#------------------------------------------------------------------------------
#$Date: 2020-04-06 01:15:10 +0300 (Mon, 06 Apr 2020) $
#$Revision: 250393 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/33/2243347.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_2243347
loop_
_publ_author_name
'Gavrish, Sergey P.'
'Shova, Sergiu'
'Cazacu, Maria'
'Dascalu, Mihaela'
'Lampeka, Yaroslaw D.'
_publ_section_title
;
 Syntheses and crystal structures of the one-dimensional coordination
 polymers formed by [Ni(cyclam)]²⁺ cations and
 1,3-bis(3-carboxypropyl)tetramethyldisiloxane anions in different degrees
 of deprotonation
;
_journal_coeditor_code           HB7892
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              446
_journal_page_last               451
_journal_paper_doi               10.1107/S2056989020002327
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '[Ni (C10 H25 O5 Si2) (C12 H24 N4)] Cl O4'
_chemical_formula_moiety         'C22 H49 N4 Ni O5 Si2 +, Cl O4 -'
_chemical_formula_sum            'C22 H49 Cl N4 Ni O9 Si2'
_chemical_formula_weight         663.99
_chemical_name_systematic
'catena-Poly[[[(1,4,8,11-tetraazacyclotetradecane-κ⁴N¹,N⁴,N⁸,N¹¹)nickel(II)]-μ-4-({[(3-carboxypropyl)dimethylsilyl]oxy}dimethylsilyl)butanoato-κ²O:O'] perchlorate]'
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_cell_angle_alpha                99.309(5)
_cell_angle_beta                 100.343(6)
_cell_angle_gamma                99.232(6)
_cell_formula_units_Z            2
_cell_length_a                   9.3815(7)
_cell_length_b                   12.9009(8)
_cell_length_c                   14.7604(10)
_cell_measurement_reflns_used    2033
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      24.5610
_cell_measurement_theta_min      1.6600
_cell_volume                     1700.9(2)
_computing_cell_refinement
;
CrysAlisPro (Agilent, 2014)
;
_computing_data_collection
;
CrysAlisPro (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlisPro (Agilent, 2014)
;
_computing_molecular_graphics
;
Mercury (Macrae et al.,  2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT  (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1593
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.063
_diffrn_reflns_av_unetI/netI     0.1003
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9606
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         1.947
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.436
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         9606
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0451P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                5769
_reflns_number_total             9606
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            hb7892sup1.cif
_cod_data_source_block           II
_cod_database_code               2243347
_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   0.724
_shelx_estimated_absorpt_t_max   0.803
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.000000 0.000000 0.000000 0.0241(2) Uani d 1 . .
Si Si1 -0.3977(2) -0.55987(11) -0.05469(15) 0.0729(6) Uani d 1 . .
O O1 -0.1184(3) -0.1542(2) -0.0727(2) 0.0310(8) Uani d 1 . .
O O2 -0.0826(3) -0.1583(2) -0.2165(2) 0.0339(8) Uani d 1 . .
H H2C -0.034950 -0.196653 -0.243367 0.051 Uiso d 0.5 . .
O O3 -0.5535(8) -0.5084(6) -0.0332(5) 0.061(3) Uani d 0.5 . .
N N1 0.1859(4) -0.0236(3) -0.0499(3) 0.0408(11) Uani d 1 . .
H H1 0.157126 -0.087684 -0.099864 0.049 Uiso calc 1 . .
N N2 -0.0809(4) 0.0725(3) -0.1075(3) 0.0390(11) Uani d 1 . .
H H2 -0.128011 0.014955 -0.161639 0.047 Uiso calc 1 . .
C C1 0.2858(6) -0.0494(5) 0.0295(4) 0.065(2) Uani d 1 . .
H H1A 0.335337 0.015969 0.073702 0.078 Uiso calc 1 . .
H H1B 0.360480 -0.083840 0.006336 0.078 Uiso calc 1 . .
C C2 -0.1992(7) 0.1219(4) -0.0773(4) 0.0649(19) Uani d 1 . .
H H2A -0.156944 0.189771 -0.034619 0.078 Uiso calc 1 . .
