#------------------------------------------------------------------------------
#$Date: 2020-07-22 04:05:26 +0300 (Wed, 22 Jul 2020) $
#$Revision: 254451 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/86/1558650.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1558650
loop_
_publ_author_name
'Chakarawet, Khetpakorn'
'Harris, T. David'
'Long, Jeffrey R.'
_publ_section_title
;
 Semiquinone radical-bridged M2 (M = Fe, Co, Ni) complexes with strong
 magnetic exchange giving rise to slow magnetic relaxation
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03078C
_journal_year                    2020
_chemical_formula_moiety
'C30 H64 N8 Ni2 O2, 2(B C24 F20), 2(C4 H8 O), C4 H10 O'
_chemical_formula_sum            'C90 H90 B2 F40 N8 Ni2 O5'
_chemical_formula_weight         2262.73
_chemical_name_systematic        '[(NiMe6tren)2(C6H4O2)][B(C6F5)4]2'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-11 deposited with the CCDC.	2020-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                97.774(3)
_cell_angle_beta                 90.679(3)
_cell_angle_gamma                101.898(2)
_cell_formula_units_Z            1
_cell_length_a                   12.015(2)
_cell_length_b                   12.540(2)
_cell_length_c                   16.083(3)
_cell_measurement_reflns_used    2066
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      14.011
_cell_measurement_theta_min      2.720
_cell_volume                     2347.4(7)
_computing_cell_refinement       'SAINT V8.38A (2016)'
_computing_data_collection       APEX3
_computing_data_reduction        'SAINT V8.38A (2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            56012
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         34.098
_diffrn_reflns_theta_min         1.719
_diffrn_source                   'Advanced Light Source, station 12.2.1'
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  0.9662
_exptl_absorpt_correction_T_min  0.9035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1552 before and 0.0602 after correction. The Ratio of minimum to maximum transmission is 0.9353. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/Et2O'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         17900
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0512P)²+0.5168P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15061
_reflns_number_total             17900
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc03078c2.cif
_cod_data_source_block           kjc182s
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        2347.5(7)
_cod_database_code               1558650
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.929
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1S-C2S = O1S-C3S
 1.34 with sigma of 0.02
 C2S-C1S = C4S-C3S
 1.54 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O1S, C1S, C2S, C3S, C4S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H3TC)=Sof(H3TD)=Sof(C5T)=Sof(H5TA)=Sof(H5TB)=1-FVAR(1)
 Sof(H3TA)=Sof(H3TB)=Sof(C4T)=Sof(H4TA)=Sof(H4TB)=FVAR(1)
 Fixed Sof: O1S(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) C2S(0.5) H2SA(0.5)
 H2SB(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) H4SC(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C8(H8A,H8B), C9(H9A,H9B), C12(H12A,H12B), C13(H13A,
 H13B), C1T(H1TA,H1TB), C2T(H2TA,H2TB), C3T(H3TC,H3TD), C3T(H3TA,H3TB),
 C4T(H4TA,H4TB), C5T(H5TA,H5TB), C2S(H2SA,H2SB), C3S(H3SA,H3SB)
5.b Me refined with riding coordinates:
 C1S(H1SA,H1SB,H1SC), C4S(H4SA,H4SB,H4SC)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3)
5.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.10212(2) 0.65566(2) 0.75084(2) 0.00978(4) Uani 1 1 d . . . . .
O1 O 0.04336(8) 0.53003(7) 0.67211(5) 0.01744(17) Uani 1 1 d . . . . .
N1 N 0.14362(8) 0.77541(8) 0.85907(6) 0.01333(17) Uani 1 1 d . . . . .
N2 N 0.27717(8) 0.65658(8) 0.75399(6) 0.01390(17) Uani 1 1 d . . . . .
N3 N 0.06727(9) 0.78836(9) 0.69316(7) 0.01589(18) Uani 1 1 d . . . . .
N4 N -0.01434(8) 0.57057(8) 0.83992(6) 0.01421(17) Uani 1 1 d . . . . .
C1 C 0.02357(10) 0.51683(10) 0.58876(7) 0.01413(19) Uani 1 1 d . . . . .
C2 C 0.11118(10) 0.52608(11) 0.53165(8) 0.0171(2) Uani 1 1 d . . . . .
H2 H 0.1881 0.5435 0.5524 0.021 Uiso 1 1 calc R . . . .
