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#$Date: 2024-08-05 21:45:00 +0300 (Mon, 05 Aug 2024) $
#$Revision: 293815 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/64/7716486.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_7716486
loop_
_publ_author_name
'Imperato, Manuel'
'Nicolini, Alessio'
'Ribas-Ariño, Jordi'
'Antkowiak, Michał'
'Roubeau, Olivier'
'Cornia, Andrea'
'Novikov, Valentin'
'Barrios, Leoní A'
'Aromí, Guillem'
_publ_section_title
;
 Guest selectivity of [Ni₂] supramolecular helicates.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12301
_journal_page_last               12306
_journal_paper_doi               10.1039/d4dt01611d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C66 H48 N18 Ni2, B F4, 3(Br), 10(C H4 O), 5(H2 O)'
_chemical_formula_sum            'C76 H98 B Br3 F4 N18 Ni2 O15'
_chemical_formula_weight         1947.66
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2024-03-25 deposited with the CCDC.	2024-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.0486(13)
_cell_length_b                   30.0486(13)
_cell_length_c                   19.3054(9)
_cell_measurement_reflns_used    9660
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.28
_cell_volume                     17431.2(13)
_computing_cell_refinement       'Bruker SAINT v8.38a'
_computing_data_collection       'Global Phasing autoPROC package'
_computing_data_reduction        'Bruker SAINT v8.38a'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation at various κ'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.72932
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            118618
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        27.488
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_min         0.983
_exptl_absorpt_coefficient_mu    2.288
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_crystal_colour            blue-violet
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       block
_exptl_crystal_F_000             7888
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.864
_refine_diff_density_min         -1.668
_refine_diff_density_rms         0.193
_refine_ls_abs_structure_details
;
 Flack x determined using 6719 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.111(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     930
_refine_ls_number_reflns         18367
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0991
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2507P)²+0.4600P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2786
_refine_ls_wR_factor_ref         0.2911
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                15958
_reflns_number_total             18367
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01611d2.cif
_cod_data_source_block           MI7
_cod_depositor_comments
'Adding full bibliography for 7716485--7716486.cif.'
_cod_original_cell_volume        17431.2(17)
_cod_database_code               7716486
_shelx_shelxl_version_number     2017/1
_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_min   0.829
_shelx_estimated_absorpt_t_max   0.860
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
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 0.28431(3) 0.86446(4) 0.35931(6) 0.0414(3) Uani 1 1 d . . . . .
Ni2 Ni 0.51695(4) 0.73728(4) 0.65072(6) 0.0452(3) Uani 1 1 d . . . . .
N1 N 0.2156(2) 0.8619(3) 0.3865(5) 0.0518(18) Uani 1 1 d . . . . .
N2 N 0.2783(2) 0.8009(2) 0.4009(4) 0.0409(14) Uani 1 1 d . . . . .
N3 N 0.3054(2) 0.7659(3) 0.4170(4) 0.0429(15) Uani 1 1 d . . . . .
H3B H 0.334406 0.765664 0.411068 0.052 Uiso 1 1 calc R U . . .
N4 N 0.4267(3) 0.7012(3) 0.5840(5) 0.0513(19) Uani 1 1 d . . . . .
H4B H 0.410616 0.725477 0.588849 0.062 Uiso 1 1 calc R U . . .
N5 N 0.4689(3) 0.6974(3) 0.6024(5) 0.0506(18) Uani 1 1 d . . . . .
N6 N 0.5527(3) 0.6776(3) 0.6333(5) 0.0515(18) Uani 1 1 d . . . . .
N7 N 0.2754(3) 0.8425(3) 0.2569(4) 0.0491(17) Uani 1 1 d . . . . .
N8 N 0.3495(2) 0.8558(2) 0.3261(4) 0.0429(15) Uani 1 1 d . . . . .
N9 N 0.3910(2) 0.8592(3) 0.3505(4) 0.0432(15) Uani 1 1 d . . . . .
H9A H 0.397670 0.866514 0.393410 0.052 Uiso 1 1 calc R U . . .
N10 N 0.5189(2) 0.7806(2) 0.4975(4) 0.0392(14) Uani 1 1 d . . . . .
H10B H 0.496096 0.766479 0.479313 0.047 Uiso 1 1 calc R U . . .
N11 N 0.5355(2) 0.7725(2) 0.5623(4) 0.0400(14) Uani 1 1 d . . . . .
N12 N 0.5744(3) 0.7730(3) 0.6834(5) 0.0523(18) Uani 1 1 d . . . . .
N13 N 0.2787(2) 0.9322(3) 0.3289(5) 0.0481(17) Uani 1 1 d . . . . .
N14 N 0.3027(3) 0.8986(3) 0.4493(4) 0.0480(17) Uani 1 1 d . . . . .
N15 N 0.3219(3) 0.8889(3) 0.5093(4) 0.0434(15) Uani 1 1 d . . . . .
H15A H 0.326934 0.861697 0.524203 0.052 Uiso 1 1 calc R U . . .
N16 N 0.4542(3) 0.8234(3) 0.6595(4) 0.0458(16) Uani 1 1 d . . . . .
H16B H 0.456464 0.831825 0.615987 0.055 Uiso 1 1 calc R U . . .
N17 N 0.4735(3) 0.7872(3) 0.6850(4) 0.0496(17) Uani 1 1 d . . . . .