H H2B -0.263674 0.135605 -0.131369 0.078 Uiso calc 1 . .
C C3 0.0282(7) 0.1448(4) -0.1388(4) 0.0634(18) Uani d 1 . .
H H3A 0.071451 0.206181 -0.088446 0.076 Uiso calc 1 . .
H H3B -0.020855 0.170724 -0.191801 0.076 Uiso calc 1 . .
C C4 0.1501(7) 0.0909(4) -0.1671(4) 0.068(2) Uani d 1 . .
H H4A 0.104405 0.025115 -0.211911 0.081 Uiso calc 1 . .
H H4B 0.205970 0.137198 -0.199462 0.081 Uiso calc 1 . .
C C5 0.2570(6) 0.0641(4) -0.0893(4) 0.0608(18) Uani d 1 . .
H H5A 0.339987 0.043288 -0.113487 0.073 Uiso calc 1 . .
H H5B 0.294711 0.127196 -0.039965 0.073 Uiso calc 1 . .
C C6 -0.1332(4) -0.2035(3) -0.1537(3) 0.0254(11) Uani d 1 . .
C C7 -0.2146(5) -0.3171(3) -0.1832(3) 0.0378(13) Uani d 1 . .
H H7A -0.303379 -0.319448 -0.229384 0.045 Uiso calc 1 . .
H H7B -0.153320 -0.358866 -0.214036 0.045 Uiso calc 1 . .
C C8 -0.2580(5) -0.3700(3) -0.1066(3) 0.0363(12) Uani d 1 . .
H H8A -0.316658 -0.327704 -0.073869 0.044 Uiso calc 1 . .
H H8B -0.169508 -0.371782 -0.061703 0.044 Uiso calc 1 . .
C C9 -0.3463(5) -0.4842(3) -0.1431(3) 0.0477(14) Uani d 1 . .
H H9A -0.289182 -0.524186 -0.179202 0.057 Uiso calc 1 . .
H H9B -0.436249 -0.480898 -0.185840 0.057 Uiso calc 1 . .
C C10 -0.2275(11) -0.5710(6) 0.0258(5) 0.168(4) Uani d 1 . .
H H10A -0.191865 -0.505635 0.071407 0.252 Uiso calc 1 . .
H H10B -0.153386 -0.583786 -0.009580 0.252 Uiso calc 1 . .
H H10C -0.248872 -0.629417 0.057238 0.252 Uiso calc 1 . .
C C11 -0.5003(7) -0.6957(4) -0.1124(5) 0.102(3) Uani d 1 . .
H H11A -0.442542 -0.730299 -0.150911 0.153 Uiso calc 1 . .
H H11B -0.592187 -0.690955 -0.150829 0.153 Uiso calc 1 . .
H H11C -0.519460 -0.736539 -0.065495 0.153 Uiso calc 1 . .
Ni Ni2 0.000000 -0.500000 -0.500000 0.0281(2) Uani d 1 . .
Si Si2 0.35316(15) 0.04647(10) -0.52679(11) 0.0404(4) Uani d 1 . .
O O4 0.0305(3) -0.3297(2) -0.47284(19) 0.0333(8) Uani d 1 . .
O O5 -0.0840(3) -0.2890(2) -0.3576(2) 0.0376(9) Uani d 1 . .
H H5C -0.095950 -0.235276 -0.324118 0.056 Uiso d 0.5 . .
N N3 -0.1442(6) -0.5206(3) -0.4129(4) 0.0621(15) Uani d 1 . .
H H3 -0.143842 -0.449452 -0.377416 0.075 Uiso calc 1 . .
N N4 0.1844(5) -0.4870(3) -0.3968(4) 0.0675(16) Uani d 1 . .
H H4 0.207815 -0.412879 -0.361974 0.081 Uiso calc 1 . .
C C12 -0.2937(7) -0.5585(5) -0.4771(6) 0.094(3) Uani d 1 . .
H H12A -0.370162 -0.545605 -0.442664 0.113 Uiso calc 1 . .
H H12B -0.309077 -0.634809 -0.501474 0.113 Uiso calc 1 . .