C3 C -0.08838(10) 0.48961(10) 0.55467(7) 0.0165(2) Uani 1 1 d . . . . .
H3 H -0.1500 0.4817 0.5914 0.020 Uiso 1 1 calc R . . . .
C4 C 0.27001(10) 0.80795(10) 0.86781(8) 0.0162(2) Uani 1 1 d . . . . .
H4A H 0.2937 0.8376 0.9270 0.019 Uiso 1 1 calc R . . . .
H4B H 0.2981 0.8661 0.8327 0.019 Uiso 1 1 calc R . . . .
C5 C 0.32050(10) 0.70784(10) 0.84019(8) 0.0165(2) Uani 1 1 d . . . . .
H5A H 0.4045 0.7302 0.8412 0.020 Uiso 1 1 calc R . . . .
H5B H 0.2999 0.6536 0.8797 0.020 Uiso 1 1 calc R . . . .
C6 C 0.34199(11) 0.71766(11) 0.69151(8) 0.0199(2) Uani 1 1 d . . . . .
H6A H 0.3104 0.6860 0.6350 0.030 Uiso 1 1 calc GR . . . .
H6B H 0.4220 0.7123 0.6957 0.030 Uiso 1 1 calc GR . . . .
H6C H 0.3365 0.7952 0.7024 0.030 Uiso 1 1 calc GR . . . .
C7 C 0.29312(11) 0.54136(11) 0.73931(9) 0.0196(2) Uani 1 1 d . . . . .
H7A H 0.2553 0.5008 0.7827 0.029 Uiso 1 1 calc GR . . . .
H7B H 0.3746 0.5411 0.7416 0.029 Uiso 1 1 calc GR . . . .
H7C H 0.2600 0.5061 0.6839 0.029 Uiso 1 1 calc GR . . . .
C8 C 0.09154(11) 0.86841(10) 0.84321(8) 0.0168(2) Uani 1 1 d . . . . .
H8A H 0.1273 0.9352 0.8821 0.020 Uiso 1 1 calc R . . . .
H8B H 0.0093 0.8509 0.8541 0.020 Uiso 1 1 calc R . . . .
C9 C 0.10702(11) 0.89082(10) 0.75317(8) 0.0185(2) Uani 1 1 d . . . . .
H9A H 0.0634 0.9466 0.7419 0.022 Uiso 1 1 calc R . . . .
H9B H 0.1885 0.9207 0.7450 0.022 Uiso 1 1 calc R . . . .
C10 C -0.05896(11) 0.76343(11) 0.68384(8) 0.0196(2) Uani 1 1 d . . . . .
H10A H -0.0915 0.7537 0.7386 0.029 Uiso 1 1 calc GR . . . .
H10B H -0.0845 0.6957 0.6444 0.029 Uiso 1 1 calc GR . . . .
H10C H -0.0841 0.8244 0.6624 0.029 Uiso 1 1 calc GR . . . .
C11 C 0.11146(13) 0.80645(13) 0.60930(9) 0.0249(3) Uani 1 1 d . . . . .
H11A H 0.1948 0.8274 0.6135 0.037 Uiso 1 1 calc GR . . . .
H11B H 0.0808 0.8654 0.5892 0.037 Uiso 1 1 calc GR . . . .
H11C H 0.0880 0.7385 0.5697 0.037 Uiso 1 1 calc GR . . . .
C12 C 0.09608(11) 0.72896(11) 0.93452(7) 0.0175(2) Uani 1 1 d . . . . .
H12A H 0.0889 0.7896 0.9791 0.021 Uiso 1 1 calc R . . . .
H12B H 0.1484 0.6867 0.9562 0.021 Uiso 1 1 calc R . . . .
C13 C -0.01993(10) 0.65412(10) 0.91284(8) 0.0171(2) Uani 1 1 d . . . . .
H13A H -0.0466 0.6171 0.9617 0.021 Uiso 1 1 calc R . . . .
H13B H -0.0753 0.6987 0.8999 0.021 Uiso 1 1 calc R . . . .
C14 C 0.03443(12) 0.48014(11) 0.86406(9) 0.0208(2) Uani 1 1 d . . . . .
H14A H 0.0434 0.4297 0.8137 0.031 Uiso 1 1 calc GR . . . .
H14B H -0.0165 0.4402 0.9019 0.031 Uiso 1 1 calc GR . . . .