N18 N 0.5016(3) 0.7170(4) 0.7543(5) 0.057(2) Uani 1 1 d . . . . .
C1 C 0.1856(4) 0.8956(5) 0.3803(9) 0.072(3) Uani 1 1 d . . . . .
H1A H 0.194101 0.923135 0.360046 0.087 Uiso 1 1 calc R U . . .
C2 C 0.1408(4) 0.8891(6) 0.4046(9) 0.082(4) Uani 1 1 d . . . . .
H2A H 0.120513 0.913361 0.404380 0.099 Uiso 1 1 calc R U . . .
C3 C 0.1275(4) 0.8498(7) 0.4274(11) 0.095(5) Uani 1 1 d . . . . .
H3A H 0.097945 0.846550 0.444330 0.114 Uiso 1 1 calc R U . . .
C4 C 0.1575(4) 0.8105(7) 0.4271(10) 0.092(5) Uani 1 1 d . . . . .
H4A H 0.147743 0.781010 0.436464 0.111 Uiso 1 1 calc R U . . .
C5 C 0.2010(3) 0.8212(4) 0.4117(6) 0.055(2) Uani 1 1 d . . . . .
C6 C 0.2370(3) 0.7884(3) 0.4176(5) 0.0451(18) Uani 1 1 d . . . . .
C7 C 0.2369(3) 0.7441(4) 0.4428(5) 0.050(2) Uani 1 1 d . . . . .
H7A H 0.212025 0.726653 0.456280 0.061 Uiso 1 1 calc R U . . .
C8 C 0.2816(3) 0.7318(3) 0.4432(5) 0.0441(18) Uani 1 1 d . . . . .
C9 C 0.3034(3) 0.6927(3) 0.4710(5) 0.0441(18) Uani 1 1 d . . . . .
C10 C 0.2808(3) 0.6518(3) 0.4773(6) 0.052(2) Uani 1 1 d . . . . .
H10A H 0.251765 0.648879 0.458358 0.062 Uiso 1 1 calc R U . . .
C11 C 0.2998(4) 0.6158(4) 0.5104(7) 0.063(3) Uani 1 1 d . . . . .
H11A H 0.283296 0.589183 0.516800 0.075 Uiso 1 1 calc R U . . .
C12 C 0.3429(4) 0.6187(3) 0.5341(7) 0.058(2) Uani 1 1 d . . . . .
H12A H 0.356589 0.593381 0.554560 0.069 Uiso 1 1 calc R U . . .
C13 C 0.3667(4) 0.6584(3) 0.5284(6) 0.051(2) Uani 1 1 d . . . . .
C14 C 0.3455(3) 0.6947(3) 0.4970(5) 0.0420(16) Uani 1 1 d . . . . .
H14A H 0.361302 0.722031 0.493581 0.050 Uiso 1 1 calc R U . . .
C15 C 0.4116(3) 0.6625(3) 0.5565(5) 0.0469(19) Uani 1 1 d . . . . .
C16 C 0.4456(3) 0.6315(3) 0.5624(6) 0.049(2) Uani 1 1 d . . . . .
H16A H 0.444799 0.600893 0.550218 0.059 Uiso 1 1 calc R U . . .
C17 C 0.4817(3) 0.6555(3) 0.5907(6) 0.052(2) Uani 1 1 d . . . . .
C18 C 0.5273(4) 0.6427(4) 0.6077(7) 0.058(2) Uani 1 1 d . . . . .
C19 C 0.5433(5) 0.6024(4) 0.5973(9) 0.074(3) Uani 1 1 d . . . . .
H19A H 0.523295 0.579806 0.582482 0.089 Uiso 1 1 calc R U . . .
C20 C 0.5875(6) 0.5911(5) 0.6068(14) 0.102(6) Uani 1 1 d . . . . .
H20A H 0.599499 0.563140 0.593602 0.123 Uiso 1 1 calc R U . . .
C21 C 0.6149(5) 0.6271(5) 0.6398(11) 0.092(5) Uani 1 1 d . . . . .
H21A H 0.644833 0.621751 0.653131 0.110 Uiso 1 1 calc R U . . .
C22 C 0.5953(3) 0.6684(4) 0.6503(6) 0.057(2) Uani 1 1 d . . . . .
H22A H 0.612703 0.691287 0.670570 0.068 Uiso 1 1 calc R U . . .
C23 C 0.2361(4) 0.8343(5) 0.2229(7) 0.067(3) Uani 1 1 d . . . . .
H23A H 0.209087 0.837815 0.247999 0.081 Uiso 1 1 calc R U . . .
C24 C 0.2335(5) 0.8215(7) 0.1553(8) 0.084(4) Uani 1 1 d . . . . .
H24A H 0.205479 0.817078 0.133702 0.101 Uiso 1 1 calc R U . . .
C25 C 0.2723(5) 0.8150(7) 0.1191(8) 0.089(5) Uani 1 1 d . . . . .
H25A H 0.271316 0.806347 0.071747 0.106 Uiso 1 1 calc R U . . .
C26 C 0.3131(4) 0.8212(5) 0.1522(6) 0.067(3) Uani 1 1 d . . . . .
H26A H 0.340227 0.815631 0.128526 0.080 Uiso 1 1 calc R U . . .
C27 C 0.3132(3) 0.8360(4) 0.2210(5) 0.0483(19) Uani 1 1 d . . . . .