C C13 0.3020(7) -0.5012(5) -0.4435(7) 0.111(4) Uani d 1 . .
H H13A 0.295115 -0.576820 -0.467592 0.133 Uiso calc 1 . .
H H13B 0.395995 -0.474737 -0.399517 0.133 Uiso calc 1 . .
C C14 0.1635(10) -0.5587(5) -0.3256(6) 0.112(3) Uani d 1 . .
H H14A 0.151266 -0.632881 -0.356424 0.134 Uiso calc 1 . .
H H14B 0.251865 -0.542354 -0.276130 0.134 Uiso calc 1 . .
C C15 0.0318(15) -0.5454(6) -0.2821(5) 0.136(4) Uani d 1 . .
H H15A 0.035328 -0.582999 -0.230129 0.163 Uiso calc 1 . .
H H15B 0.040102 -0.470013 -0.256570 0.163 Uiso calc 1 . .
C C16 -0.1145(11) -0.5851(5) -0.3474(6) 0.116(4) Uani d 1 . .
H H16A -0.117774 -0.657098 -0.380421 0.139 Uiso calc 1 . .
H H16B -0.191132 -0.588632 -0.311103 0.139 Uiso calc 1 . .
C C17 0.0036(5) -0.2625(3) -0.4108(3) 0.0278(11) Uani d 1 . .
C C18 0.0724(5) -0.1463(3) -0.3978(3) 0.0287(12) Uani d 1 . .
H H18A 0.132997 -0.123812 -0.334828 0.034 Uiso calc 1 . .
H H18B -0.006193 -0.105610 -0.401545 0.034 Uiso calc 1 . .
C C19 0.1664(5) -0.1164(3) -0.4662(3) 0.0359(12) Uani d 1 . .
H H19A 0.108087 -0.140813 -0.529665 0.043 Uiso calc 1 . .
H H19B 0.249045 -0.153188 -0.460348 0.043 Uiso calc 1 . .
C C20 0.2255(5) 0.0035(3) -0.4507(3) 0.0373(13) Uani d 1 . .
H H20A 0.276718 0.028112 -0.385648 0.045 Uiso calc 1 . .
H H20B 0.142064 0.039091 -0.460546 0.045 Uiso calc 1 . .
C C21 0.2725(6) -0.0094(4) -0.6529(4) 0.0706(18) Uani d 1 . .
H H21A 0.180766 0.013540 -0.670484 0.106 Uiso calc 1 . .
H H21B 0.255162 -0.086153 -0.663382 0.106 Uiso calc 1 . .
H H21C 0.339876 0.015653 -0.690111 0.106 Uiso calc 1 . .
C C22 0.3997(6) 0.1939(4) -0.5079(5) 0.084(2) Uani d 1 . .
H H22A 0.445438 0.222461 -0.443122 0.126 Uiso calc 1 . .
H H22B 0.311213 0.221370 -0.523912 0.126 Uiso calc 1 . .
H H22C 0.466709 0.214650 -0.546789 0.126 Uiso calc 1 . .
O O6X 0.493(3) -0.013(5) -0.497(6) 0.037(3) Uiso d 0.25 A 1
O O6 0.510(3) 0.021(4) -0.4772(12) 0.037(3) Uiso d 0.25 A 2
Cl Cl1 0.38292(17) -0.21590(12) -0.21055(12) 0.0683(5) Uani d 1 . .
O O7 0.3941(6) -0.2883(5) -0.2826(4) 0.194(3) Uani d 1 . .
O O8 0.2362(5) -0.2323(4) -0.1955(4) 0.1227(19) Uani d 1 . .
O O9 0.4112(6) -0.1102(4) -0.2279(4) 0.147(2) Uani d 1 . .
O O10 0.4768(6) -0.2161(4) -0.1271(4) 0.137(2) Uani d 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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
O1 Ni1 O1 . 2 180.0 ?
N1 Ni1 O1 2 . 88.17(12) ?
N1 Ni1 O1 2 2 91.83(12) ?
N1 Ni1 O1 . 2 88.17(12) ?
N1 Ni1 O1 . . 91.83(12) ?
N1 Ni1 N1 2 . 180.0 ?