H14C H 0.1089 0.5104 0.8927 0.031 Uiso 1 1 calc GR . . . .
C15 C -0.12975(10) 0.52229(11) 0.80302(8) 0.0197(2) Uani 1 1 d . . . . .
H15A H -0.1635 0.5803 0.7844 0.029 Uiso 1 1 calc GR . . . .
H15B H -0.1772 0.4879 0.8453 0.029 Uiso 1 1 calc GR . . . .
H15C H -0.1252 0.4666 0.7549 0.029 Uiso 1 1 calc GR . . . .
F12B F 0.32715(6) 0.29618(6) 0.76787(5) 0.01750(14) Uani 1 1 d . . . . .
F13B F 0.13945(6) 0.27506(7) 0.85592(6) 0.02344(17) Uani 1 1 d . . . . .
F14B F 0.11172(6) 0.14333(7) 0.98000(5) 0.02160(16) Uani 1 1 d . . . . .
F15B F 0.27918(7) 0.03755(7) 1.01405(5) 0.02035(15) Uani 1 1 d . . . . .
F16B F 0.46933(6) 0.06218(6) 0.93189(5) 0.01680(14) Uani 1 1 d . . . . .
F22B F 0.47959(6) -0.02346(6) 0.76081(5) 0.01688(14) Uani 1 1 d . . . . .
F23B F 0.62207(8) -0.15935(6) 0.76821(6) 0.02575(18) Uani 1 1 d . . . . .
F24B F 0.84365(7) -0.07868(7) 0.82102(6) 0.02543(17) Uani 1 1 d . . . . .
F25B F 0.91974(6) 0.14213(7) 0.86276(5) 0.02198(16) Uani 1 1 d . . . . .
F26B F 0.78160(6) 0.27945(6) 0.85581(5) 0.01730(14) Uani 1 1 d . . . . .
F32B F 0.69801(6) 0.29435(6) 0.68171(5) 0.01753(14) Uani 1 1 d . . . . .
F33B F 0.69293(7) 0.25374(8) 0.51436(5) 0.02591(18) Uani 1 1 d . . . . .
F34B F 0.50599(8) 0.12369(8) 0.42793(5) 0.02796(18) Uani 1 1 d . . . . .
F35B F 0.32359(7) 0.03539(8) 0.51459(5) 0.02650(18) Uani 1 1 d . . . . .
F36B F 0.32570(6) 0.07523(6) 0.68037(5) 0.01841(14) Uani 1 1 d . . . . .
F42B F 0.60556(6) 0.29152(6) 0.96631(5) 0.01651(14) Uani 1 1 d . . . . .
F43B F 0.65751(8) 0.49948(7) 1.04256(5) 0.02352(17) Uani 1 1 d . . . . .
F44B F 0.64541(8) 0.66836(7) 0.95448(6) 0.02860(19) Uani 1 1 d . . . . .
F45B F 0.58686(7) 0.62438(6) 0.78791(5) 0.02229(16) Uani 1 1 d . . . . .
F46B F 0.53452(6) 0.42064(6) 0.71048(5) 0.01606(13) Uani 1 1 d . . . . .
C11B C 0.40839(9) 0.17877(9) 0.84286(7) 0.01063(17) Uani 1 1 d . . . . .
C12B C 0.31856(9) 0.22984(9) 0.82806(7) 0.01311(19) Uani 1 1 d . . . . .
C13B C 0.21983(9) 0.21967(10) 0.87223(8) 0.0148(2) Uani 1 1 d . . . . .
C14B C 0.20566(10) 0.15395(10) 0.93512(8) 0.0152(2) Uani 1 1 d . . . . .
C15B C 0.29146(10) 0.10130(9) 0.95260(7) 0.01403(19) Uani 1 1 d . . . . .
C16B C 0.39007(9) 0.11481(9) 0.90758(7) 0.01195(18) Uani 1 1 d . . . . .
C21B C 0.62083(9) 0.13550(9) 0.80895(7) 0.01092(18) Uani 1 1 d . . . . .
C22B C 0.58850(9) 0.02191(9) 0.78659(7) 0.01307(19) Uani 1 1 d . . . . .
C23B C 0.66054(11) -0.05041(10) 0.78923(8) 0.0161(2) Uani 1 1 d . . . . .
