 . N11 . 121.4(4) yes
N10 . C34 . N11 . 116.1(4) yes
C34 . C35 . C36 . 119.2(4) yes
C34 . C35 . H351 . 119.9 no
C36 . C35 . H351 . 120.9 no
C35 . C36 . C37 . 121.1(4) yes
C35 . C36 . H361 . 119.9 no
C37 . C36 . H361 . 119.0 no
C36 . C37 . C38 . 115.7(4) yes
C36 . C37 . C42 . 126.4(4) yes
C38 . C37 . C42 . 117.9(4) yes
C37 . C38 . C39 . 119.5(3) yes
C37 . C38 . N11 . 123.9(4) yes
C39 . C38 . N11 . 116.7(3) yes
C38 . C39 . C40 . 121.5(4) yes
C38 . C39 . N12 . 115.8(3) yes
C40 . C39 . N12 . 122.7(3) yes
C39 . C40 . C41 . 118.3(4) yes
C39 . C40 . C43 . 115.4(4) yes
C41 . C40 . C43 . 126.3(4) yes
C40 . C41 . C42 . 120.4(4) yes
C40 . C41 . H411 . 120.3 no
C42 . C41 . H411 . 119.3 no
C37 . C42 . C41 . 122.4(4) yes
C37 . C42 . H421 . 118.6 no
C41 . C42 . H421 . 119.0 no
C40 . C43 . C44 . 121.3(3) yes
C40 . C43 . H431 . 119.3 no
C44 . C43 . H431 . 119.4 no
C43 . C44 . C45 . 119.1(4) yes
C43 . C44 . H441 . 121.5 no
C45 . C44 . H441 . 119.4 no
C44 . C45 . N12 . 120.0(4) yes
C44 . C45 . N13 . 123.9(4) yes
N12 . C45 . N13 . 116.0(3) yes
N13 . C46 . H463 . 109.3 no
N13 . C46 . H462 . 107.3 no
H463 . C46 . H462 . 110.9 no
N13 . C46 . H461 . 109.1 no
H463 . C46 . H461 . 110.7 no
H462 . C46 . H461 . 109.4 no
C48 . C47 . N14 . 128.7(4) yes
C48 . C47 . C26 . 118.5(4) yes
N14 . C47 . C26 . 112.7(4) yes
C47 . C48 . H481 . 109.5 no
C47 . C48 . H482 . 109.2 no
H481 . C48 . H482 . 110.5 no
C47 . C48 . H483 . 108.4 no
H481 . C48 . H483 . 109.3 no
H482 . C48 . H483 . 109.9 no
N15 . C49 . H491 . 110.0 no
N15 . C49 . H492 . 109.4 no
H491 . C49 . H492 . 109.5 no
N15 . C49 . H493 . 109.0 no
H491 . C49 . H493 . 109.5 no
H492 . C49 . H493 . 109.5 no
N15 . C50 . H501 . 110.7 no
N15 . C50 . H502 . 108.9 no
H501 . C50 . H502 . 109.5 no
N15 . C50 . H503 . 108.8 no
H501 . C50 . H503 . 109.5 no
H502 . C50 . H503 . 109.5 no
C53 . C51 . H511 . 102.7 no
N16 . C51 . H511 . 112.0 no
C53 . C51 . H512 . 115.2 no
N16 . C51 . H512 . 107.4 no
H511 . C51 . H512 . 109.5 no
C53 . C51 . H513 . 110.2 no
N16 . C51 . H513 . 108.9 no
H511 . C51 . H513 . 109.5 no
H512 . C51 . H513 . 109.5 no
N16 . C52 . H521 . 113.8 no
N16 . C52 . H522 . 107.9 no
H521 . C52 . H522 . 109.5 no
N16 . C52 . H523 . 106.6 no
H521 . C52 . H523 . 109.5 no
H522 . C52 . H523 . 109.5 no
C51 . C53 . O7 . 160.3(13) yes
N15 . C53 . O7 . 133.1(13) yes
C51 . C53 . H531 . 87.2 no
N15 . C53 . H531 . 114.4 no
O7 . C53 . H531 . 112.4 no
N16 . C54 . O8 . 123.4(18) yes
N16 . C54 . H541 . 118.0 no
O8 . C54 . H541 . 118.6 no
C33 . N10 . C34 . 120.7(4) yes
C33 . N10 . N9 . 123.5(4) yes
C34 . N10 . N9 . 114.0(3) yes
C38 . N11 . C34 . 118.8(4) yes
C38 . N11 . Ni1 . 111.7(3) yes
C34 . N11 . Ni1 . 129.4(3) yes
C39 . N12 . C45 . 121.5(3) yes
C39 . N12 . Ni1 . 118.8(2) yes
C45 . N12 . Ni1 . 119.7(3) yes
C46 . N13 . C45 . 120.1(3) yes
