#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/57/2205757.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2205757
loop_
_publ_author_name
'Annie Michaud'
'Frédéric-Georges Fontaine'
'Davit Zargarian'
_publ_section_title
;[Bis[tris(3,5-dimethylpyrazolyl)methane]nickel(II)][tetrachloronickelate(II)]--methanol--water
 (1/1/1)
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m904
_journal_page_last               m906
_journal_paper_doi               10.1107/S1600536805011128
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Ni (C16 H22 N6)2] [Ni Cl4] , C H4 O , H2 O'
_chemical_formula_moiety
'C32 H44 N12 Ni 2+ , Cl4 Ni 2- , C H4 O , H2 O'
_chemical_formula_sum            'C33 H50 Cl4 N12 Ni2 O2'
_chemical_formula_weight         906.07
_chemical_name_systematic
;
[Bis[tris(3,5-dimethylpyrazolyl)methane]nickel(II)][tetrachloronickel(II)]
methanol water solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.1180(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2998(2)
_cell_length_b                   18.5245(3)
_cell_length_c                   21.9660(3)
_cell_measurement_reflns_used    36297
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      72.60
_cell_measurement_theta_min      2.38
_cell_volume                     4180.26(12)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'UdMX (local program)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      220(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART 2K/Platform CCD area-detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0913
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            49482
_diffrn_reflns_theta_full        72.59
_diffrn_reflns_theta_max         72.59
_diffrn_reflns_theta_min         3.12
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  60
_diffrn_standards_number         376
_exptl_absorpt_coefficient_mu    3.846
_exptl_absorpt_correction_T_max  0.7395
_exptl_absorpt_correction_T_min  0.2871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1899
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.050
_refine_diff_density_min         -0.569
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8242
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.1017P)²+0.294P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1523
_refine_ls_wR_factor_ref         0.1561
_reflns_number_gt                7048
_reflns_number_total             8242
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            lh6402.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2205757
_cod_database_fobs_code          2205757
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Ni1 1.0000 0.5000 0.5000 0.02969(10) Uani d S 1 Ni
N1 0.84141(15) 0.44415(9) 0.45692(7) 0.0361(4) Uani d . 1 N
N2 0.75964(14) 0.41052(8) 0.49442(7) 0.0320(3) Uani d . 1 N
N3 0.97738(14) 0.59002(9) 0.44310(7) 0.0365(4) Uani d . 1 N
N4 1.08906(14) 0.61892(8) 0.42337(7) 0.0317(3) Uani d . 1 N
N5 1.13211(15) 0.46284(8) 0.43795(7) 0.0364(4) Uani d . 1 N