N1 Ni1 N2 2 . 85.82(17) ?
N1 Ni1 N2 . 2 85.82(17) ?
N1 Ni1 N2 2 2 94.18(17) ?
N1 Ni1 N2 . . 94.18(17) ?
N2 Ni1 O1 . 2 87.38(12) ?
N2 Ni1 O1 2 . 87.38(12) ?
N2 Ni1 O1 . . 92.62(12) ?
N2 Ni1 O1 2 2 92.62(12) ?
N2 Ni1 N2 . 2 180.0 ?
O3 Si1 O3 2_445 . 42.6(4) ?
O3 Si1 C9 2_445 . 115.6(3) ?
O3 Si1 C9 . . 100.2(3) ?
O3 Si1 C10 . . 131.5(4) ?
O3 Si1 C10 2_445 . 89.4(4) ?
O3 Si1 C11 2_445 . 121.3(4) ?
O3 Si1 C11 . . 95.7(3) ?
C9 Si1 C10 . . 109.0(3) ?
C9 Si1 C11 . . 110.1(3) ?
C11 Si1 C10 . . 108.8(3) ?
C6 O1 Ni1 . . 132.9(3) ?
C6 O2 H2C . . 109.8 ?
Si1 O3 Si1 2_445 . 137.4(4) ?
O3 O3 Si1 2_445 . 63.0(6) ?
O3 O3 Si1 2_445 2_445 74.4(7) ?
Ni1 N1 H1 . . 107.4 ?
C1 N1 Ni1 . . 105.0(3) ?
C1 N1 H1 . . 107.4 ?
C5 N1 Ni1 . . 116.2(3) ?
C5 N1 H1 . . 107.4 ?
C5 N1 C1 . . 113.1(4) ?
Ni1 N2 H2 . . 106.7 ?
C2 N2 Ni1 . . 105.7(3) ?
C2 N2 H2 . . 106.7 ?
C3 N2 Ni1 . . 116.1(3) ?
C3 N2 H2 . . 106.7 ?
C3 N2 C2 . . 114.2(4) ?
N1 C1 H1A . . 109.7 ?
N1 C1 H1B . . 109.7 ?
N1 C1 C2 . 2 109.7(4) ?
H1A C1 H1B . . 108.2 ?
C2 C1 H1A 2 . 109.7 ?
C2 C1 H1B 2 . 109.7 ?
N2 C2 C1 . 2 109.8(4) ?
N2 C2 H2B . . 109.7 ?
N2 C2 H2A . . 109.7 ?
C1 C2 H2B 2 . 109.7 ?
C1 C2 H2A 2 . 109.7 ?
H2B C2 H2A . . 108.2 ?
N2 C3 H3A . . 109.1 ?
N2 C3 H3B . . 109.1 ?
N2 C3 C4 . . 112.3(4) ?
H3A C3 H3B . . 107.9 ?
C4 C3 H3A . . 109.1 ?
C4 C3 H3B . . 109.1 ?
C3 C4 H4A . . 108.1 ?
C3 C4 H4B . . 108.1 ?
H4A C4 H4B . . 107.3 ?
C5 C4 C3 . . 116.7(4) ?
C5 C4 H4A . . 108.1 ?
C5 C4 H4B . . 108.1 ?
N1 C5 C4 . . 111.4(4) ?
N1 C5 H5A . . 109.4 ?
N1 C5 H5B . . 109.4 ?
C4 C5 H5A . . 109.4 ?
C4 C5 H5B . . 109.4 ?
H5A C5 H5B . . 108.0 ?
O1 C6 O2 . . 121.4(4) ?
O1 C6 C7 . . 120.8(4) ?
O2 C6 C7 . . 117.7(4) ?
C6 C7 H7A . . 108.3 ?
C6 C7 H7B . . 108.3 ?
H7A C7 H7B . . 107.4 ?
C8 C7 C6 . . 116.0(4) ?
C8 C7 H7A . . 108.3 ?
C8 C7 H7B . . 108.3 ?
C7 C8 H8A . . 109.0 ?
C7 C8 H8B . . 109.0 ?