C46 . N13 . N14 . 121.4(3) yes
C45 . N13 . N14 . 114.2(3) yes
N13 . N14 . C47 . 126.1(3) yes
N13 . N14 . Ni1 . 114.4(2) yes
C47 . N14 . Ni1 . 118.6(3) yes
C50 . N15 . C49 . 117.4(8) yes
C50 . N15 . C53 . 116.2(9) yes
C49 . N15 . C53 . 126.2(9) yes
C52 . N16 . C51 . 116.1(18) yes
C52 . N16 . C54 . 120.7(17) yes
C51 . N16 . C54 . 123.1(17) yes
C10 . O1 . Cr1 . 120.3(3) yes
C11 . O2 . Cr1 . 118.8(2) yes
C1 . N1 . Ni1 . 170.7(3) yes
C2 . N2 . Ni1 . 167.5(3) yes
C3 . N3 . C7 . 120.0(4) yes
C3 . N3 . Cr1 . 119.8(3) yes
C7 . N3 . Cr1 . 119.8(3) yes
N5 . N4 . C8 . 117.8(3) yes
N5 . N4 . Cr1 . 114.5(2) yes
C8 . N4 . Cr1 . 127.6(3) yes
N4 . N5 . C10 . 108.6(3) yes
N7 . N6 . C11 . 108.7(3) yes
N6 . N7 . C12 . 118.1(3) yes
N6 . N7 . Cr1 . 114.4(2) yes
C12 . N7 . Cr1 . 127.4(3) yes
C26 . N8 . C30 . 120.8(3) yes
C26 . N8 . Ni1 . 113.2(2) yes
C30 . N8 . Ni1 . 125.7(3) yes
N10 . N9 . C31 . 127.6(4) yes
N10 . N9 . Ni1 . 116.5(2) yes
C31 . N9 . Ni1 . 115.0(3) yes
N1 . C1 . Cr1 . 172.3(3) yes
Cr1 5_565 C2 . N2 . 171.6(3) yes
N3 . C3 . C4 . 122.0(4) yes
N3 . C3 . C12 . 112.5(4) yes
C4 . C3 . C12 . 125.5(4) yes
C3 . C4 . C5 . 118.1(5) yes
C3 . C4 . H41 . 120.9 no
C5 . C4 . H41 . 120.9 no
C4 . C5 . C6 . 119.7(5) yes
C4 . C5 . H51 . 120.6 no
C6 . C5 . H51 . 119.7 no
C5 . C6 . C7 . 117.9(4) yes
C5 . C6 . H61 . 121.5 no
C7 . C6 . H61 . 120.7 no
C6 . C7 . N3 . 122.3(4) yes
C6 . C7 . C8 . 124.5(4) yes
N3 . C7 . C8 . 113.1(4) yes
C7 . C8 . N4 . 113.6(3) yes
C7 . C8 . C9 . 121.1(4) yes
N4 . C8 . C9 . 125.3(4) yes
C8 . C9 . H92 . 110.1 no
C8 . C9 . H93 . 108.9 no
H92 . C9 . H93 . 110.5 no
C8 . C9 . H91 . 109.0 no
H92 . C9 . H91 . 110.2 no
H93 . C9 . H91 . 108.0 no
N5 . C10 . O1 . 123.8(4) yes
N5 . C10 . C14 . 118.9(3) yes
O1 . C10 . C14 . 117.3(4) yes
N6 . C11 . O2 . 124.8(3) yes
N6 . C11 . C20 . 117.9(3) yes
O2 . C11 . C20 . 117.3(3) yes
C3 . C12 . N7 . 114.1(3) yes
C3 . C12 . C13 . 121.0(4) yes
N7 . C12 . C13 . 124.9(4) yes
C12 . C13 . H132 . 110.1 no
C12 . C13 . H131 . 107.9 no
H132 . C13 . H131 . 109.9 no
C12 . C13 . H133 . 108.8 no
H132 . C13 . H133 . 110.0 no
H131 . C13 . H133 . 110.1 no
C10 . C14 . C15 . 120.8(4) yes
C10 . C14 . C19 . 119.6(4) yes
C15 . C14 . C19 . 119.5(4) yes
C14 . C15 . C16 . 120.1(5) yes
C14 . C15 . H151 . 119.6 no
C16 . C15 . H151 . 120.3 no
C15 . C16 . C17 . 119.8(4) yes
C15 . C16 . H161 . 119.7 no
C17 . C16 . H161 . 120.5 no
C16 . C17 . C18 . 120.7(5) yes
C16 . C17 . H171 . 120.1 no
C18 . C17 . H171 . 119.2 no
C17 . C18 . C19 . 119.2(6) yes
C17 . C18 . H181 . 119.9 no
C19 . C18 . H181 . 120.9 no
C18 . C19 . C14 . 120.6(5) yes
C18 . C19 . H191 . 121.0 no
C14 . C19 . H191 . 118.3 no
C11 . C20 . C21 . 120.3(3) yes
C11 . C20 . C25 . 120.1(4) yes
C21 . C20 . C25 . 119.5(4) yes
C20 . C21 . C22 . 120.2(4) yes
C20 . C21 . H211 . 119.2 no