C28 C 0.3544(3) 0.8444(3) 0.2582(5) 0.0409(16) Uani 1 1 d . . . . .
C29 C 0.3988(3) 0.8416(3) 0.2417(5) 0.0463(19) Uani 1 1 d . . . . .
H29A H 0.411249 0.834904 0.197716 0.056 Uiso 1 1 calc R U . . .
C30 C 0.4210(3) 0.8502(3) 0.3012(5) 0.0465(18) Uani 1 1 d . . . . .
C31 C 0.4699(3) 0.8505(3) 0.3186(5) 0.0437(17) Uani 1 1 d . . . . .
C32 C 0.5014(3) 0.8705(4) 0.2730(6) 0.053(2) Uani 1 1 d . . . . .
H32A H 0.492184 0.883864 0.230723 0.063 Uiso 1 1 calc R U . . .
C33 C 0.5451(3) 0.8700(4) 0.2917(6) 0.059(3) Uani 1 1 d . . . . .
H33A H 0.566584 0.882095 0.260963 0.071 Uiso 1 1 calc R U . . .
C34 C 0.5591(3) 0.8524(4) 0.3546(7) 0.057(2) Uani 1 1 d . . . . .
H34A H 0.589497 0.854333 0.367878 0.069 Uiso 1 1 calc R U . . .
C35 C 0.5284(3) 0.8319(3) 0.3976(5) 0.0448(18) Uani 1 1 d . . . . .
C36 C 0.4829(3) 0.8309(3) 0.3797(5) 0.0420(17) Uani 1 1 d . . . . .
H36A H 0.461777 0.817014 0.409228 0.050 Uiso 1 1 calc R U . . .
C37 C 0.5420(3) 0.8132(3) 0.4651(5) 0.0458(18) Uani 1 1 d . . . . .
C38 C 0.5760(3) 0.8266(3) 0.5098(5) 0.0470(19) Uani 1 1 d . . . . .
H38A H 0.598269 0.848431 0.501607 0.056 Uiso 1 1 calc R U . . .
C39 C 0.5699(3) 0.8003(3) 0.5701(5) 0.0458(18) Uani 1 1 d . . . . .
C40 C 0.5934(3) 0.7989(3) 0.6362(6) 0.0478(19) Uani 1 1 d . . . . .
C41 C 0.6328(3) 0.8221(3) 0.6491(7) 0.058(3) Uani 1 1 d . . . . .
H41A H 0.645754 0.840093 0.614029 0.070 Uiso 1 1 calc R U . . .
C42 C 0.6523(4) 0.8185(4) 0.7126(8) 0.068(3) Uani 1 1 d . . . . .
H42A H 0.679220 0.834002 0.722158 0.081 Uiso 1 1 calc R U . . .
C43 C 0.6329(5) 0.7925(5) 0.7625(8) 0.076(3) Uani 1 1 d . . . . .
H43A H 0.645954 0.790468 0.807215 0.091 Uiso 1 1 calc R U . . .
C44 C 0.5939(4) 0.7690(5) 0.7474(6) 0.061(3) Uani 1 1 d . . . . .
H44A H 0.580850 0.750335 0.781469 0.074 Uiso 1 1 calc R U . . .
C45 C 0.2635(4) 0.9466(4) 0.2669(6) 0.061(3) Uani 1 1 d . . . . .
H45A H 0.260114 0.925714 0.230363 0.074 Uiso 1 1 calc R U . . .
C46 C 0.2529(4) 0.9901(4) 0.2551(7) 0.063(3) Uani 1 1 d . . . . .
H46A H 0.242020 0.999065 0.211103 0.076 Uiso 1 1 calc R U . . .
C47 C 0.2585(4) 1.0229(4) 0.3105(8) 0.068(3) Uani 1 1 d . . . . .
H47A H 0.250600 1.053260 0.304239 0.082 Uiso 1 1 calc R U . . .
C48 C 0.2757(4) 1.0075(4) 0.3723(7) 0.063(3) Uani 1 1 d . . . . .
H48A H 0.281384 1.027503 0.409412 0.076 Uiso 1 1 calc R U . . .
C49 C 0.2849(3) 0.9613(3) 0.3795(6) 0.051(2) Uani 1 1 d . . . . .
C50 C 0.3022(3) 0.9423(3) 0.4444(6) 0.0476(19) Uani 1 1 d . . . . .
C51 C 0.3205(3) 0.9619(3) 0.5036(6) 0.052(2) Uani 1 1 d . . . . .
H51A H 0.324015 0.992645 0.513833 0.062 Uiso 1 1 calc R U . . .
C52 C 0.3325(3) 0.9254(3) 0.5439(5) 0.0476(19) Uani 1 1 d . . . . .
C53 C 0.3566(4) 0.9248(3) 0.6101(5) 0.051(2) Uani 1 1 d . . . . .
C54 C 0.3534(5) 0.9608(4) 0.6587(6) 0.064(3) Uani 1 1 d . . . . .
H54A H 0.335162 0.985914 0.649453 0.076 Uiso 1 1 calc R U . . .
C55 C 0.3776(5) 0.9578(4) 0.7195(7) 0.067(3) Uani 1 1 d . . . . .
H55A H 0.376768 0.982266 0.750624 0.081 Uiso 1 1 calc R U . . .