C7 C8 C9 . . 112.8(4) ?
H8A C8 H8B . . 107.8 ?
C9 C8 H8A . . 109.0 ?
C9 C8 H8B . . 109.0 ?
Si1 C9 H9A . . 108.1 ?
Si1 C9 H9B . . 108.1 ?
C8 C9 Si1 . . 116.8(3) ?
C8 C9 H9A . . 108.1 ?
C8 C9 H9B . . 108.1 ?
H9A C9 H9B . . 107.3 ?
Si1 C10 H10A . . 109.5 ?
Si1 C10 H10B . . 109.5 ?
Si1 C10 H10C . . 109.5 ?
H10A C10 H10B . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
Si1 C11 H11A . . 109.5 ?
Si1 C11 H11B . . 109.5 ?
Si1 C11 H11C . . 109.5 ?
H11A C11 H11B . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
O4 Ni2 O4 . 2_544 180.00(3) ?
N3 Ni2 O4 2_544 2_544 94.96(13) ?
N3 Ni2 O4 . . 94.96(13) ?
N3 Ni2 O4 2_544 . 85.04(13) ?
N3 Ni2 O4 . 2_544 85.04(13) ?
N3 Ni2 N3 2_544 . 180.0 ?
N3 Ni2 N4 2_544 2_544 94.3(2) ?
N3 Ni2 N4 . . 94.3(2) ?
N3 Ni2 N4 . 2_544 85.7(2) ?
N3 Ni2 N4 2_544 . 85.7(2) ?
N4 Ni2 O4 . 2_544 91.33(14) ?
N4 Ni2 O4 . . 88.67(14) ?
N4 Ni2 O4 2_544 . 91.33(14) ?
N4 Ni2 O4 2_544 2_544 88.67(14) ?
N4 Ni2 N4 . 2_544 180.0 ?
C21 Si2 C20 . . 111.6(2) ?
C22 Si2 C20 . . 110.6(2) ?
C22 Si2 C21 . . 109.6(3) ?
O6X Si2 C20 2_654 . 113.4(14) ?
O6X Si2 C20 . . 102.5(13) ?
O6X Si2 C21 . . 107(3) ?
O6X Si2 C21 2_654 . 107(3) ?
O6X Si2 C22 . . 116(2) ?
O6X Si2 C22 2_654 . 104(2) ?
O6X Si2 O6X 2_654 . 13(3) ?
O6X Si2 O6 . 2_654 13(3) ?
O6X Si2 O6 2_654 2_654 17(2) ?
O6 Si2 C20 2_654 . 111.2(17) ?
O6 Si2 C20 . . 103.5(15) ?
O6 Si2 C21 . . 120.4(6) ?
O6 Si2 C21 2_654 . 94.3(5) ?
O6 Si2 C22 . . 100.3(19) ?
O6 Si2 C22 2_654 . 118.5(19) ?
O6 Si2 O6 . 2_654 26.9(17) ?
C17 O4 Ni2 . . 133.8(3) ?
C17 O5 H5C . . 109.9 ?
Ni2 N3 H3 . . 106.9 ?
C12 N3 Ni2 . . 105.1(4) ?
C12 N3 H3 . . 106.9 ?
C16 N3 Ni2 . . 117.3(4) ?
C16 N3 H3 . . 106.9 ?
C16 N3 C12 . . 113.2(6) ?
Ni2 N4 H4 . . 106.8 ?
C13 N4 Ni2 . . 106.5(4) ?
C13 N4 H4 . . 106.8 ?
C13 N4 C14 . . 115.0(6) ?
C14 N4 Ni2 . . 114.4(4) ?
C14 N4 H4 . . 106.8 ?
N3 C12 H12A . . 109.9 ?
N3 C12 H12B . . 109.9 ?
N3 C12 C13 . 2_544 108.8(5) ?
H12A C12 H12B . . 108.3 ?
C13 C12 H12A 2_544 . 109.9 ?
C13 C12 H12B 2_544 . 109.9 ?
N4 C13 C12 . 2_544 109.6(6) ?
N4 C13 H13A . . 109.8 ?
N4 C13 H13B . . 109.8 ?