C22 . C21 . H211 . 120.6 no
C21 . C22 . C23 . 120.2(5) yes
C21 . C22 . H221 . 120.5 no
C23 . C22 . H221 . 119.3 no
C22 . C23 . C24 . 119.8(4) yes
C22 . C23 . H231 . 120.0 no
C24 . C23 . H231 . 120.1 no
C23 . C24 . C25 . 120.3(4) yes
C23 . C24 . H241 . 120.4 no
C25 . C24 . H241 . 119.3 no
C20 . C25 . C24 . 120.0(4) yes
C20 . C25 . H251 . 119.8 no
C24 . C25 . H251 . 120.2 no
C47 . C26 . N8 . 117.7(3) yes
C47 . C26 . C27 . 121.5(4) yes
N8 . C26 . C27 . 120.8(4) yes
C26 . C27 . C28 . 118.2(5) yes
C26 . C27 . H271 . 120.5 no
C28 . C27 . H271 . 121.3 no
C27 . C28 . C29 . 120.4(4) yes
C27 . C28 . H281 . 120.5 no
C29 . C28 . H281 . 119.1 no
C28 . C29 . C30 . 119.0(4) yes
C28 . C29 . H291 . 120.5 no
C30 . C29 . H291 . 120.5 no
C29 . C30 . N8 . 120.6(4) yes
C29 . C30 . C31 . 122.5(4) yes
N8 . C30 . C31 . 116.9(3) yes
C30 . C31 . N9 . 113.7(3) yes
C30 . C31 . C32 . 115.6(4) yes
N9 . C31 . C32 . 130.4(4) yes
C31 . C32 . H322 . 110.0 no
C31 . C32 . H321 . 107.3 no
H322 . C32 . H321 . 108.7 no
C31 . C32 . H323 . 110.0 no
H322 . C32 . H323 . 110.9 no
H321 . C32 . H323 . 109.8 no
N11 . Ni1 . N9 . 63.85(11) yes
N11 . Ni1 . N8 . 131.04(13) yes
N9 . Ni1 . N8 . 67.33(12) yes
N11 . Ni1 . N14 . 152.64(12) yes
N9 . Ni1 . N14 . 143.47(12) yes
N8 . Ni1 . N14 . 76.16(13) yes
N11 . Ni1 . N2 . 92.39(12) yes
N9 . Ni1 . N2 . 84.56(11) yes
N8 . Ni1 . N2 . 86.53(11) yes
N14 . Ni1 . N2 . 92.31(12) yes
N11 . Ni1 . N1 . 86.57(11) yes
N9 . Ni1 . N1 . 86.20(11) yes
N8 . Ni1 . N1 . 86.78(11) yes
N14 . Ni1 . N1 . 93.09(12) yes
N2 . Ni1 . N1 . 170.15(12) yes
N11 . Ni1 . N12 . 77.01(12) yes
N9 . Ni1 . N12 . 140.85(12) yes
N8 . Ni1 . N12 . 151.78(14) yes
N14 . Ni1 . N12 . 75.68(12) yes
N2 . Ni1 . N12 . 96.33(11) yes
N1 . Ni1 . N12 . 92.98(11) yes
N7 . Cr1 . N4 . 131.90(12) yes
N7 . Cr1 . C2 5_564 87.86(11) yes
N4 . Cr1 . C2 5_564 92.10(11) yes
N7 . Cr1 . C1 . 89.93(11) yes
N4 . Cr1 . C1 . 85.11(11) yes
C2 5_564 Cr1 . C1 . 173.86(14) yes
N7 . Cr1 . N3 . 66.09(11) yes
N4 . Cr1 . N3 . 65.82(12) yes
C2 5_564 Cr1 . N3 . 89.48(12) yes
C1 . Cr1 . N3 . 84.38(12) yes
N7 . Cr1 . O2 . 73.28(11) yes
N4 . Cr1 . O2 . 154.76(12) yes
C2 5_564 Cr1 . O2 . 90.55(11) yes
C1 . Cr1 . O2 . 94.31(11) yes
N3 . Cr1 . O2 . 139.34(11) yes
N7 . Cr1 . O1 . 155.36(12) yes
N4 . Cr1 . O1 . 72.69(12) yes
C2 5_564 Cr1 . O1 . 93.42(12) yes
C1 . Cr1 . O1 . 90.98(12) yes
N3 . Cr1 . O1 . 138.48(11) yes
O2 . Cr1 . O1 . 82.10(11) yes
O5 . Cl1 . O4 . 108.4(4) yes
O5 . Cl1 . O3 . 108.2(3) yes
O4 . Cl1 . O3 . 109.9(6) yes
O5 . Cl1 . O6 . 111.3(4) yes
O4 . Cl1 . O6 . 107.5(5) yes
O3 . Cl1 . O6 . 111.5(5) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C48 . H483 . O3 4_556 167 0.97 2.35 3.303(8) yes
C6 . H61 . O4 3_555 138 0.94 2.53 3.283(8) yes
C17 . H171 . O5 2_566 143 0.94 2.56 3.356(8) yes