C56 C 0.4025(4) 0.9219(4) 0.7370(6) 0.064(3) Uani 1 1 d . . . . .
H56A H 0.417574 0.921172 0.780324 0.077 Uiso 1 1 calc R U . . .
C57 C 0.4062(3) 0.8857(4) 0.6914(6) 0.053(2) Uani 1 1 d . . . . .
C58 C 0.3817(3) 0.8877(3) 0.6284(5) 0.051(2) Uani 1 1 d . . . . .
H58A H 0.382634 0.862981 0.597786 0.061 Uiso 1 1 calc R U . . .
C59 C 0.4309(3) 0.8457(3) 0.7070(5) 0.0488(19) Uani 1 1 d . . . . .
C60 C 0.4370(3) 0.8233(4) 0.7697(5) 0.051(2) Uani 1 1 d . . . . .
H60A H 0.426167 0.831346 0.814226 0.061 Uiso 1 1 calc R U . . .
C61 C 0.4631(3) 0.7856(3) 0.7511(5) 0.0477(19) Uani 1 1 d . . . . .
C62 C 0.4786(3) 0.7465(4) 0.7904(6) 0.055(2) Uani 1 1 d . . . . .
C63 C 0.4689(4) 0.7431(5) 0.8616(7) 0.068(3) Uani 1 1 d . . . . .
H63A H 0.451989 0.765488 0.884416 0.082 Uiso 1 1 calc R U . . .
C64 C 0.4841(5) 0.7073(6) 0.8969(8) 0.081(4) Uani 1 1 d . . . . .
H64A H 0.479393 0.704186 0.945313 0.097 Uiso 1 1 calc R U . . .
C65 C 0.5081(5) 0.6737(5) 0.8575(9) 0.077(4) Uani 1 1 d . . . . .
H65A H 0.518502 0.647488 0.879758 0.093 Uiso 1 1 calc R U . . .
C66 C 0.5156(4) 0.6800(5) 0.7888(8) 0.070(3) Uani 1 1 d . . . . .
H66A H 0.531235 0.657746 0.763775 0.083 Uiso 1 1 calc R U . . .
Br1 Br 0.40211(5) 0.80157(5) 0.50648(8) 0.0747(4) Uani 1 1 d . . . . .
Br2 Br 0.39336(5) 0.73400(5) 0.32262(9) 0.0775(4) Uani 1 1 d . . . . .
Br3A Br 0.47428(17) 0.70009(17) 0.4128(3) 0.0970(14) Uani 0.39 1 d . . P A 1
Br3B Br 0.2893(2) 0.79644(14) 0.5888(2) 0.1034(17) Uani 0.39 1 d . . P B 2
Br3C Br 0.3449(3) 0.7906(3) 0.5933(5) 0.099(2) Uani 0.22 1 d . . P C 3
B1 B 0.3962(3) 0.8097(4) 0.9972(5) 0.060(3) Uani 1 1 d D . . . .
F1 F 0.4081(3) 0.8324(3) 1.0598(4) 0.081(2) Uani 1 1 d D . . . .
F2 F 0.3519(2) 0.8080(4) 0.9924(5) 0.089(3) Uani 1 1 d D . . . .
F3 F 0.4166(3) 0.8326(4) 0.9433(5) 0.094(3) Uani 1 1 d D . . . .
F4 F 0.4158(4) 0.7676(3) 1.0010(5) 0.097(3) Uani 1 1 d D . . . .
O1W O 0.3598(7) 0.7541(5) 0.6757(10) 0.135(6) Uani 1 1 d . . . . .
O2W O 0.7260(19) 0.7179(19) 0.762(3) 0.27(2) Uani 1 1 d . U . . .
O3W O 0.3999(17) 0.6077(18) 0.728(3) 0.250(17) Uani 1 1 d . U . . .
O4W O 0.0134(11) 0.8656(11) 0.5473(18) 0.195(11) Uani 1 1 d . U . . .
O5W O 0.4266(5) 0.9252(7) 0.4483(8) 0.135(6) Uani 1 1 d . U . . .
O1S O 0.4815(8) 0.8779(8) 0.5463(12) 0.141(6) Uani 1 1 d . U . . .
H1S H 0.463988 0.882958 0.508462 0.211 Uiso 1 1 d R U . . .
C1S C 0.5039(10) 0.9095(8) 0.5716(15) 0.124(7) Uani 1 1 d . U . . .
H1S1 H 0.484839 0.935803 0.576657 0.187 Uiso 1 1 calc R U . . .
H1S2 H 0.528811 0.916519 0.540786 0.187 Uiso 1 1 calc R U . . .
H1S3 H 0.515355 0.900753 0.617147 0.187 Uiso 1 1 calc R U . . .
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
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Br Br -0.4703 2.5520
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Ni Ni 0.3377 1.1698
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
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
N8 Ni1 N2 94.9(3) . . ?
N8 Ni1 N14 93.9(3) . . ?
N2 Ni1 N14 98.8(3) . . ?
N8 Ni1 N7 77.9(3) . . ?
N2 Ni1 N7 93.6(3) . . ?
N14 Ni1 N7 165.7(3) . . ?
N8 Ni1 N13 96.3(3) . . ?
N2 Ni1 N13 168.4(3) . . ?
N14 Ni1 N13 77.3(3) . . ?
N7 Ni1 N13 91.8(3) . . ?