C24B C 0.77269(10) -0.01004(10) 0.81530(8) 0.0166(2) Uani 1 1 d . . . . .
C25B C 0.81047(10) 0.10157(10) 0.83743(7) 0.0149(2) Uani 1 1 d . . . . .
C26B C 0.73515(9) 0.17159(9) 0.83385(7) 0.01247(18) Uani 1 1 d . . . . .
C31B C 0.51124(9) 0.19077(9) 0.69048(7) 0.01156(18) Uani 1 1 d . . . . .
C32B C 0.60211(10) 0.23091(9) 0.64253(7) 0.01356(19) Uani 1 1 d . . . . .
C33B C 0.60228(11) 0.21066(10) 0.55605(8) 0.0171(2) Uani 1 1 d . . . . .
C34B C 0.50753(11) 0.14502(11) 0.51204(7) 0.0186(2) Uani 1 1 d . . . . .
C35B C 0.41559(11) 0.10119(10) 0.55607(8) 0.0175(2) Uani 1 1 d . . . . .
C36B C 0.41907(10) 0.12425(9) 0.64304(7) 0.01403(19) Uani 1 1 d . . . . .
C41B C 0.56984(9) 0.34314(9) 0.83348(7) 0.01106(18) Uani 1 1 d . . . . .
C42B C 0.60022(9) 0.37143(9) 0.91875(7) 0.01285(19) Uani 1 1 d . . . . .
C43B C 0.62631(10) 0.47834(10) 0.96029(7) 0.0159(2) Uani 1 1 d . . . . .
C44B C 0.62042(10) 0.56426(10) 0.91613(8) 0.0175(2) Uani 1 1 d . . . . .
C45B C 0.59018(10) 0.54145(9) 0.83178(8) 0.0152(2) Uani 1 1 d . . . . .
C46B C 0.56515(9) 0.43305(9) 0.79255(7) 0.01252(18) Uani 1 1 d . . . . .
B1 B 0.52767(10) 0.21197(10) 0.79372(8) 0.01036(19) Uani 1 1 d . . . . .
O1T O -0.03106(13) 0.05210(11) 0.63227(12) 0.0545(4) Uani 1 1 d . . . . .
C1T C -0.11505(14) 0.11466(14) 0.62071(10) 0.0298(3) Uani 1 1 d . . . . .
H1TA H -0.1817 0.0928 0.6549 0.036 Uiso 1 1 calc R . . . .
H1TB H -0.1409 0.1045 0.5609 0.036 Uiso 1 1 calc R . . . .
C2T C -0.05579(16) 0.23202(15) 0.64937(12) 0.0371(4) Uani 1 1 d . . . . .
H2TA H -0.0574 0.2506 0.7111 0.044 Uiso 1 1 calc R . . . .
H2TB H -0.0912 0.2838 0.6222 0.044 Uiso 1 1 calc R . . . .
C3T C 0.06517(15) 0.23479(15) 0.62143(13) 0.0375(4) Uani 1 1 d . . . . .
H3TC H 0.0725 0.2446 0.5615 0.045 Uiso 0.399(18) 1 calc R . P A 2
H3TD H 0.1209 0.2935 0.6563 0.045 Uiso 0.399(18) 1 calc R . P A 2
H3TA H 0.1211 0.2683 0.6682 0.045 Uiso 0.601(18) 1 calc R . P A 1
H3TB H 0.0814 0.2774 0.5739 0.045 Uiso 0.601(18) 1 calc R . P A 1
C4T C 0.0698(5) 0.1119(5) 0.5941(6) 0.0459(13) Uani 0.601(18) 1 d . . P A 1
H4TA H 0.0648 0.0933 0.5322 0.055 Uiso 0.601(18) 1 calc R . P A 1
H4TB H 0.1407 0.0950 0.6160 0.055 Uiso 0.601(18) 1 calc R . P A 1
C5T C 0.0781(6) 0.1248(6) 0.6357(11) 0.047(2) Uani 0.399(18) 1 d . . P A 2
H5TA H 0.1262 0.0958 0.5924 0.056 Uiso 0.399(18) 1 calc R . P A 2
H5TB H 0.1162 0.1294 0.6914 0.056 Uiso 0.399(18) 1 calc R . P A 2
O1S O 0.4680(6) 0.5062(5) 0.5272(3) 0.0855(14) Uani 0.5 1 d D U P B -1
C1S C 0.3399(7) 0.3577(7) 0.5111(5) 0.095(2) Uani 0.5 1 d D U P B -1