C12 C13 H13A 2_544 . 109.8 ?
C12 C13 H13B 2_544 . 109.8 ?
H13A C13 H13B . . 108.2 ?
N4 C14 H14A . . 109.0 ?
N4 C14 H14B . . 109.0 ?
H14A C14 H14B . . 107.8 ?
C15 C14 N4 . . 113.0(6) ?
C15 C14 H14A . . 109.0 ?
C15 C14 H14B . . 109.0 ?
C14 C15 H15A . . 108.5 ?
C14 C15 H15B . . 108.5 ?
H15A C15 H15B . . 107.5 ?
C16 C15 C14 . . 115.0(6) ?
C16 C15 H15A . . 108.5 ?
C16 C15 H15B . . 108.5 ?
N3 C16 C15 . . 113.1(7) ?
N3 C16 H16A . . 109.0 ?
N3 C16 H16B . . 109.0 ?
C15 C16 H16A . . 109.0 ?
C15 C16 H16B . . 109.0 ?
H16A C16 H16B . . 107.8 ?
Si2 C20 H20A . . 108.3 ?
Si2 C20 H20B . . 108.3 ?
H20A C20 H20B . . 107.4 ?
C19 C20 Si2 . . 115.9(3) ?
C19 C20 H20A . . 108.3 ?
C19 C20 H20B . . 108.3 ?
C20 C19 H19A . . 109.0 ?
C20 C19 H19B . . 109.0 ?
H19A C19 H19B . . 107.8 ?
C18 C19 C20 . . 113.1(3) ?
C18 C19 H19A . . 109.0 ?
C18 C19 H19B . . 109.0 ?
C19 C18 H18A . . 108.1 ?
C19 C18 H18B . . 108.1 ?
H18A C18 H18B . . 107.3 ?
C17 C18 C19 . . 116.7(3) ?
C17 C18 H18A . . 108.1 ?
C17 C18 H18B . . 108.1 ?
O4 C17 O5 . . 121.9(4) ?
O4 C17 C18 . . 120.1(4) ?
O5 C17 C18 . . 118.0(3) ?
Si2 C21 H21A . . 109.5 ?
Si2 C21 H21B . . 109.5 ?
Si2 C21 H21C . . 109.5 ?
H21A C21 H21B . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
Si2 C22 H22A . . 109.5 ?
Si2 C22 H22B . . 109.5 ?
Si2 C22 H22C . . 109.5 ?
H22A C22 H22B . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
Si2 O6X Si2 2_654 . 167(3) ?
O6X O6X Si2 2_654 2_654 96(6) ?
O6X O6X Si2 2_654 . 71(6) ?
Si2 O6 Si2 . 2_654 153.1(17) ?
O6 O6 Si2 2_654 . 78(2) ?
O7 Cl1 O8 . . 110.3(3) ?
O7 Cl1 O9 . . 112.0(4) ?
O7 Cl1 O10 . . 114.2(4) ?
O9 Cl1 O8 . . 105.3(3) ?
O10 Cl1 O8 . . 107.7(4) ?
O10 Cl1 O9 . . 106.8(3) ?
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 O1 . 2.125(2) ?
Ni1 O1 2 2.125(2) ?
Ni1 N1 2 2.058(3) ?
Ni1 N1 . 2.058(3) ?
Ni1 N2 2 2.060(4) ?
Ni1 N2 . 2.060(4) ?
Si1 O3 . 1.757(8) ?
Si1 O3 2_445 1.626(7) ?
Si1 C9 . 1.837(5) ?
Si1 C10 . 1.852(9) ?
Si1 C11 . 1.845(5) ?
O1 C6 . 1.232(4) ?
O2 H2C . 0.8200 ?
O2 C6 . 1.291(5) ?
O3 O3 2_445 1.234(13) ?
N1 H1 . 0.9800 ?
N1 C1 . 1.481(6) ?
N1 C5 . 1.475(6) ?
N2 H2 . 0.9800 ?
N2 C2 . 1.467(6) ?
N2 C3 . 1.461(6) ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
C1 C2 2 1.486(7) ?
C2 H2B . 0.9700 ?