N8 Ni1 N1 170.0(3) . . ?
N2 Ni1 N1 77.8(3) . . ?
N14 Ni1 N1 94.0(3) . . ?
N7 Ni1 N1 95.6(3) . . ?
N13 Ni1 N1 91.5(3) . . ?
N11 Ni2 N5 96.3(3) . . ?
N11 Ni2 N17 93.5(3) . . ?
N5 Ni2 N17 96.9(3) . . ?
N11 Ni2 N6 99.5(3) . . ?
N5 Ni2 N6 78.1(3) . . ?
N17 Ni2 N6 166.5(4) . . ?
N11 Ni2 N12 76.7(3) . . ?
N5 Ni2 N12 168.3(4) . . ?
N17 Ni2 N12 92.9(3) . . ?
N6 Ni2 N12 93.6(3) . . ?
N11 Ni2 N18 165.2(4) . . ?
N5 Ni2 N18 96.0(4) . . ?
N17 Ni2 N18 77.0(4) . . ?
N6 Ni2 N18 90.9(4) . . ?
N12 Ni2 N18 92.3(4) . . ?
C1 N1 C5 118.5(9) . . ?
C1 N1 Ni1 126.4(9) . . ?
C5 N1 Ni1 115.1(6) . . ?
C6 N2 N3 106.4(7) . . ?
C6 N2 Ni1 115.6(6) . . ?
N3 N2 Ni1 138.0(5) . . ?
C8 N3 N2 110.8(7) . . ?
C8 N3 H3B 124.6 . . ?
N2 N3 H3B 124.6 . . ?
N5 N4 C15 110.7(8) . . ?
N5 N4 H4B 124.7 . . ?
C15 N4 H4B 124.7 . . ?
N4 N5 C17 108.1(8) . . ?
N4 N5 Ni2 137.0(7) . . ?
C17 N5 Ni2 114.6(7) . . ?
C22 N6 C18 116.8(9) . . ?
C22 N6 Ni2 128.0(8) . . ?
C18 N6 Ni2 114.8(7) . . ?
C27 N7 C23 117.0(9) . . ?
C27 N7 Ni1 115.0(6) . . ?
C23 N7 Ni1 128.0(8) . . ?
N9 N8 C28 104.9(7) . . ?
N9 N8 Ni1 139.5(6) . . ?
C28 N8 Ni1 115.6(6) . . ?
N8 N9 C30 111.2(8) . . ?
N8 N9 H9A 124.4 . . ?
C30 N9 H9A 124.4 . . ?
C37 N10 N11 111.5(7) . . ?
C37 N10 H10B 124.3 . . ?
N11 N10 H10B 124.3 . . ?
C39 N11 N10 105.9(7) . . ?
C39 N11 Ni2 115.5(6) . . ?
N10 N11 Ni2 137.9(5) . . ?
C40 N12 C44 119.0(9) . . ?
C40 N12 Ni2 116.2(7) . . ?
C44 N12 Ni2 124.7(8) . . ?
C49 N13 C45 119.3(9) . . ?
C49 N13 Ni1 114.7(7) . . ?
C45 N13 Ni1 125.3(8) . . ?
C50 N14 N15 106.7(8) . . ?
C50 N14 Ni1 115.3(7) . . ?
N15 N14 Ni1 137.1(6) . . ?
C52 N15 N14 111.3(8) . . ?
C52 N15 H15A 124.3 . . ?
N14 N15 H15A 124.3 . . ?
N17 N16 C59 112.7(8) . . ?
N17 N16 H16B 123.7 . . ?
C59 N16 H16B 123.7 . . ?
C61 N17 N16 106.6(8) . . ?
C61 N17 Ni2 115.4(7) . . ?
N16 N17 Ni2 137.9(7) . . ?
C62 N18 C66 116.8(11) . . ?
C62 N18 Ni2 114.4(7) . . ?
C66 N18 Ni2 128.5(10) . . ?
N1 C1 C2 119.4(13) . . ?
N1 C1 H1A 120.3 . . ?
C2 C1 H1A 120.3 . . ?
C3 C2 C1 120.9(14) . . ?
C3 C2 H2A 119.6 . . ?
C1 C2 H2A 119.6 . . ?
C2 C3 C4 121.6(13) . . ?
C2 C3 H3A 119.2 . . ?
C4 C3 H3A 119.2 . . ?
C5 C4 C3 113.0(16) . . ?
C5 C4 H4A 123.5 . . ?
C3 C4 H4A 123.5 . . ?
C4 C5 N1 125.5(11) . . ?
C4 C5 C6 121.6(12) . . ?
N1 C5 C6 112.8(8) . . ?
N2 C6 C7 110.3(8) . . ?
N2 C6 C5 118.4(8) . . ?
C7 C6 C5 131.2(8) . . ?
C8 C7 C6 104.5(7) . . ?
C8 C7 H7A 127.8 . . ?
C6 C7 H7A 127.8 . . ?
N3 C8 C7 108.0(9) . . ?
N3 C8 C9 121.0(8) . . ?
C7 C8 C9 130.8(8) . . ?
C14 C9 C10 117.0(9) . . ?
C14 C9 C8 121.4(8) . . ?
C10 C9 C8 121.4(8) . . ?
C11 C10 C9 121.6(8) . . ?
C11 C10 H10A 119.2 . . ?