H1SA H 0.3025 0.2875 0.4784 0.142 Uiso 0.5 1 calc R . P B -1
H1SB H 0.3691 0.3444 0.5651 0.142 Uiso 0.5 1 calc R . P B -1
H1SC H 0.2849 0.4055 0.5211 0.142 Uiso 0.5 1 calc R . P B -1
C2S C 0.4287(9) 0.4081(7) 0.4673(6) 0.097(2) Uani 0.5 1 d D U P B -1
H2SA H 0.4024 0.4253 0.4131 0.117 Uiso 0.5 1 calc R . P B -1
H2SB H 0.4876 0.3635 0.4576 0.117 Uiso 0.5 1 calc R . P B -1
C3S C 0.5770(8) 0.5565(10) 0.4994(6) 0.114(3) Uani 0.5 1 d D U P B -1
H3SA H 0.5665 0.5825 0.4450 0.137 Uiso 0.5 1 calc R . P B -1
H3SB H 0.6248 0.5007 0.4903 0.137 Uiso 0.5 1 calc R . P B -1
C4S C 0.6417(6) 0.6585(7) 0.5660(3) 0.0795(19) Uani 0.5 1 d D U P B -1
H4SA H 0.7155 0.6902 0.5446 0.119 Uiso 0.5 1 calc R . P B -1
H4SB H 0.5954 0.7146 0.5744 0.119 Uiso 0.5 1 calc R . P B -1
H4SC H 0.6537 0.6328 0.6197 0.119 Uiso 0.5 1 calc R . P B -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
H H 0.0000 0.0000
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
B B 0.0017 0.0007
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
F F 0.0185 0.0109
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
N N 0.0065 0.0035
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
Ni Ni 0.3380 1.1680
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
O O 0.0115 0.0064
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 N1 166.39(4) . . ?
O1 Ni1 N2 102.19(4) . . ?
O1 Ni1 N3 104.04(4) . . ?
O1 Ni1 N4 85.13(4) . . ?
N1 Ni1 N3 84.33(4) . . ?
N1 Ni1 N4 81.29(4) . . ?
N2 Ni1 N1 84.26(4) . . ?
N2 Ni1 N3 111.26(4) . . ?
N2 Ni1 N4 121.40(4) . . ?
N3 Ni1 N4 123.19(4) . . ?
C1 O1 Ni1 132.08(8) . . ?
C4 N1 Ni1 107.44(7) . . ?
C8 N1 Ni1 105.90(7) . . ?
C8 N1 C4 111.97(9) . . ?
C8 N1 C12 110.57(9) . . ?
C12 N1 Ni1 110.13(7) . . ?
C12 N1 C4 110.67(9) . . ?
C5 N2 Ni1 105.82(7) . . ?
C6 N2 Ni1 114.40(8) . . ?
C6 N2 C5 109.78(10) . . ?
C6 N2 C7 108.22(10) . . ?
C7 N2 Ni1 109.03(7) . . ?
C7 N2 C5 109.52(10) . . ?
C9 N3 Ni1 107.41(8) . . ?
C10 N3 Ni1 103.29(8) . . ?
C10 N3 C9 109.94(10) . . ?
C11 N3 Ni1 120.01(8) . . ?
C11 N3 C9 108.85(11) . . ?
C11 N3 C10 107.00(10) . . ?
C13 N4 Ni1 106.40(7) . . ?
C13 N4 C15 110.07(10) . . ?
C14 N4 Ni1 108.07(8) . . ?
C14 N4 C13 111.53(10) . . ?
C14 N4 C15 107.57(10) . . ?
C15 N4 Ni1 113.25(8) . . ?
O1 C1 C2 122.79(11) . . ?
O1 C1 C3 120.39(11) . . ?
C2 C1 C3 116.80(11) . . ?
C1 C2 H2 119.2 . . ?
C3 C2 C1 121.69(11) 2_566 . ?
C3 C2 H2 119.2 2_566 . ?
C1 C3 H3 119.2 . . ?
C2 C3 C1 121.51(11) 2_566 . ?
C2 C3 H3 119.2 2_566 . ?
N1 C4 H4A 109.8 . . ?
N1 C4 H4B 109.8 . . ?