N6 1.21832(14) 0.51278(8) 0.41874(7) 0.0311(3) Uani d . 1 N
C1 0.8539(3) 0.45594(17) 0.34510(10) 0.0682(8) Uani d . 1 C
H1A 0.9355 0.4799 0.3572 0.102 Uiso calc R 1 H
H1B 0.7962 0.4895 0.3227 0.102 Uiso calc R 1 H
H1C 0.8704 0.4149 0.3193 0.102 Uiso calc R 1 H
C2 0.7919(2) 0.43049(12) 0.40067(9) 0.0441(5) Uani d . 1 C
C3 0.6785(2) 0.38900(12) 0.40213(9) 0.0455(5) Uani d . 1 C
H3 0.6253 0.3728 0.3683 0.055 Uiso calc R 1 H
C4 0.66017(17) 0.37659(11) 0.46202(9) 0.0375(4) Uani d . 1 C
C5 0.5570(2) 0.33501(14) 0.49058(11) 0.0559(6) Uani d . 1 C
H5A 0.5971 0.2994 0.5184 0.084 Uiso calc R 1 H
H5B 0.5024 0.3108 0.4591 0.084 Uiso calc R 1 H
H5C 0.5043 0.3677 0.5130 0.084 Uiso calc R 1 H
C6 1.0915(3) 0.33253(12) 0.42014(14) 0.0629(7) Uani d . 1 C
H6A 1.0200 0.3417 0.4455 0.094 Uiso calc R 1 H
H6B 1.1495 0.2969 0.4397 0.094 Uiso calc R 1 H
H6C 1.0576 0.3145 0.3807 0.094 Uiso calc R 1 H
C7 1.1650(2) 0.40132(11) 0.41166(10) 0.0424(5) Uani d . 1 C
C8 1.2721(2) 0.41145(11) 0.37708(9) 0.0418(5) Uani d . 1 C
H8 1.3136 0.3761 0.3547 0.050 Uiso calc R 1 H
C9 1.30475(18) 0.48283(11) 0.38218(8) 0.0358(4) Uani d . 1 C
C10 1.4092(2) 0.52464(13) 0.35493(11) 0.0525(6) Uani d . 1 C
H10A 1.3712 0.5657 0.3328 0.079 Uiso calc R 1 H
H10B 1.4531 0.4940 0.3271 0.079 Uiso calc R 1 H
H10C 1.4713 0.5415 0.3871 0.079 Uiso calc R 1 H
C11 0.7432(2) 0.61966(16) 0.43184(14) 0.0678(8) Uani d . 1 C
H11A 0.7298 0.5685 0.4383 0.102 Uiso calc R 1 H
H11B 0.6878 0.6356 0.3968 0.102 Uiso calc R 1 H
H11C 0.7214 0.6463 0.4678 0.102 Uiso calc R 1 H
C12 0.8825(2) 0.63294(12) 0.42041(10) 0.0444(5) Uani d . 1 C
C13 0.9332(2) 0.68830(12) 0.38660(10) 0.0490(5) Uani d . 1 C
H13 0.8857 0.7253 0.3659 0.059 Uiso calc R 1 H
C14 1.0652(2) 0.67893(10) 0.38914(8) 0.0385(4) Uani d . 1 C
C15 1.1701(3) 0.71997(12) 0.36165(12) 0.0564(6) Uani d . 1 C
H15A 1.2313 0.7379 0.3938 0.085 Uiso calc R 1 H
H15B 1.1324 0.7603 0.3384 0.085 Uiso calc R 1 H
H15C 1.2151 0.6885 0.3348 0.085 Uiso calc R 1 H
C16 1.21270(16) 0.58590(9) 0.44066(8) 0.0293(4) Uani d . 1 C
H16 1.2806 0.6139 0.4214 0.035 Uiso calc R 1 H
Ni2 1.0000 0.5000 0.0000 0.03056(10) Uani d S 1 Ni
N21 0.99622(14) 0.45153(9) 0.08592(7) 0.0349(3) Uani d . 1 N
N22 1.11431(14) 0.43399(8) 0.11478(7) 0.0327(3) Uani d . 1 N
N23 1.15014(15) 0.56432(8) 0.04077(7) 0.0355(4) Uani d . 1 N
N24 1.24117(14) 0.53040(8) 0.07845(7) 0.0326(3) Uani d . 1 N
N25 0.85380(15) 0.57610(9) 0.01538(7) 0.0359(4) Uani d . 1 N
N26 0.75850(14) 0.58431(8) -0.03054(7) 0.0339(3) Uani d . 1 N
C21 0.7660(2) 0.43614(15) 0.10752(12) 0.0551(6) Uani d . 1 C
H21A 0.7371 0.4821 0.1229 0.083 Uiso calc R 1 H
H21B 0.7200 0.3972 0.1263 0.083 Uiso calc R 1 H
H21C 0.7480 0.4344 0.0636 0.083 Uiso calc R 1 H
C22 0.90868(18) 0.42801(11) 0.12266(9) 0.0378(4) Uani d . 1 C
C23 0.9693(2) 0.39611(12) 0.17472(9) 0.0416(5) Uani d . 1 C
H23 0.9281 0.3759 0.2075 0.050 Uiso calc R 1 H
C24 1.1004(2) 0.39999(11) 0.16884(8) 0.0384(4) Uani d . 1 C
C25 1.2136(2) 0.37426(15) 0.20925(11) 0.0615(7) Uani d . 1 C