C9 C10 H10A 119.2 . . ?
C12 C11 C10 119.7(9) . . ?
C12 C11 H11A 120.2 . . ?
C10 C11 H11A 120.1 . . ?
C11 C12 C13 120.6(10) . . ?
C11 C12 H12A 119.7 . . ?
C13 C12 H12A 119.7 . . ?
C12 C13 C14 117.8(10) . . ?
C12 C13 C15 121.0(9) . . ?
C14 C13 C15 121.1(8) . . ?
C9 C14 C13 123.2(8) . . ?
C9 C14 H14A 118.4 . . ?
C13 C14 H14A 118.4 . . ?
N4 C15 C16 107.2(9) . . ?
N4 C15 C13 121.8(8) . . ?
C16 C15 C13 131.0(9) . . ?
C15 C16 C17 104.8(8) . . ?
C15 C16 H16A 127.6 . . ?
C17 C16 H16A 127.6 . . ?
N5 C17 C16 109.1(8) . . ?
N5 C17 C18 118.7(10) . . ?
C16 C17 C18 132.3(10) . . ?
C19 C18 N6 123.3(11) . . ?
C19 C18 C17 123.3(12) . . ?
N6 C18 C17 113.3(9) . . ?
C18 C19 C20 123.6(15) . . ?
C18 C19 H19A 118.2 . . ?
C20 C19 H19A 118.2 . . ?
C19 C20 C21 114.0(14) . . ?
C19 C20 H20A 123.0 . . ?
C21 C20 H20A 123.0 . . ?
C22 C21 C20 118.2(12) . . ?
C22 C21 H21A 120.9 . . ?
C20 C21 H21A 120.9 . . ?
N6 C22 C21 123.4(12) . . ?
N6 C22 H22A 118.3 . . ?
C21 C22 H22A 118.3 . . ?
C24 C23 N7 123.8(12) . . ?
C24 C23 H23A 118.1 . . ?
N7 C23 H23A 118.1 . . ?
C23 C24 C25 118.8(12) . . ?
C23 C24 H24A 120.6 . . ?
C25 C24 H24A 120.6 . . ?
C24 C25 C26 119.5(13) . . ?
C24 C25 H25A 120.2 . . ?
C26 C25 H25A 120.2 . . ?
C25 C26 C27 118.6(12) . . ?
C25 C26 H26A 120.7 . . ?
C27 C26 H26A 120.7 . . ?
N7 C27 C26 122.2(9) . . ?
N7 C27 C28 116.1(9) . . ?
C26 C27 C28 121.7(9) . . ?
N8 C28 C29 110.2(8) . . ?
N8 C28 C27 115.2(8) . . ?
C29 C28 C27 134.6(9) . . ?
C30 C29 C28 105.7(9) . . ?
C30 C29 H29A 127.1 . . ?
C28 C29 H29A 127.1 . . ?
N9 C30 C29 108.0(8) . . ?
N9 C30 C31 119.8(9) . . ?
C29 C30 C31 132.2(9) . . ?
C36 C31 C32 121.4(8) . . ?
C36 C31 C30 117.8(8) . . ?
C32 C31 C30 120.8(8) . . ?
C33 C32 C31 118.1(9) . . ?
C33 C32 H32A 121.0 . . ?
C31 C32 H32A 121.0 . . ?
C32 C33 C34 122.0(9) . . ?
C32 C33 H33A 119.0 . . ?
C34 C33 H33A 119.0 . . ?
C35 C34 C33 119.4(9) . . ?
C35 C34 H34A 120.3 . . ?
C33 C34 H34A 120.3 . . ?
C34 C35 C36 120.5(9) . . ?
C34 C35 C37 121.0(8) . . ?
C36 C35 C37 118.4(8) . . ?
C31 C36 C35 118.5(8) . . ?
C31 C36 H36A 120.8 . . ?
C35 C36 H36A 120.8 . . ?
N10 C37 C38 107.3(9) . . ?
N10 C37 C35 122.9(8) . . ?
C38 C37 C35 129.5(9) . . ?
C37 C38 C39 104.5(8) . . ?
C37 C38 H38A 127.7 . . ?
C39 C38 H38A 127.7 . . ?
N11 C39 C38 110.8(8) . . ?
N11 C39 C40 117.0(9) . . ?
C38 C39 C40 132.1(8) . . ?
N12 C40 C41 122.4(10) . . ?
N12 C40 C39 114.2(8) . . ?
C41 C40 C39 123.4(10) . . ?
C42 C41 C40 119.1(12) . . ?
C42 C41 H41A 120.5 . . ?
C40 C41 H41A 120.5 . . ?
C41 C42 C43 119.5(11) . . ?
C41 C42 H42A 120.2 . . ?
C43 C42 H42A 120.2 . . ?
C42 C43 C44 119.8(12) . . ?
C42 C43 H43A 120.1 . . ?
C44 C43 H43A 120.1 . . ?
N12 C44 C43 120.1(13) . . ?
N12 C44 H44A 120.0 . . ?
C43 C44 H44A 120.0 . . ?
N13 C45 C46 122.2(12) . . ?
N13 C45 H45A 118.9 . . ?
C46 C45 H45A 118.9 . . ?
C45 C46 C47 119.8(11) . . ?
C45 C46 H46A 120.1 . . ?
C47 C46 H46A 120.1 . . ?