C2 H2A . 0.9700 ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C3 C4 . 1.516(7) ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
C4 C5 . 1.507(7) ?
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
C6 C7 . 1.496(5) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C7 C8 . 1.496(6) ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C8 C9 . 1.529(5) ?
C9 H9A . 0.9700 ?
C9 H9B . 0.9700 ?
C10 H10A . 0.9600 ?
C10 H10B . 0.9600 ?
C10 H10C . 0.9600 ?
C11 H11A . 0.9600 ?
C11 H11B . 0.9600 ?
C11 H11C . 0.9600 ?
Ni2 O4 2_544 2.131(2) ?
Ni2 O4 . 2.131(2) ?
Ni2 N3 2_544 2.043(4) ?
Ni2 N3 . 2.043(4) ?
Ni2 N4 . 2.054(4) ?
Ni2 N4 2_544 2.054(4) ?
Si2 C20 . 1.864(5) ?
Si2 C21 . 1.855(5) ?
Si2 C22 . 1.845(5) ?
Si2 O6X 2_654 1.570(19) ?
Si2 O6X . 1.651(19) ?
Si2 O6 2_654 1.66(2) ?
Si2 O6 . 1.632(16) ?
O4 C17 . 1.245(4) ?
O5 H5C . 0.8199 ?
O5 C17 . 1.280(5) ?
N3 H3 . 0.9800 ?
N3 C12 . 1.502(8) ?
N3 C16 . 1.393(9) ?
N4 H4 . 0.9800 ?
N4 C13 . 1.422(8) ?
N4 C14 . 1.527(9) ?
C12 H12A . 0.9700 ?
C12 H12B . 0.9700 ?
C12 C13 2_544 1.502(10) ?
C13 H13A . 0.9700 ?
C13 H13B . 0.9700 ?
C14 H14A . 0.9700 ?
C14 H14B . 0.9700 ?
C14 C15 . 1.512(11) ?
C15 H15A . 0.9700 ?
C15 H15B . 0.9700 ?
C15 C16 . 1.488(11) ?
C16 H16A . 0.9700 ?
C16 H16B . 0.9700 ?
C20 H20A . 0.9700 ?
C20 H20B . 0.9700 ?
C20 C19 . 1.521(5) ?
C19 H19A . 0.9700 ?
C19 H19B . 0.9700 ?
C19 C18 . 1.512(6) ?
C18 H18A . 0.9700 ?
C18 H18B . 0.9700 ?
C18 C17 . 1.501(5) ?
C21 H21A . 0.9600 ?
C21 H21B . 0.9600 ?
C21 H21C . 0.9600 ?
C22 H22A . 0.9600 ?
C22 H22B . 0.9600 ?
C22 H22C . 0.9600 ?
O6X O6X 2_654 0.38(7) ?
O6 O6 2_654 0.77(5) ?
Cl1 O7 . 1.329(4) ?
Cl1 O8 . 1.421(5) ?
Cl1 O9 . 1.420(5) ?
Cl1 O10 . 1.380(5) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1 O2 . 0.98 2.51 3.225(5) 130 yes
N1 H1 O8 . 0.98 2.45 3.315(6) 147 yes
N2 H2 O2 . 0.98 2.38 3.143(4) 134 yes
N3 H3 O5 . 0.98 2.01 2.901(5) 150 yes
N4 H4 O7 . 0.98 2.18 3.012(6) 142 yes
O2 H2C O5 . 0.82 1.84 2.456(4) 131 yes
O2 H2C O8 . 0.82 2.65 3.260(5) 133 yes
O5 H5C O2 . 0.82 1.70 2.456(4) 151 yes
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Ni1 O1 C6 O2 . . . . -7.2(6) ?
Ni1 O1 C6 C7 . . . . 174.5(3) ?
Ni1 N1 C1 C2 . . . 2 40.9(4) ?
Ni1 N1 C5 C4 . . . . -56.2(5) ?
Ni1 N2 C2 C1 . . . 2 -39.8(4) ?
Ni1 N2 C3 C4 . . . . 55.3(5) ?
O1 C6 C7 C8 . . . . -7.7(6) ?