N1 C4 C5 109.18(9) . . ?
H4A C4 H4B 108.3 . . ?
C5 C4 H4A 109.8 . . ?
C5 C4 H4B 109.8 . . ?
N2 C5 C4 110.35(10) . . ?
N2 C5 H5A 109.6 . . ?
N2 C5 H5B 109.6 . . ?
C4 C5 H5A 109.6 . . ?
C4 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
N1 C8 C9 110.84(10) . . ?
H8A C8 H8B 108.1 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
N3 C9 C8 110.85(10) . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N1 C12 H12A 109.6 . . ?
N1 C12 H12B 109.6 . . ?
N1 C12 C13 110.38(10) . . ?
H12A C12 H12B 108.1 . . ?
C13 C12 H12A 109.6 . . ?
C13 C12 H12B 109.6 . . ?
N4 C13 C12 110.74(10) . . ?
N4 C13 H13A 109.5 . . ?
N4 C13 H13B 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
N4 C14 H14A 109.5 . . ?
N4 C14 H14B 109.5 . . ?
N4 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N4 C15 H15A 109.5 . . ?
N4 C15 H15B 109.5 . . ?
N4 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C12B C11B B1 118.87(10) . . ?
C16B C11B C12B 113.56(10) . . ?
C16B C11B B1 126.99(9) . . ?
F12B C12B C11B 119.24(10) . . ?
F12B C12B C13B 116.09(10) . . ?
C13B C12B C11B 124.65(11) . . ?
F13B C13B C12B 120.72(11) . . ?
F13B C13B C14B 120.00(10) . . ?
C14B C13B C12B 119.26(10) . . ?
F14B C14B C13B 120.89(11) . . ?
F14B C14B C15B 120.34(11) . . ?
C15B C14B C13B 118.74(10) . . ?
F15B C15B C14B 119.42(10) . . ?
F15B C15B C16B 120.31(11) . . ?
C14B C15B C16B 120.27(11) . . ?
F16B C16B C11B 121.50(10) . . ?
F16B C16B C15B 114.99(10) . . ?
C15B C16B C11B 123.51(10) . . ?
C22B C21B B1 118.59(9) . . ?
C26B C21B C22B 113.62(10) . . ?
C26B C21B B1 127.41(10) . . ?
F22B C22B C21B 119.39(10) . . ?
F22B C22B C23B 116.08(10) . . ?
C23B C22B C21B 124.52(11) . . ?
F23B C23B C22B 120.87(11) . . ?
F23B C23B C24B 119.82(10) . . ?
C24B C23B C22B 119.29(11) . . ?
F24B C24B C23B 120.55(11) . . ?
F24B C24B C25B 120.31(11) . . ?
C25B C24B C23B 119.12(10) . . ?
F25B C25B C24B 119.77(10) . . ?
F25B C25B C26B 120.45(11) . . ?
C24B C25B C26B 119.78(11) . . ?
F26B C26B C21B 121.56(10) . . ?
F26B C26B C25B 114.79(10) . . ?
C25B C26B C21B 123.66(11) . . ?
C32B C31B B1 119.11(10) . . ?
C36B C31B C32B 113.55(10) . . ?
C36B C31B B1 126.86(10) . . ?
F32B C32B C31B 119.13(10) . . ?
F32B C32B C33B 116.29(10) . . ?
C33B C32B C31B 124.58(11) . . ?
F33B C33B C32B 120.91(11) . . ?
F33B C33B C34B 119.78(11) . . ?
C32B C33B C34B 119.31(11) . . ?
F34B C34B C33B 120.37(12) . . ?
F34B C34B C35B 120.78(12) . . ?
C35B C34B C33B 118.85(11) . . ?
F35B C35B C34B 119.77(11) . . ?
F35B C35B C36B 120.42(11) . . ?
C34B C35B C36B 119.81(11) . . ?
F36B C36B C31B 120.92(10) . . ?
F36B C36B C35B 115.18(10) . . ?
C35B C36B C31B 123.88(11) . . ?
C42B C41B B1 119.57(10) . . ?
C46B C41B C42B 113.66(10) . . ?
C46B C41B B1 126.25(10) . . ?
F42B C42B C41B 119.67(10) . . ?
F42B C42B C43B 115.86(10) . . ?
C43B C42B C41B 124.47(11) . . ?
F43B C43B C42B 121.10(11) . . ?