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.001 1202 397 ' '
2 0.500 0.000 -0.003 1202 397 ' '
_platon_squeeze_details          
;
;



# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
-1 1 4 x .
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Cpd1
_database_code_depnum_ccdc_archive 'CCDC 1958001'
loop_
_audit_author_name
_audit_author_address
'Carine Duhayon'
;LCC CNRS
France
;
_audit_update_record             
;
2019-10-08 deposited with the CCDC.	2019-12-16 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   14.8737(12)
_cell_length_b                   11.9090(9)
_cell_length_c                   15.8139(13)
_cell_angle_alpha                90
_cell_angle_beta                 109.989(3)
_cell_angle_gamma                90
_cell_volume                     2632.4(4)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c '
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x,-y+1/2,z+1/2
-x,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mo -1.6832 0.6857 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584
4.3875 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4


_chemical_formula_sum            'C23 H25 B2 F8 N7 Ni1 O2'
_chemical_formula_moiety         'C23 H25 N7 Ni O2, 2(B F4) '
_chemical_compound_source        ?
_chemical_formula_weight         663.81


_cell_measurement_reflns_used    9934
_cell_measurement_theta_min      3
_cell_measurement_theta_max      27
_cell_measurement_temperature    107

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_max          0.160

_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1352
_exptl_absorpt_coefficient_mu    0.832

# Sheldrick geometric approximatio 0.90 0.90 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_T_max  0.90
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      107
_diffrn_reflns_number            55103
_reflns_number_total             6533
_diffrn_reflns_av_R_equivalents  0.052
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 6533 
# Theoretical number of reflections is about 13164 


_diffrn_reflns_theta_min         1.457
_diffrn_reflns_theta_max         28.357
_diffrn_measured_fraction_theta_max 0.992

_diffrn_reflns_theta_full        27.790
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_reflns_limit_h_min              -19
_reflns_limit_h_max              18
_reflns_limit_k_min              0
_reflns_limit_k_max              15
_reflns_limit_l_min              0
_reflns_limit_l_max              21

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.37
_refine_diff_density_max         1.53


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns         5008
_refine_ls_number_restraints     0
_refine_ls_number_parameters     388
_oxford_refine_ls_R_factor_ref   0.0492
_refine_ls_wR_factor_ref         0.0499
_refine_ls_goodness_of_fit_ref   1.0937
_refine_ls_shift/su_max          0.0002831
_refine_ls_shift/su_mean         0.0000203


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        6523
_refine_ls_R_factor_all          0.0664
_refine_ls_wR_factor_all         0.0719

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5284
_refine_ls_R_factor_gt           0.0519
_refine_ls_wR_factor_gt          0.0517