H25A 1.2688 0.3440 0.1860 0.092 Uiso calc R 1 H
H25B 1.1825 0.3466 0.2428 0.092 Uiso calc R 1 H
H25C 1.2632 0.4154 0.2253 0.092 Uiso calc R 1 H
C26 1.1081(2) 0.69081(12) 0.00798(12) 0.0537(6) Uani d . 1 C
H26A 1.0920 0.6758 -0.0342 0.081 Uiso calc R 1 H
H26B 1.1566 0.7357 0.0096 0.081 Uiso calc R 1 H
H26C 1.0257 0.6978 0.0260 0.081 Uiso calc R 1 H
C27 1.1847(2) 0.63414(11) 0.04262(9) 0.0394(4) Uani d . 1 C
C28 1.2973(2) 0.64331(11) 0.08114(10) 0.0433(5) Uani d . 1 C
H28 1.3407 0.6871 0.0901 0.052 Uiso calc R 1 H
C29 1.33216(18) 0.57706(11) 0.10331(9) 0.0379(4) Uani d . 1 C
C30 1.4421(2) 0.55469(13) 0.14730(12) 0.0541(6) Uani d . 1 C
H30A 1.4081 0.5285 0.1810 0.081 Uiso calc R 1 H
H30B 1.4885 0.5972 0.1628 0.081 Uiso calc R 1 H
H30C 1.5011 0.5238 0.1267 0.081 Uiso calc R 1 H
C31 0.8930(3) 0.62224(14) 0.12066(10) 0.0580(6) Uani d . 1 C
H31A 0.9708 0.5928 0.1198 0.087 Uiso calc R 1 H
H31B 0.8414 0.6057 0.1532 0.087 Uiso calc R 1 H
H31C 0.9176 0.6722 0.1278 0.087 Uiso calc R 1 H
C32 0.8154(2) 0.61600(11) 0.06126(9) 0.0414(5) Uani d . 1 C
C33 0.6957(2) 0.64820(13) 0.04463(10) 0.0482(5) Uani d . 1 C
H33 0.6481 0.6785 0.0691 0.058 Uiso calc R 1 H
C34 0.66092(19) 0.62771(11) -0.01338(10) 0.0437(5) Uani d . 1 C
C35 0.5422(2) 0.64314(17) -0.05376(14) 0.0706(8) Uani d . 1 C
H35A 0.5633 0.6769 -0.0853 0.106 Uiso calc R 1 H
H35B 0.4760 0.6639 -0.0298 0.106 Uiso calc R 1 H
H35C 0.5098 0.5986 -0.0725 0.106 Uiso calc R 1 H
C36 0.76798(17) 0.54663(10) -0.08759(8) 0.0317(4) Uani d . 1 C
H36 0.6935 0.5616 -0.1158 0.038 Uiso calc R 1 H
Ni3 0.42641(4) 0.77631(2) 0.245018(15) 0.04356(9) Uani d . 1 Ni
Cl1 0.49993(7) 0.71671(4) 0.33024(3) 0.07339(19) Uani d . 1 Cl
Cl2 0.21731(6) 0.75424(4) 0.20784(3) 0.06300(17) Uani d . 1 Cl
Cl3 0.55720(6) 0.75212(3) 0.16896(3) 0.05183(14) Uani d . 1 Cl
Cl4 0.43912(6) 0.89555(3) 0.26514(3) 0.05340(14) Uani d . 1 Cl
C97 0.0810(3) 0.56757(17) 0.25579(12) 0.0685(8) Uani d D 1 C
H97A 0.1145 0.5600 0.2977 0.103 Uiso calc R 1 H
H97B 0.0296 0.5261 0.2419 0.103 Uiso calc R 1 H
H97C 0.0268 0.6105 0.2534 0.103 Uiso calc R 1 H
O97 0.1815(3) 0.57619(15) 0.22006(15) 0.1196(10) Uani d D 1 O
H97D 0.1956 0.6199 0.2155 0.179 Uiso calc RD 1 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N3 Ni1 N3 . 3_766 180 y
N3 Ni1 N1 . 3_766 85.76(6) y
N3 Ni1 N1 3_766 3_766 94.24(6) ?
N3 Ni1 N1 . . 94.24(6) y
N3 Ni1 N1 3_766 . 85.76(6) ?
N1 Ni1 N1 3_766 . 180 y
N3 Ni1 N5 . 3_766 94.40(6) y
N3 Ni1 N5 3_766 3_766 85.60(6) ?
N1 Ni1 N5 3_766 3_766 93.73(6) ?
N1 Ni1 N5 . 3_766 86.27(6) ?
N3 Ni1 N5 . . 85.59(6) y
N3 Ni1 N5 3_766 . 94.40(6) ?
N1 Ni1 N5 3_766 . 86.27(6) y
N1 Ni1 N5 . . 93.73(6) y
N5 Ni1 N5 3_766 . 180 y
C2 N1 N2 . . 105.14(15) ?
C2 N1 Ni1 . . 138.43(13) ?
N2 N1 Ni1 . . 116.43(11) ?
C4 N2 N1 . . 111.63(15) ?
C4 N2 C16 . 3_766 129.05(15) ?
N1 N2 C16 . 3_766 119.32(14) ?
C12 N3 N4 . . 105.03(15) ?
C12 N3 Ni1 . . 138.63(14) ?
N4 N3 Ni1 . . 116.26(11) ?
C14 N4 N3 . . 111.97(15) ?
C14 N4 C16 . . 128.10(16) ?
N3 N4 C16 . . 119.91(14) ?