F43B C43B C44B 119.75(10) . . ?
C44B C43B C42B 119.15(11) . . ?
F44B C44B C43B 120.50(11) . . ?
F44B C44B C45B 120.43(11) . . ?
C45B C44B C43B 119.06(11) . . ?
F45B C45B C44B 119.54(10) . . ?
F45B C45B C46B 120.57(11) . . ?
C44B C45B C46B 119.88(11) . . ?
F46B C46B C41B 121.63(10) . . ?
F46B C46B C45B 114.60(10) . . ?
C45B C46B C41B 123.76(11) . . ?
C11B B1 C21B 113.53(9) . . ?
C11B B1 C41B 100.77(8) . . ?
C21B B1 C41B 114.06(9) . . ?
C31B B1 C11B 113.99(9) . . ?
C31B B1 C21B 101.31(8) . . ?
C31B B1 C41B 113.80(9) . . ?
C1T O1T C4T 103.2(2) . . ?
C1T O1T C5T 107.7(3) . . ?
O1T C1T H1TA 110.9 . . ?
O1T C1T H1TB 110.9 . . ?
O1T C1T C2T 104.50(14) . . ?
H1TA C1T H1TB 108.9 . . ?
C2T C1T H1TA 110.9 . . ?
C2T C1T H1TB 110.9 . . ?
C1T C2T H2TA 111.2 . . ?
C1T C2T H2TB 111.2 . . ?
C1T C2T C3T 103.03(14) . . ?
H2TA C2T H2TB 109.1 . . ?
C3T C2T H2TA 111.2 . . ?
C3T C2T H2TB 111.2 . . ?
C2T C3T H3TC 111.7 . . ?
C2T C3T H3TD 111.7 . . ?
C2T C3T H3TA 110.8 . . ?
C2T C3T H3TB 110.8 . . ?
C2T C3T C4T 104.7(2) . . ?
H3TC C3T H3TD 109.5 . . ?
H3TA C3T H3TB 108.9 . . ?
C4T C3T H3TA 110.8 . . ?
C4T C3T H3TB 110.8 . . ?
C5T C3T C2T 100.3(4) . . ?
C5T C3T H3TC 111.7 . . ?
C5T C3T H3TD 111.7 . . ?
O1T C4T C3T 103.1(4) . . ?
O1T C4T H4TA 111.2 . . ?
O1T C4T H4TB 111.2 . . ?
C3T C4T H4TA 111.2 . . ?
C3T C4T H4TB 111.2 . . ?
H4TA C4T H4TB 109.1 . . ?
O1T C5T C3T 110.1(4) . . ?
O1T C5T H5TA 109.6 . . ?
O1T C5T H5TB 109.6 . . ?
C3T C5T H5TA 109.6 . . ?
C3T C5T H5TB 109.6 . . ?
H5TA C5T H5TB 108.2 . . ?
C3S O1S C2S 105.3(5) . . ?
H1SA C1S H1SB 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?
C2S C1S H1SA 109.5 . . ?
C2S C1S H1SB 109.5 . . ?
C2S C1S H1SC 109.5 . . ?
O1S C2S H2SA 112.1 . . ?
O1S C2S H2SB 112.1 . . ?
C1S C2S O1S 98.6(8) . . ?
C1S C2S H2SA 112.1 . . ?
C1S C2S H2SB 112.1 . . ?
H2SA C2S H2SB 109.7 . . ?
O1S C3S H3SA 109.2 . . ?
O1S C3S H3SB 109.2 . . ?
O1S C3S C4S 112.2(7) . . ?
H3SA C3S H3SB 107.9 . . ?
C4S C3S H3SA 109.2 . . ?
C4S C3S H3SB 109.2 . . ?
C3S C4S H4SA 109.5 . . ?
C3S C4S H4SB 109.5 . . ?
C3S C4S H4SC 109.5 . . ?
H4SA C4S H4SB 109.5 . . ?
H4SA C4S H4SC 109.5 . . ?
H4SB C4S H4SC 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 1.8879(9) . ?
Ni1 N1 2.1207(10) . ?
Ni1 N2 2.1009(11) . ?
Ni1 N3 2.1215(11) . ?
Ni1 N4 2.2348(10) . ?
O1 C1 1.3405(14) . ?
N1 C4 1.4887(15) . ?