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.192 0.160 0.612E-01 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ni1 Ni 0.24984(2) 0.40341(3) 0.22144(2) 0.0279 1.0000 Uani . . . . . .
C1 C 0.15819(17) 0.6300(2) 0.14574(17) 0.0219 1.0000 Uani . . . . . .
C2 C 0.10980(18) 0.7076(2) 0.07987(18) 0.0263 1.0000 Uani . . . . . .
C3 C 0.07888(19) 0.6746(2) -0.00924(19) 0.0299 1.0000 Uani . . . . . .
C4 C 0.09548(19) 0.5662(2) -0.03148(17) 0.0280 1.0000 Uani . . . . . .
C5 C 0.14422(17) 0.4919(2) 0.03735(16) 0.0225 1.0000 Uani . . . . . .
C6 C 0.16324(17) 0.3732(2) 0.01899(16) 0.0224 1.0000 Uani . . . . . .
C7 C 0.1470(2) 0.3395(3) -0.07683(17) 0.0294 1.0000 Uani . . . . . .
C8 C 0.1565(2) 0.1231(2) 0.02464(19) 0.0314 1.0000 Uani . . . . . .
C9 C 0.26481(17) 0.1638(2) 0.18010(18) 0.0236 1.0000 Uani . . . . . .
C10 C 0.2890(2) 0.0483(2) 0.2001(2) 0.0293 1.0000 Uani . . . . . .
C11 C 0.3338(2) 0.0184(2) 0.2877(2) 0.0317 1.0000 Uani . . . . . .
C12 C 0.35589(18) 0.0990(2) 0.35803(19) 0.0291 1.0000 Uani . . . . . .
C13 C 0.33337(17) 0.2102(2) 0.33145(17) 0.0230 1.0000 Uani . . . . . .
C14 C 0.35268(17) 0.2988(2) 0.39543(17) 0.0231 1.0000 Uani . . . . . .
C15 C 0.39691(18) 0.2762(3) 0.48694(18) 0.0294 1.0000 Uani . . . . . .
C16 C 0.4184(2) 0.1616(3) 0.5139(2) 0.0353 1.0000 Uani . . . . . .
C17 C 0.3979(2) 0.0770(3) 0.4522(2) 0.0350 1.0000 Uani . . . . . .
C18 C 0.41399(19) 0.3699(3) 0.54493(18) 0.0315 1.0000 Uani . . . . . .
C19 C 0.38601(18) 0.4750(3) 0.51257(17) 0.0283 1.0000 Uani . . . . . .
C20 C 0.33782(16) 0.4890(2) 0.41822(16) 0.0219 1.0000 Uani . . . . . .
C21 C 0.3282(2) 0.6964(2) 0.4327(2) 0.0338 1.0000 Uani . . . . . .
C22 C 0.19531(17) 0.6597(2) 0.24283(17) 0.0213 1.0000 Uani . . . . . .
C23 C 0.1563(2) 0.7636(2) 0.2720(2) 0.0307 1.0000 Uani . . . . . .
N1 N 0.17452(14) 0.52530(17) 0.12432(14) 0.0210 1.0000 Uani . . . . . .
N2 N 0.19534(15) 0.31454(18) 0.09081(14) 0.0224 1.0000 Uani . . . . . .
N3 N 0.21652(15) 0.20111(18) 0.09293(15) 0.0243 1.0000 Uani . . . . . .
N4 N 0.28944(15) 0.23994(17) 0.24385(14) 0.0217 1.0000 Uani . . . . . .
N5 N 0.32325(14) 0.40295(18) 0.36255(14) 0.0222 1.0000 Uani . . . . . .
N6 N 0.30037(15) 0.59132(19) 0.38104(14) 0.0239 1.0000 Uani . . . . . .
N7 N 0.25333(14) 0.58676(18) 0.29053(13) 0.0218 1.0000 Uani . . . . . .