C7 N5 N6 . . 104.70(15) ?
C7 N5 Ni1 . . 139.02(14) ?
N6 N5 Ni1 . . 116.18(11) ?
C9 N6 N5 . . 111.89(15) ?
C9 N6 C16 . . 128.69(15) ?
N5 N6 C16 . . 119.33(14) ?
C2 C1 H1A . . 109.5 ?
C2 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
C2 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
N1 C2 C3 . . 110.43(18) ?
N1 C2 C1 . . 122.81(19) ?
C3 C2 C1 . . 126.75(19) ?
C4 C3 C2 . . 106.76(17) ?
C4 C3 H3 . . 126.6 ?
C2 C3 H3 . . 126.6 ?
N2 C4 C3 . . 106.04(16) ?
N2 C4 C5 . . 123.59(18) ?
C3 C4 C5 . . 130.37(18) ?
C4 C5 H5A . . 109.5 ?
C4 C5 H5B . . 109.5 ?
H5A C5 H5B . . 109.5 ?
C4 C5 H5C . . 109.5 ?
H5A C5 H5C . . 109.5 ?
H5B C5 H5C . . 109.5 ?
C7 C6 H6A . . 109.5 ?
C7 C6 H6B . . 109.5 ?
H6A C6 H6B . . 109.5 ?
C7 C6 H6C . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
N5 C7 C8 . . 110.86(18) ?
N5 C7 C6 . . 121.8(2) ?
C8 C7 C6 . . 127.4(2) ?
C9 C8 C7 . . 106.54(17) ?
C9 C8 H8 . . 126.7 ?
C7 C8 H8 . . 126.7 ?
N6 C9 C8 . . 106.00(17) ?
N6 C9 C10 . . 123.29(18) ?
C8 C9 C10 . . 130.71(18) ?
C9 C10 H10A . . 109.5 ?
C9 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
C9 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
C12 C11 H11A . . 109.5 ?
C12 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
C12 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
N3 C12 C13 . . 110.37(18) ?
N3 C12 C11 . . 121.8(2) ?
C13 C12 C11 . . 127.8(2) ?
C14 C13 C12 . . 107.14(18) ?
C14 C13 H13 . . 126.4 ?
C12 C13 H13 . . 126.4 ?
N4 C14 C13 . . 105.48(17) ?
N4 C14 C15 . . 122.54(19) ?
C13 C14 C15 . . 131.97(19) ?
C14 C15 H15A . . 109.5 ?
C14 C15 H15B . . 109.5 ?
H15A C15 H15B . . 109.5 ?
C14 C15 H15C . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
N2 C16 N4 3_766 . 110.57(14) ?
N2 C16 N6 3_766 . 111.44(14) ?
N4 C16 N6 . . 111.57(14) ?
N2 C16 H16 3_766 . 107.7 ?
N4 C16 H16 . . 107.7 ?
N6 C16 H16 . . 107.7 ?
N21 Ni2 N21 . 3_765 180 y
N21 Ni2 N23 . 3_765 94.60(6) y
N21 Ni2 N23 3_765 3_765 85.40(6) ?
N21 Ni2 N23 . . 85.39(6) y
N21 Ni2 N23 3_765 . 94.61(6) ?
N23 Ni2 N23 3_765 . 180 y
N21 Ni2 N25 . . 94.74(6) y
N21 Ni2 N25 3_765 . 85.26(6) y
N23 Ni2 N25 3_765 . 86.28(6) y
N23 Ni2 N25 . . 93.72(6) y
N21 Ni2 N25 . 3_765 85.26(6) ?
N21 Ni2 N25 3_765 3_765 94.74(6) ?
N23 Ni2 N25 3_765 3_765 93.71(6) ?
N23 Ni2 N25 . 3_765 86.28(6) ?
N25 Ni2 N25 . 3_765 180 y
C22 N21 N22 . . 105.09(15) ?
C22 N21 Ni2 . . 138.35(13) ?
N22 N21 Ni2 . . 116.47(11) ?
C24 N22 N21 . . 111.62(15) ?
C24 N22 C36 . 3_765 128.59(15) ?
N21 N22 C36 . 3_765 119.78(14) ?
C27 N23 N24 . . 104.91(15) ?
C27 N23 Ni2 . . 138.19(13) ?
N24 N23 Ni2 . . 116.86(11) ?
N23 N24 C29 . . 112.08(15) ?
N23 N24 C36 . 3_765 119.48(14) ?
C29 N24 C36 . 3_765 128.44(15) ?
C32 N25 N26 . . 105.11(15) ?