N1 C8 1.4814(16) . ?
N1 C12 1.4862(16) . ?
N2 C5 1.4865(15) . ?
N2 C6 1.4779(17) . ?
N2 C7 1.4842(16) . ?
N3 C9 1.4869(17) . ?
N3 C10 1.4855(17) . ?
N3 C11 1.4842(17) . ?
N4 C13 1.4752(16) . ?
N4 C14 1.4725(17) . ?
N4 C15 1.4760(16) . ?
C1 C2 1.4024(17) . ?
C1 C3 1.4032(16) . ?
C2 H2 0.9500 . ?
C2 C3 1.3914(17) 2_566 ?
C3 C2 1.3914(17) 2_566 ?
C3 H3 0.9500 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.5203(17) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.5184(18) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.5185(18) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
F12B C12B 1.3507(13) . ?
F13B C13B 1.3431(13) . ?
F14B C14B 1.3401(13) . ?
F15B C15B 1.3440(14) . ?
F16B C16B 1.3474(13) . ?
F22B C22B 1.3506(13) . ?
F23B C23B 1.3436(14) . ?
F24B C24B 1.3410(13) . ?
F25B C25B 1.3433(14) . ?
F26B C26B 1.3492(13) . ?
F32B C32B 1.3516(13) . ?
F33B C33B 1.3417(14) . ?
F34B C34B 1.3421(14) . ?
F35B C35B 1.3437(14) . ?
F36B C36B 1.3521(14) . ?
F42B C42B 1.3512(13) . ?
F43B C43B 1.3468(14) . ?
F44B C44B 1.3382(14) . ?
F45B C45B 1.3401(14) . ?
F46B C46B 1.3459(13) . ?
C11B C12B 1.3972(15) . ?
C11B C16B 1.3905(16) . ?
C11B B1 1.6498(16) . ?
C12B C13B 1.3821(16) . ?
C13B C14B 1.3795(18) . ?
C14B C15B 1.3791(17) . ?
C15B C16B 1.3883(16) . ?
C21B C22B 1.3925(15) . ?
C21B C26B 1.3905(15) . ?
C21B B1 1.6530(16) . ?
C22B C23B 1.3809(16) . ?
C23B C24B 1.3769(18) . ?
C24B C25B 1.3752(18) . ?
C25B C26B 1.3905(16) . ?
C31B C32B 1.3924(16) . ?
C31B C36B 1.3898(16) . ?
C31B B1 1.6485(17) . ?
C32B C33B 1.3797(17) . ?
C33B C34B 1.3826(18) . ?
C34B C35B 1.3774(18) . ?
C35B C36B 1.3878(17) . ?
C41B C42B 1.3940(16) . ?
C41B C46B 1.3906(16) . ?
C41B B1 1.6540(16) . ?
C42B C43B 1.3862(16) . ?
C43B C44B 1.3812(18) . ?
C44B C45B 1.3766(18) . ?
C45B C46B 1.3896(16) . ?
O1T C1T 1.425(2) . ?
O1T C4T 1.475(6) . ?
O1T C5T 1.430(7) . ?
C1T H1TA 0.9900 . ?
C1T H1TB 0.9900 . ?
C1T C2T 1.504(2) . ?
C2T H2TA 0.9900 . ?
C2T H2TB 0.9900 . ?
C2T C3T 1.521(3) . ?
C3T H3TC 0.9900 . ?
C3T H3TD 0.9900 . ?
C3T H3TA 0.9900 . ?
C3T H3TB 0.9900 . ?
C3T C4T 1.557(6) . ?
C3T C5T 1.467(7) . ?
C4T H4TA 0.9900 . ?
C4T H4TB 0.9900 . ?
C5T H5TA 0.9900 . ?
C5T H5TB 0.9900 . ?
O1S C2S 1.447(10) . ?
O1S C3S 1.436(10) . ?
C1S H1SA 0.9800 . ?
C1S H1SB 0.9800 . ?
C1S H1SC 0.9800 . ?
C1S C2S 1.376(11) . ?
C2S H2SA 0.9900 . ?
C2S H2SB 0.9900 . ?
C3S H3SA 0.9900 . ?
C3S H3SB 0.9900 . ?
C3S C4S 1.609(11) . ?
C4S H4SA 0.9800 . ?
C4S H4SB 0.9800 . ?
C4S H4SC 0.9800 . ?