O1 O 0.12668(12) 0.36122(15) 0.25071(13) 0.0268 1.0000 Uani . . . . . .
O2 O 0.37525(13) 0.44225(16) 0.19730(13) 0.0284 1.0000 Uani . . . . . .
B1 B 0.4096(2) 0.7587(3) 0.1892(2) 0.0327 1.0000 Uani . . . . . .
B2 B -0.0029(2) 0.5566(2) 0.3322(2) 0.0262 1.0000 Uani . . . . . .
F1 F 0.41706(19) 0.65501(17) 0.1523(2) 0.0695 1.0000 Uani . . . . . .
F2 F 0.42723(16) 0.7519(2) 0.27972(14) 0.0602 1.0000 Uani . . . . . .
F3 F 0.31889(12) 0.79946(15) 0.14796(13) 0.0408 1.0000 Uani . . . . . .
F4 F 0.47470(12) 0.83330(16) 0.17303(13) 0.0421 1.0000 Uani . . . . . .
F5 F -0.05937(12) 0.65314(13) 0.32121(12) 0.0327 1.0000 Uani . . . . . .
F6 F 0.00443(14) 0.52938(16) 0.24809(11) 0.0428 1.0000 Uani . . . . . .
F7 F 0.08740(12) 0.57938(15) 0.39122(12) 0.0395 1.0000 Uani . . . . . .
F8 F -0.04289(14) 0.46927(14) 0.36356(13) 0.0427 1.0000 Uani . . . . . .
H21 H 0.1010 0.7816 0.0958 0.0328 1.0000 Uiso R . . . . .
H31 H 0.0480 0.7256 -0.0544 0.0355 1.0000 Uiso R . . . . .
H41 H 0.0740 0.5421 -0.0918 0.0336 1.0000 Uiso R . . . . .
H71 H 0.1769 0.2689 -0.0755 0.0446 1.0000 Uiso R . . . . .
H73 H 0.1717 0.3965 -0.1057 0.0453 1.0000 Uiso R . . . . .
H72 H 0.0800 0.3301 -0.1084 0.0446 1.0000 Uiso R . . . . .
H81 H 0.0962 0.1590 -0.0066 0.0489 1.0000 Uiso R . . . . .
H83 H 0.1867 0.1048 -0.0182 0.0489 1.0000 Uiso R . . . . .
H82 H 0.1472 0.0543 0.0543 0.0487 1.0000 Uiso R . . . . .
H101 H 0.2717 -0.0069 0.1538 0.0358 1.0000 Uiso R . . . . .
H111 H 0.3498 -0.0572 0.3012 0.0392 1.0000 Uiso R . . . . .
H161 H 0.4457 0.1458 0.5755 0.0438 1.0000 Uiso R . . . . .
H171 H 0.4049 0.0023 0.4709 0.0427 1.0000 Uiso R . . . . .
H181 H 0.4454 0.3615 0.6055 0.0374 1.0000 Uiso R . . . . .
H191 H 0.3982 0.5364 0.5519 0.0327 1.0000 Uiso R . . . . .
H211 H 0.3280 0.7561 0.3916 0.0507 1.0000 Uiso R . . . . .
H213 H 0.3928 0.6883 0.4758 0.0507 1.0000 Uiso R . . . . .
H212 H 0.2848 0.7146 0.4638 0.0507 1.0000 Uiso R . . . . .
H231 H 0.1910 0.8285 0.2615 0.0473 1.0000 Uiso R . . . . .
H233 H 0.0884 0.7710 0.2371 0.0471 1.0000 Uiso R . . . . .
H232 H 0.1644 0.7592 0.3356 0.0470 1.0000 Uiso R . . . . .
H11 H 0.0866 0.4106 0.2441 0.0412 1.0000 Uiso R . . . . .
H12 H 0.0938 0.3060 0.2310 0.0411 1.0000 Uiso R . . . . .
H23 H 0.3989 0.5058 0.1891 0.0440 1.0000 Uiso R . . . . .
H22 H 0.4294 0.4247 0.2344 0.0446 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None

loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 . N1 . 2.132(2) yes
Ni1 . N2 . 2.213(2) yes
Ni1 . N4 . 2.030(2) yes
Ni1 . N5 . 2.123(2) yes
Ni1 . N7 . 2.434(2) yes
Ni1 . O1 . 2.0980(17) yes
Ni1 . O2 . 2.0799(18) yes
C1 . C2 . 1.395(3) yes
C1 . C22 . 1.486(3) yes
C1 . N1 . 1.336(3) yes
C2 . C3 . 1.382(4) yes
C2 . H21 . 0.937 no
C3 . C4 . 1.382(4) yes
C3 . H31 . 0.930 no
C4 . C5 . 1.397(4) yes
C4 . H41 . 0.942 no
C5 . C6 . 1.490(4) yes
C5 . N1 . 1.352(3) yes
C6 . C7 . 1.505(3) yes
C6 . N2 . 1.279(3) yes
C7 . H71 . 0.948 no
C7 . H73 . 0.958 no
C7 . H72 . 0.956 no
C8 . N3 . 1.472(3) yes
C8 . H81 . 0.964 no
C8 . H83 . 0.956 no
C8 . H82 . 0.977 no
C9 . C10 . 1.430(4) yes
C9 . N3 . 1.392(3) yes
C9 . N4 . 1.311(3) yes
C10 . C11 . 1.364(4) yes
C10 . H101 . 0.953 no
C11 . C12 . 1.419(4) yes
C11 . H111 . 0.937 no
C12 . C13 . 1.395(4) yes
C12 . C17 . 1.428(4) yes
C13 . C14 . 1.422(4) yes
C13 . N4 . 1.361(3) yes
C14 . C15 . 1.396(4) yes
C14 . N5 . 1.358(3) yes
C15 . C16 . 1.432(4) yes
C15 . C18 . 1.412(4) yes
C16 . C17 . 1.363(5) yes
C16 . H161 . 0.937 no
C17 . H171 . 0.933 no
C18 . C19 . 1.362(4) yes
C18 . H181 . 0.916 no
C19 . C20 . 1.427(3) yes
C19 . H191 . 0.936 no
C20 . N5 . 1.320(3) yes
C20 . N6 . 1.384(3) yes
C21 . N6 . 1.474(3) yes
C21 . H211 . 0.963 no
C21 . H213 . 0.974 no
C21 . H212 . 0.962 no
C22 . C23 . 1.505(3) yes
C22 . N7 . 1.274(3) yes
C23 . H231 . 0.975 no
C23 . H233 . 0.976 no
C23 . H232 . 0.972 no
N2 . N3 . 1.385(3) yes
N6 . N7 . 1.363(3) yes
O1 . H11 . 0.819 no
O1 . H12 . 0.815 no
O2 . H23 . 0.863 no
O2 . H22 . 0.845 no
B1 . F1 . 1.387(4) yes
B1 . F2 . 1.366(4) yes
B1 . F3 . 1.371(4) yes
B1 . F4 . 1.401(4) yes
B2 . F5 . 1.399(3) yes
B2 . F6 . 1.408(3) yes
B2 . F7 . 1.375(4) yes
B2 . F8 . 1.373(3) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . Ni1 . N2 . 73.66(8) yes
N1 . Ni1 . N4 . 145.95(8) yes
N2 . Ni1 . N4 . 72.31(8) yes
N1 . Ni1 . N5 . 135.55(8) yes
N2 . Ni1 . N5 . 150.75(8) yes
N4 . Ni1 . N5 . 78.45(8) yes
N1 . Ni1 . N7 . 68.77(7) yes
N2 . Ni1 . N7 . 142.42(7) yes
N4 . Ni1 . N7 . 145.25(8) yes
N5 . Ni1 . N7 . 66.80(8) yes
N1 . Ni1 . O1 . 92.21(7) yes
N2 . Ni1 . O1 . 91.29(8) yes
N4 . Ni1 . O1 . 87.42(8) yes
N5 . Ni1 . O1 . 86.65(8) yes
N7 . Ni1 . O1 . 90.12(7) yes
N1 . Ni1 . O2 . 89.98(8) yes
N2 . Ni1 . O2 . 90.02(8) yes
N4 . Ni1 . O2 . 91.17(8) yes
N5 . Ni1 . O2 . 91.27(8) yes
N7 . Ni1 . O2 . 90.00(7) yes
O1 . Ni1 . O2 . 177.69(8) yes
C2 . C1 . C22 . 121.9(2) yes
C2 . C1 . N1 . 121.4(2) yes
C22 . C1 . N1 . 116.7(2) yes
C1 . C2 . C3 . 118.7(2) yes
C1 . C2 . H21 . 120.4 no
C3 . C2 . H21 . 120.9 no
C2 . C3 . C4 . 119.9(2) yes
C2 . C3 . H31 . 120.1 no
C4 . C3 . H31 . 119.9 no
C3 . C4 . C5 . 118.9(2) yes
C3 . C4 . H41 . 120.9 no
C5 . C4 . H41 . 120.2 no
C4 . C5 . C6 . 122.1(2) yes
C4 . C5 . N1 . 120.7(2) yes
C6 . C5 . N1 . 117.2(2) yes
C5 . C6 . C7 . 118.3(2) yes
C5 . C6 . N2 . 112.6(2) yes
C7 . C6 . N2 . 129.1(2) yes
C6 . C7 . H71 . 107.6 no