C32 N25 Ni2 . . 138.29(13) ?
N26 N25 Ni2 . . 116.12(11) ?
C34 N26 N25 . . 111.55(16) ?
C34 N26 C36 . . 128.55(16) ?
N25 N26 C36 . . 119.86(14) ?
C22 C21 H21A . . 109.5 ?
C22 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
C22 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
N21 C22 C23 . . 110.74(17) ?
N21 C22 C21 . . 122.25(18) ?
C23 C22 C21 . . 127.01(19) ?
C24 C23 C22 . . 106.71(17) ?
C24 C23 H23 . . 126.6 ?
C22 C23 H23 . . 126.6 ?
N22 C24 C23 . . 105.85(17) ?
N22 C24 C25 . . 122.73(19) ?
C23 C24 C25 . . 131.42(19) ?
C24 C25 H25A . . 109.5 ?
C24 C25 H25B . . 109.5 ?
H25A C25 H25B . . 109.5 ?
C24 C25 H25C . . 109.5 ?
H25A C25 H25C . . 109.5 ?
H25B C25 H25C . . 109.5 ?
C27 C26 H26A . . 109.5 ?
C27 C26 H26B . . 109.5 ?
H26A C26 H26B . . 109.5 ?
C27 C26 H26C . . 109.5 ?
H26A C26 H26C . . 109.5 ?
H26B C26 H26C . . 109.5 ?
N23 C27 C28 . . 110.04(17) ?
N23 C27 C26 . . 122.31(18) ?
C28 C27 C26 . . 127.64(19) ?
C29 C28 C27 . . 107.10(18) ?
C29 C28 H28 . . 126.4 ?
C27 C28 H28 . . 126.4 ?
C28 C29 N24 . . 105.85(17) ?
C28 C29 C30 . . 130.62(19) ?
N24 C29 C30 . . 123.50(18) ?
C29 C30 H30A . . 109.5 ?
C29 C30 H30B . . 109.5 ?
H30A C30 H30B . . 109.5 ?
C29 C30 H30C . . 109.5 ?
H30A C30 H30C . . 109.5 ?
H30B C30 H30C . . 109.5 ?
C32 C31 H31A . . 109.5 ?
C32 C31 H31B . . 109.5 ?
H31A C31 H31B . . 109.5 ?
C32 C31 H31C . . 109.5 ?
H31A C31 H31C . . 109.5 ?
H31B C31 H31C . . 109.5 ?
N25 C32 C33 . . 110.11(18) ?
N25 C32 C31 . . 122.51(19) ?
C33 C32 C31 . . 127.37(19) ?
C34 C33 C32 . . 107.23(18) ?
C34 C33 H33 . . 126.4 ?
C32 C33 H33 . . 126.4 ?
C33 C34 N26 . . 105.99(18) ?
C33 C34 C35 . . 131.2(2) ?
N26 C34 C35 . . 122.7(2) ?
C34 C35 H35A . . 109.5 ?
C34 C35 H35B . . 109.5 ?
H35A C35 H35B . . 109.5 ?
C34 C35 H35C . . 109.5 ?
H35A C35 H35C . . 109.5 ?
H35B C35 H35C . . 109.5 ?
N22 C36 N26 3_765 . 110.62(14) ?
N22 C36 N24 3_765 3_765 111.74(14) ?
N26 C36 N24 . 3_765 110.34(15) ?
N22 C36 H36 3_765 . 108.0 ?
N26 C36 H36 . . 108.0 ?
N24 C36 H36 3_765 . 108.0 ?
Cl4 Ni3 Cl1 . . 107.78(3) y
Cl4 Ni3 Cl3 . . 108.01(2) y
Cl1 Ni3 Cl3 . . 109.46(3) y
Cl4 Ni3 Cl2 . . 106.58(3) y
Cl1 Ni3 Cl2 . . 117.42(3) y
Cl3 Ni3 Cl2 . . 107.24(3) y
O97 C97 H97A . . 109.5 ?
O97 C97 H97B . . 109.5 ?
H97A C97 H97B . . 109.5 ?
O97 C97 H97C . . 109.5 ?
H97A C97 H97C . . 109.5 ?
H97B C97 H97C . . 109.5 ?
C97 O97 H97D . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 N3 . 2.0870(16) y
Ni1 N3 3_766 2.0870(16) ?
Ni1 N1 3_766 2.1004(15) ?
Ni1 N1 . 2.1004(15) y
Ni1 N5 3_766 2.1094(16) ?
Ni1 N5 . 2.1094(16) y
N1 C2 . 1.327(2) y
N1 N2 . 1.369(2) y
N2 C4 . 1.359(2) ?