O2 C6 C7 C8 . . . . 174.0(4) ?
O3 Si1 O3 Si1 2_445 . . 2_445 -0.001(2) ?
O3 Si1 C9 C8 . . . . 81.0(4) ?
O3 Si1 C9 C8 2_445 . . . 39.0(5) ?
N2 C3 C4 C5 . . . . -70.0(6) ?
C1 N1 C5 C4 . . . . -177.7(4) ?
C2 N2 C3 C4 . . . . 178.7(4) ?
C3 N2 C2 C1 . . . 2 -168.7(4) ?
C3 C4 C5 N1 . . . . 70.1(5) ?
C5 N1 C1 C2 . . . 2 168.6(4) ?
C6 C7 C8 C9 . . . . 177.5(4) ?
C7 C8 C9 Si1 . . . . 176.9(4) ?
C9 Si1 O3 Si1 . . . 2_445 -116.9(7) ?
C9 Si1 O3 O3 . . . 2_445 -116.9(7) ?
C10 Si1 O3 Si1 . . . 2_445 10.0(10) ?
C10 Si1 O3 O3 . . . 2_445 10.0(10) ?
C10 Si1 C9 C8 . . . . -59.7(5) ?
C11 Si1 O3 Si1 . . . 2_445 131.5(8) ?
C11 Si1 O3 O3 . . . 2_445 131.5(8) ?
C11 Si1 C9 C8 . . . . -179.0(4) ?
Ni2 O4 C17 O5 . . . . -16.3(6) ?
Ni2 O4 C17 C18 . . . . 164.8(3) ?
Ni2 N3 C12 C13 . . . 2_544 -39.0(6) ?
Ni2 N3 C16 C15 . . . . 59.1(7) ?
Ni2 N4 C13 C12 . . . 2_544 42.1(6) ?
Ni2 N4 C14 C15 . . . . -52.9(7) ?
Si2 C20 C19 C18 . . . . 176.0(3) ?
N4 C14 C15 C16 . . . . 68.4(9) ?
C12 N3 C16 C15 . . . . -178.2(6) ?
C13 N4 C14 C15 . . . . -176.6(6) ?
C14 N4 C13 C12 . . . 2_544 169.9(5) ?
C14 C15 C16 N3 . . . . -71.7(8) ?
C16 N3 C12 C13 . . . 2_544 -168.2(5) ?
C20 Si2 O6X Si2 . . . 2_654 -15E1(3) ?
C20 Si2 O6X O6X . . . 2_654 -15E1(3) ?
C20 Si2 O6 Si2 . . . 2_654 110(7) ?
C20 Si2 O6 O6 . . . 2_654 110(7) ?
C20 C19 C18 C17 . . . . 177.2(4) ?
C19 C18 C17 O4 . . . . 3.3(6) ?
C19 C18 C17 O5 . . . . -175.7(4) ?
C21 Si2 C20 C19 . . . . 52.0(4) ?
C21 Si2 O6X Si2 . . . 2_654 10E1(3) ?
C21 Si2 O6X O6X . . . 2_654 10E1(3) ?
C21 Si2 O6 Si2 . . . 2_654 -15(9) ?
C21 Si2 O6 O6 . . . 2_654 -15(9) ?
C22 Si2 C20 C19 . . . . 174.3(4) ?
C22 Si2 O6X Si2 . . . 2_654 -3E1(3) ?
C22 Si2 O6X O6X . . . 2_654 -3E1(3) ?
C22 Si2 O6 Si2 . . . 2_654 -135(8) ?
C22 Si2 O6 O6 . . . 2_654 -135(8) ?
O6X Si2 C20 C19 2_654 . . . -70(4) ?
O6X Si2 C20 C19 . . . . -62(3) ?
O6X Si2 O6X Si2 2_654 . . 2_654 -0.01(14) ?
O6 Si2 C20 C19 2_654 . . . -51.9(12) ?
O6 Si2 C20 C19 . . . . -79.0(15) ?
O6 Si2 O6 Si2 2_654 . . 2_654 0.006(14) ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.7118(8)
2 0.2882(8)

_cod_database_fobs_code 2243347