C6 . C7 . H73 . 109.5 no
H71 . C7 . H73 . 112.7 no
C6 . C7 . H72 . 109.7 no
H71 . C7 . H72 . 107.6 no
H73 . C7 . H72 . 109.6 no
N3 . C8 . H81 . 108.7 no
N3 . C8 . H83 . 110.5 no
H81 . C8 . H83 . 108.6 no
N3 . C8 . H82 . 109.1 no
H81 . C8 . H82 . 111.0 no
H83 . C8 . H82 . 109.1 no
C10 . C9 . N3 . 122.1(2) yes
C10 . C9 . N4 . 120.8(2) yes
N3 . C9 . N4 . 117.1(2) yes
C9 . C10 . C11 . 118.4(3) yes
C9 . C10 . H101 . 120.8 no
C11 . C10 . H101 . 120.7 no
C10 . C11 . C12 . 121.4(2) yes
C10 . C11 . H111 . 118.7 no
C12 . C11 . H111 . 120.0 no
C11 . C12 . C13 . 116.0(2) yes
C11 . C12 . C17 . 126.4(3) yes
C13 . C12 . C17 . 117.5(3) yes
C12 . C13 . C14 . 121.4(2) yes
C12 . C13 . N4 . 122.4(2) yes
C14 . C13 . N4 . 116.2(2) yes
C13 . C14 . C15 . 120.2(2) yes
C13 . C14 . N5 . 116.4(2) yes
C15 . C14 . N5 . 123.3(2) yes
C14 . C15 . C16 . 118.1(3) yes
C14 . C15 . C18 . 115.9(3) yes
C16 . C15 . C18 . 126.0(3) yes
C15 . C16 . C17 . 121.2(3) yes
C15 . C16 . H161 . 118.4 no
C17 . C16 . H161 . 120.4 no
C12 . C17 . C16 . 121.5(3) yes
C12 . C17 . H171 . 117.9 no
C16 . C17 . H171 . 120.3 no
C15 . C18 . C19 . 121.2(2) yes
C15 . C18 . H181 . 120.5 no
C19 . C18 . H181 . 118.3 no
C18 . C19 . C20 . 118.7(3) yes
C18 . C19 . H191 . 120.1 no
C20 . C19 . H191 . 121.2 no
C19 . C20 . N5 . 121.1(2) yes
C19 . C20 . N6 . 122.2(2) yes
N5 . C20 . N6 . 116.7(2) yes
N6 . C21 . H211 . 108.5 no
N6 . C21 . H213 . 109.1 no
H211 . C21 . H213 . 108.7 no
N6 . C21 . H212 . 111.4 no
H211 . C21 . H212 . 109.3 no
H213 . C21 . H212 . 109.8 no
C1 . C22 . C23 . 117.8(2) yes
C1 . C22 . N7 . 112.7(2) yes
C23 . C22 . N7 . 129.3(2) yes
C22 . C23 . H231 . 108.5 no
C22 . C23 . H233 . 109.4 no
H231 . C23 . H233 . 109.8 no
C22 . C23 . H232 . 110.4 no
H231 . C23 . H232 . 109.5 no
H233 . C23 . H232 . 109.2 no
C5 . N1 . C1 . 120.4(2) yes
C5 . N1 . Ni1 . 116.30(17) yes
C1 . N1 . Ni1 . 123.31(16) yes
Ni1 . N2 . C6 . 118.29(17) yes
Ni1 . N2 . N3 . 115.86(15) yes
C6 . N2 . N3 . 124.6(2) yes
C8 . N3 . C9 . 120.2(2) yes
C8 . N3 . N2 . 121.5(2) yes
C9 . N3 . N2 . 111.8(2) yes
C13 . N4 . C9 . 120.9(2) yes
C13 . N4 . Ni1 . 115.91(17) yes
C9 . N4 . Ni1 . 122.73(17) yes
C14 . N5 . C20 . 119.7(2) yes
C14 . N5 . Ni1 . 112.80(16) yes
C20 . N5 . Ni1 . 127.40(17) yes
C21 . N6 . C20 . 121.0(2) yes
C21 . N6 . N7 . 124.2(2) yes
C20 . N6 . N7 . 113.5(2) yes
Ni1 . N7 . N6 . 115.58(15) yes
Ni1 . N7 . C22 . 116.09(16) yes
N6 . N7 . C22 . 126.5(2) yes
Ni1 . O1 . H11 . 116.9 no
Ni1 . O1 . H12 . 124.3 no
H11 . O1 . H12 . 102.5 no
Ni1 . O2 . H23 . 131.3 no
Ni1 . O2 . H22 . 121.3 no
H23 . O2 . H22 . 88.9 no
F1 . B1 . F2 . 112.0(3) yes
F1 . B1 . F3 . 108.8(3) yes
F2 . B1 . F3 . 109.0(3) yes
F1 . B1 . F4 . 109.1(3) yes
F2 . B1 . F4 . 109.4(3) yes
F3 . B1 . F4 . 108.5(3) yes
F5 . B2 . F6 . 108.0(2) yes
F5 . B2 . F7 . 109.1(2) yes
F6 . B2 . F7 . 108.3(2) yes
F5 . B2 . F8 . 110.5(2) yes
F6 . B2 . F8 . 110.5(2) yes
F7 . B2 . F8 . 110.3(2) yes