N2 C16 3_766 1.436(2) ?
N3 C12 . 1.328(2) y
N3 N4 . 1.367(2) y
N4 C14 . 1.355(2) y
N4 C16 . 1.439(2) ?
N5 C7 . 1.332(2) y
N5 N6 . 1.370(2) y
N6 C9 . 1.359(2) y
N6 C16 . 1.440(2) ?
C1 C2 . 1.494(3) ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
C1 H1C . 0.9700 ?
C2 C3 . 1.400(3) y
C3 C4 . 1.362(3) y
C3 H3 . 0.9400 ?
C4 C5 . 1.487(3) ?
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
C5 H5C . 0.9700 ?
C6 C7 . 1.501(3) ?
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
C6 H6C . 0.9700 ?
C7 C8 . 1.397(3) ?
C8 C9 . 1.367(3) ?
C8 H8 . 0.9400 ?
C9 C10 . 1.486(3) ?
C10 H10A . 0.9700 ?
C10 H10B . 0.9700 ?
C10 H10C . 0.9700 ?
C11 C12 . 1.496(3) ?
C11 H11A . 0.9700 ?
C11 H11B . 0.9700 ?
C11 H11C . 0.9700 ?
C12 C13 . 1.390(3) y
C13 C14 . 1.368(3) y
C13 H13 . 0.9400 ?
C14 C15 . 1.484(3) ?
C15 H15A . 0.9700 ?
C15 H15B . 0.9700 ?
C15 H15C . 0.9700 ?
C16 N2 3_766 1.436(2) ?
C16 H16 . 0.9900 ?
Ni2 N21 . 2.0929(16) y
Ni2 N21 3_765 2.0929(16) ?
Ni2 N23 3_765 2.1010(15) ?
Ni2 N23 . 2.1010(15) y
Ni2 N25 . 2.1076(15) y
Ni2 N25 3_765 2.1077(15) ?
N21 C22 . 1.326(2) y
N21 N22 . 1.370(2) y
N22 C24 . 1.361(2) y
N22 C36 3_765 1.435(2) ?
N23 C27 . 1.341(3) y
N23 N24 . 1.359(2) y
N24 C29 . 1.360(2) y
N24 C36 3_765 1.445(2) ?
N25 C32 . 1.332(2) y
N25 N26 . 1.365(2) y
N26 C34 . 1.361(2) y
N26 C36 . 1.444(2) ?
C21 C22 . 1.491(3) ?
C21 H21A . 0.9700 ?
C21 H21B . 0.9700 ?
C21 H21C . 0.9700 ?
C22 C23 . 1.395(3) y
C23 C24 . 1.368(3) y
C23 H23 . 0.9400 ?
C24 C25 . 1.492(3) ?
C25 H25A . 0.9700 ?
C25 H25B . 0.9700 ?
C25 H25C . 0.9700 ?
C26 C27 . 1.489(3) ?
C26 H26A . 0.9700 ?
C26 H26B . 0.9700 ?
C26 H26C . 0.9700 ?
C27 C28 . 1.396(3) y
C28 C29 . 1.359(3) y
C28 H28 . 0.9400 ?
C29 C30 . 1.494(3) ?
C30 H30A . 0.9700 ?
C30 H30B . 0.9700 ?
C30 H30C . 0.9700 ?
C31 C32 . 1.485(3) ?
C31 H31A . 0.9700 ?
C31 H31B . 0.9700 ?
C31 H31C . 0.9700 ?
C32 C33 . 1.394(3) y
C33 C34 . 1.353(3) y
C33 H33 . 0.9400 ?
C34 C35 . 1.486(3) ?
C35 H35A . 0.9700 ?
C35 H35B . 0.9700 ?
C35 H35C . 0.9700 ?
C36 N22 3_765 1.435(2) ?
C36 N24 3_765 1.445(2) ?
C36 H36 . 0.9900 ?
Ni3 Cl4 . 2.2547(7) y
Ni3 Cl1 . 2.2568(7) y
Ni3 Cl3 . 2.2649(7) y
Ni3 Cl2 . 2.2847(7) y
C97 O97 . 1.353(4) ?
C97 H97A . 0.9700 ?
C97 H97B . 0.9700 ?
C97 H97C . 0.9700 ?