C48 C47 C46 116.7(11) . . ?
C48 C47 H47A 121.7 . . ?
C46 C47 H47A 121.7 . . ?
C47 C48 C49 118.9(12) . . ?
C47 C48 H48A 120.5 . . ?
C49 C48 H48A 120.5 . . ?
N13 C49 C48 123.1(10) . . ?
N13 C49 C50 114.9(9) . . ?
C48 C49 C50 122.0(11) . . ?
N14 C50 C51 110.9(9) . . ?
N14 C50 C49 116.8(9) . . ?
C51 C50 C49 132.2(9) . . ?
C52 C51 C50 103.1(8) . . ?
C52 C51 H51A 128.5 . . ?
C50 C51 H51A 128.5 . . ?
N15 C52 C51 108.0(9) . . ?
N15 C52 C53 123.3(9) . . ?
C51 C52 C53 128.5(9) . . ?
C58 C53 C54 118.3(9) . . ?
C58 C53 C52 119.8(9) . . ?
C54 C53 C52 121.8(9) . . ?
C55 C54 C53 118.1(10) . . ?
C55 C54 H54A 121.0 . . ?
C53 C54 H54A 121.0 . . ?
C56 C55 C54 123.6(10) . . ?
C56 C55 H55A 118.2 . . ?
C54 C55 H55A 118.2 . . ?
C55 C56 C57 120.1(11) . . ?
C55 C56 H56A 119.9 . . ?
C57 C56 H56A 119.9 . . ?
C56 C57 C58 117.7(10) . . ?
C56 C57 C59 123.6(10) . . ?
C58 C57 C59 118.6(9) . . ?
C53 C58 C57 122.0(9) . . ?
C53 C58 H58A 119.0 . . ?
C57 C58 H58A 119.0 . . ?
N16 C59 C60 106.7(9) . . ?
N16 C59 C57 123.0(10) . . ?
C60 C59 C57 130.4(10) . . ?
C59 C60 C61 103.7(9) . . ?
C59 C60 H60A 128.2 . . ?
C61 C60 H60A 128.2 . . ?
N17 C61 C60 110.3(9) . . ?
N17 C61 C62 117.1(9) . . ?
C60 C61 C62 132.6(10) . . ?
N18 C62 C63 124.9(11) . . ?
N18 C62 C61 115.3(10) . . ?
C63 C62 C61 119.8(11) . . ?
C64 C63 C62 118.6(14) . . ?
C64 C63 H63A 120.7 . . ?
C62 C63 H63A 120.7 . . ?
C63 C64 C65 117.2(13) . . ?
C63 C64 H64A 121.4 . . ?
C65 C64 H64A 121.4 . . ?
C66 C65 C64 119.7(12) . . ?
C66 C65 H65A 120.2 . . ?
C64 C65 H65A 120.2 . . ?
C65 C66 N18 122.7(15) . . ?
C65 C66 H66A 118.6 . . ?
N18 C66 H66A 118.6 . . ?
O1W Br3C Br1 118.0(8) . . ?
F2 B1 F3 114.0(9) . . ?
F2 B1 F4 112.8(11) . . ?
F3 B1 F4 107.6(9) . . ?
F2 B1 F1 108.9(8) . . ?
F3 B1 F1 106.7(10) . . ?
F4 B1 F1 106.4(8) . . ?
C1S O1S H1S 119.6 . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 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 N8 2.076(8) . ?
Ni1 N2 2.080(8) . ?
Ni1 N14 2.092(8) . ?
Ni1 N7 2.101(9) . ?
Ni1 N13 2.125(8) . ?
Ni1 N1 2.131(8) . ?
Ni2 N11 2.085(8) . ?
Ni2 N5 2.096(9) . ?
Ni2 N17 2.096(8) . ?
Ni2 N6 2.117(9) . ?
Ni2 N12 2.128(8) . ?
Ni2 N18 2.141(9) . ?
N1 C1 1.362(14) . ?
N1 C5 1.387(14) . ?
N2 C6 1.337(11) . ?
N2 N3 1.364(11) . ?
N3 C8 1.348(12) . ?
N3 H3B 0.8800 . ?
N4 N5 1.322(11) . ?
N4 C15 1.356(13) . ?
N4 H4B 0.8800 . ?
N5 C17 1.336(14) . ?
N6 C22 1.350(13) . ?
N6 C18 1.387(15) . ?
N7 C27 1.345(13) . ?
N7 C23 1.373(13) . ?
N8 N9 1.337(10) . ?
N8 C28 1.363(12) . ?
N9 C30 1.341(13) . ?
N9 H9A 0.8800 . ?
N10 C37 1.352(12) . ?
N10 N11 1.367(11) . ?
N10 H10B 0.8800 . ?
N11 C39 1.337(12) . ?
N12 C40 1.326(15) . ?
N12 C44 1.372(14) . ?
N13 C49 1.324(15) . ?
N13 C45 1.351(14) . ?
N14 C50 1.315(13) . ?
N14 N15 1.328(12) . ?
N15 C52 1.322(13) . ?
N15 H15A 0.8800 . ?
N16 N17 1.329(12) . ?
N16 C59 1.333(13) . ?
N16 H16B 0.8800 . ?
N17 C61 1.314(14) . ?
N18 C62 1.325(17) . ?
N18 C66 1.361(16) . ?