O97 H97D . 0.8300 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
N3 Ni1 N1 C2 . . 43.6(2)
N3 Ni1 N1 C2 3_766 . -136.4(2)
N5 Ni1 N1 C2 3_766 . 137.7(2)
N5 Ni1 N1 C2 . . -42.3(2)
N3 Ni1 N1 N2 . . -136.12(13)
N3 Ni1 N1 N2 3_766 . 43.88(13)
N5 Ni1 N1 N2 3_766 . -41.98(13)
N5 Ni1 N1 N2 . . 138.03(13)
C2 N1 N2 C4 . . -0.2(2)
Ni1 N1 N2 C4 . . 179.54(12)
C2 N1 N2 C16 . 3_766 179.16(17)
Ni1 N1 N2 C16 . 3_766 -1.1(2)
N1 Ni1 N3 C12 3_766 . -133.9(2)
N1 Ni1 N3 C12 . . 46.1(2)
N5 Ni1 N3 C12 3_766 . -40.4(2)
N5 Ni1 N3 C12 . . 139.6(2)
N1 Ni1 N3 N4 3_766 . 42.24(13)
N1 Ni1 N3 N4 . . -137.76(13)
N5 Ni1 N3 N4 3_766 . 135.66(13)
N5 Ni1 N3 N4 . . -44.34(13)
C12 N3 N4 C14 . . 0.2(2)
Ni1 N3 N4 C14 . . -177.12(12)
C12 N3 N4 C16 . . 179.07(16)
Ni1 N3 N4 C16 . . 1.7(2)
N3 Ni1 N5 C7 . . -140.3(2)
N3 Ni1 N5 C7 3_766 . 39.7(2)
N1 Ni1 N5 C7 3_766 . 133.7(2)
N1 Ni1 N5 C7 . . -46.3(2)
N3 Ni1 N5 N6 . . 44.03(12)
N3 Ni1 N5 N6 3_766 . -135.97(12)
N1 Ni1 N5 N6 3_766 . -41.99(12)
N1 Ni1 N5 N6 . . 138.01(12)
C7 N5 N6 C9 . . -1.1(2)
Ni1 N5 N6 C9 . . 175.94(12)
C7 N5 N6 C16 . . -177.99(16)
Ni1 N5 N6 C16 . . -0.90(19)
N2 N1 C2 C3 . . 0.6(2)
Ni1 N1 C2 C3 . . -179.13(16)
N2 N1 C2 C1 . . -178.3(2)
Ni1 N1 C2 C1 . . 2.0(4)
N1 C2 C3 C4 . . -0.7(3)
C1 C2 C3 C4 . . 178.1(2)
N1 N2 C4 C3 . . -0.2(2)
C16 N2 C4 C3 3_766 . -179.51(18)
N1 N2 C4 C5 . . 179.40(19)
C16 N2 C4 C5 3_766 . 0.1(3)
C2 C3 C4 N2 . . 0.5(2)
C2 C3 C4 C5 . . -179.0(2)
N6 N5 C7 C8 . . 1.1(2)
Ni1 N5 C7 C8 . . -174.92(15)
N6 N5 C7 C6 . . -178.7(2)
Ni1 N5 C7 C6 . . 5.3(4)
N5 C7 C8 C9 . . -0.7(2)
C6 C7 C8 C9 . . 179.1(2)
N5 N6 C9 C8 . . 0.8(2)
C16 N6 C9 C8 . . 177.22(17)
N5 N6 C9 C10 . . -179.96(18)
C16 N6 C9 C10 . . -3.5(3)
C7 C8 C9 N6 . . -0.1(2)
C7 C8 C9 C10 . . -179.3(2)
N4 N3 C12 C13 . . 0.1(2)
Ni1 N3 C12 C13 . . 176.51(17)
N4 N3 C12 C11 . . -179.9(2)
Ni1 N3 C12 C11 . . -3.5(4)
N3 C12 C13 C14 . . -0.4(3)
C11 C12 C13 C14 . . 179.6(2)
N3 N4 C14 C13 . . -0.5(2)
C16 N4 C14 C13 . . -179.21(18)
N3 N4 C14 C15 . . -179.27(19)
C16 N4 C14 C15 . . 2.0(3)
C12 C13 C14 N4 . . 0.5(2)
C12 C13 C14 C15 . . 179.2(2)
C14 N4 C16 N2 . 3_766 115.04(19)
N3 N4 C16 N2 . 3_766 -63.6(2)
C14 N4 C16 N6 . . -120.34(19)
N3 N4 C16 N6 . . 61.0(2)
C9 N6 C16 N2 . 3_766 -113.14(19)
N5 N6 C16 N2 . 3_766 63.10(19)
C9 N6 C16 N4 . . 122.73(18)
N5 N6 C16 N4 . . -61.0(2)
N23 Ni2 N21 C22 3_765 . -41.2(2)
N23 Ni2 N21 C22 . . 138.8(2)
N25 Ni2 N21 C22 . . 45.5(2)
N25 Ni2 N21 C22 3_765 . -134.5(2)
N23 Ni2 N21 N22 3_765 . 134.82(13)
N23 Ni2 N21 N22 . . -45.18(13)
N25 Ni2 N21 N22 . . -138.54(13)
N25 Ni2 N21 N22 3_765 . 41.46(13)
C22 N21 N22 C24 . . 0.0(2)
Ni2 N21 N22 C24 . . -177.25(12)
C22 N21 N22 C36 . 3_765 -178.72(16)
Ni2 N21 N22 C36 . 3_765 4.0(2)
N21 Ni2 N23 C27 . . -134.8(2)
N21 Ni2 N23 C27 3_765 . 45.2(2)
N25 Ni2 N23 C27 . . -40.3(2)
N25 Ni2 N23 C27 3_765 . 139.7(2)
N21 Ni2 N23 N24 . . 42.61(13)
N21 Ni2 N23 N24 3_765 . -137.39(13)
N25 Ni2 N23 N24 . . 137.07(13)
N25 Ni2 N23 N24 3_765 . -42.93(13)
C27 N23 N24 C29 . . -0.6(2)
Ni2 N23 N24 C29 . . -178.77(12)
C27 N23 N24 C36 . 3_765 179.35(16)
Ni2 N23 N24 C36 . 3_765 1.1(2)
N21 Ni2 N25 C32 . . 36.7(2)
N21 Ni2 N25 C32 3_765 . -143.3(2)
N23 Ni2 N25 C32 3_765 . 131.0(2)
N23 Ni2 N25 C32 . . -49.0(2)
N21 Ni2 N25 N26 . . -133.78(13)
N21 Ni2 N25 N26 3_765 . 46.22(13)
N23 Ni2 N25 N26 3_765 . -39.46(13)
N23 Ni2 N25 N26 . . 140.54(13)
C32 N25 N26 C34 . . -1.0(2)
Ni2 N25 N26 C34 . . 172.49(13)
C32 N25 N26 C36 . . -178.77(16)
Ni2 N25 N26 C36 . . -5.3(2)
N22 N21 C22 C23 . . 0.4(2)
Ni2 N21 C22 C23 . . 176.63(15)
N22 N21 C22 C21 . . -179.50(19)
Ni2 N21 C22 C21 . . -3.2(3)
N21 C22 C23 C24 . . -0.6(2)
C21 C22 C23 C24 . . 179.3(2)
N21 N22 C24 C23 . . -0.3(2)
C36 N22 C24 C23 3_765 . 178.23(17)
N21 N22 C24 C25 . . 179.31(19)
C36 N22 C24 C25 3_765 . -2.1(3)
C22 C23 C24 N22 . . 0.5(2)
C22 C23 C24 C25 . . -179.1(2)
N24 N23 C27 C28 . . 0.3(2)
Ni2 N23 C27 C28 . . 177.90(15)
N24 N23 C27 C26 . . -178.92(19)
Ni2 N23 C27 C26 . . -1.3(3)
N23 C27 C28 C29 . . 0.1(2)
C26 C27 C28 C29 . . 179.2(2)
C27 C28 C29 N24 . . -0.4(2)
C27 C28 C29 C30 . . -178.4(2)
N23 N24 C29 C28 . . 0.6(2)
C36 N24 C29 C28 3_765 . -179.29(18)
N23 N24 C29 C30 . . 178.81(19)
C36 N24 C29 C30 3_765 . -1.1(3)
N26 N25 C32 C33 . . 0.9(2)
Ni2 N25 C32 C33 . . -170.26(16)
N26 N25 C32 C31 . . -179.7(2)
Ni2 N25 C32 C31 . . 9.1(4)
N25 C32 C33 C34 . . -0.5(3)
C31 C32 C33 C34 . . -179.9(2)
C32 C33 C34 N26 . . -0.1(3)
C32 C33 C34 C35 . . 177.6(3)
N25 N26 C34 C33 . . 0.7(2)
C36 N26 C34 C33 . . 178.20(19)
N25 N26 C34 C35 . . -177.3(2)
C36 N26 C34 C35 . . 0.2(3)
C34 N26 C36 N22 . 3_765 124.1(2)
N25 N26 C36 N22 . 3_765 -58.5(2)
C34 N26 C36 N24 . 3_765 -111.7(2)
N25 N26 C36 N24 . 3_765 65.7(2)