C1 C2 1.439(19) . ?
C1 H1A 0.9500 . ?
C2 C3 1.32(3) . ?
C2 H2A 0.9500 . ?
C3 C4 1.49(3) . ?
C3 H3A 0.9500 . ?
C4 C5 1.380(17) . ?
C4 H4A 0.9500 . ?
C5 C6 1.467(13) . ?
C6 C7 1.417(15) . ?
C7 C8 1.391(13) . ?
C7 H7A 0.9500 . ?
C8 C9 1.449(14) . ?
C9 C14 1.363(12) . ?
C9 C10 1.412(12) . ?
C10 C11 1.379(16) . ?
C10 H10A 0.9500 . ?
C11 C12 1.375(16) . ?
C11 H11A 0.9500 . ?
C12 C13 1.397(13) . ?
C12 H12A 0.9500 . ?
C13 C14 1.401(13) . ?
C13 C15 1.457(15) . ?
C14 H14A 0.9500 . ?
C15 C16 1.388(13) . ?
C16 C17 1.411(15) . ?
C16 H16A 0.9500 . ?
C17 C18 1.463(15) . ?
C18 C19 1.317(18) . ?
C19 C20 1.38(2) . ?
C19 H19A 0.9500 . ?
C20 C21 1.50(3) . ?
C20 H20A 0.9500 . ?
C21 C22 1.388(19) . ?
C21 H21A 0.9500 . ?
C22 H22A 0.9500 . ?
C23 C24 1.36(2) . ?
C23 H23A 0.9500 . ?
C24 C25 1.37(2) . ?
C24 H24A 0.9500 . ?
C25 C26 1.396(19) . ?
C25 H25A 0.9500 . ?
C26 C27 1.401(16) . ?
C26 H26A 0.9500 . ?
C27 C28 1.454(13) . ?
C28 C29 1.373(13) . ?
C29 C30 1.353(15) . ?
C29 H29A 0.9500 . ?
C30 C31 1.507(12) . ?
C31 C36 1.376(14) . ?
C31 C32 1.426(12) . ?
C32 C33 1.361(15) . ?
C32 H32A 0.9500 . ?
C33 C34 1.389(17) . ?
C33 H33A 0.9500 . ?
C34 C35 1.386(14) . ?
C34 H34A 0.9500 . ?
C35 C36 1.410(11) . ?
C35 C37 1.475(14) . ?
C36 H36A 0.9500 . ?
C37 C38 1.398(13) . ?
C38 C39 1.419(14) . ?
C38 H38A 0.9500 . ?
C39 C40 1.460(15) . ?
C40 C41 1.395(13) . ?
C41 C42 1.364(19) . ?
C41 H41A 0.9500 . ?
C42 C43 1.37(2) . ?
C42 H42A 0.9500 . ?
C43 C44 1.401(19) . ?
C43 H43A 0.9500 . ?
C44 H44A 0.9500 . ?
C45 C46 1.365(17) . ?
C45 H45A 0.9500 . ?
C46 C47 1.46(2) . ?
C46 H46A 0.9500 . ?
C47 C48 1.380(19) . ?
C47 H47A 0.9500 . ?
C48 C49 1.423(15) . ?
C48 H48A 0.9500 . ?
C49 C50 1.473(15) . ?
C50 C51 1.399(15) . ?
C51 C52 1.393(15) . ?
C51 H51A 0.9500 . ?
C52 C53 1.468(15) . ?
C53 C58 1.392(14) . ?
C53 C54 1.435(14) . ?
C54 C55 1.383(19) . ?
C54 H54A 0.9500 . ?
C55 C56 1.36(2) . ?
C55 H55A 0.9500 . ?
C56 C57 1.402(15) . ?
C56 H56A 0.9500 . ?
C57 C58 1.422(15) . ?
C57 C59 1.447(15) . ?
C58 H58A 0.9500 . ?
C59 C60 1.396(15) . ?
C60 C61 1.426(15) . ?
C60 H60A 0.9500 . ?
C61 C62 1.472(15) . ?
C62 C63 1.409(18) . ?
C63 C64 1.35(2) . ?
C63 H63A 0.9500 . ?
C64 C65 1.45(3) . ?
C64 H64A 0.9500 . ?
C65 C66 1.36(2) . ?
C65 H65A 0.9500 . ?
C66 H66A 0.9500 . ?
Br1 Br3C 2.423(10) . ?
Br3C O1W 1.98(2) . ?
B1 F2 1.336(12) . ?
B1 F3 1.389(13) . ?
B1 F4 1.397(12) . ?
B1 F1 1.433(12) . ?
O1S C1S 1.26(4) . ?
O1S H1S 0.9123 . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3B Br2 0.88 2.64 3.351(8) 138.8 . yes
N4 H4B O1W 0.88 2.43 3.11(2) 135.5 . yes
N9 H9A O5W 0.88 2.23 2.938(18) 137.0 . yes
N10 H10B Br3A^a 0.88 2.46 3.215(9) 143.9 . yes
N15 H15A Br3C^c 0.88 2.57 3.439(13) 167.4 . yes
N16 H16B O1S 0.88 2.07 2.85(2) 147.1 . yes
N16 H16B Br1 0.88 2.82 3.407(8) 125.3 . yes
O1S H1S O5W 0.91 2.06 2.88(3) 150.4 . yes
