#------------------------------------------------------------------------------
#$Date: 2019-01-24 05:42:30 +0200 (Thu, 24 Jan 2019) $
#$Revision: 213285 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/14/2021446.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_2021446
loop_
_publ_author_name
'Qin, Tao'
'Zhang, Shunlin'
'Wang, Yixiong'
'Hou, Tianjiao'
'Zhu, Dunru'
'Jing, Su'
_publ_section_title
;
 Three novel topologically different metal--organic frameworks built from
 3-nitro-4-(pyridin-4-yl)benzoic acid
;
_journal_coeditor_code           SK3712
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229618018211
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Ni (C12 H7 N2 O4)2 (H2 O)2], 2C4 H9 N O'
_chemical_formula_moiety         'C24 H18 N4 Ni O10, 2(C4 H9 N O)'
_chemical_formula_sum            'C32 H36 N6 Ni O12'
_chemical_formula_weight         755.38
_chemical_name_systematic
;catena-Poly[[[diaquanickel(II)]-bis[μ₂-3-nitro-4-(pyridin-4-yl)benzoato-κ²O:N]] N,N-dimethylacetamide
disolvate]
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                98.341(9)
_cell_angle_beta                 93.604(9)
_cell_angle_gamma                117.018(6)
_cell_formula_units_Z            2
_cell_length_a                   11.866(7)
_cell_length_b                   12.259(7)
_cell_length_c                   14.248(14)
_cell_measurement_reflns_used    4686
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.0515
_cell_measurement_theta_min      2.2571
_cell_volume                     1807(2)
_computing_cell_refinement
;
SAINT (Bruker, 2005)
;
_computing_data_collection
;
APEX2 (Bruker, 2005)
;
_computing_data_reduction
;
SAINT (Bruker, 2005)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2010)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12864
_diffrn_reflns_theta_full        25.005
_diffrn_reflns_theta_max         25.005
_diffrn_reflns_theta_min         1.460
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_T_max  0.9309
_exptl_absorpt_correction_T_min  0.8885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2005)
;
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       block
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.464
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         6294
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0739P)²+0.9830P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1358
_reflns_number_gt                5054
_reflns_number_total             6294
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            sk3712sup1.cif
_cod_data_source_block           1845690
_cod_database_code               2021446
_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   0.889
_shelx_estimated_absorpt_t_max   0.931
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 0.02411(15) Uani d 1 . .
Ni Ni2 0.000000 1.000000 0.500000 0.02426(15) Uani d 1 . .
O O1 -0.0510(2) 0.82674(18) 0.42739(13) 0.0335(5) Uani d 1 . .
O O1W -0.1279(2) -0.1305(2) 0.06831(15) 0.0443(6) Uani d 1 . .
H H1WA -0.082098 -0.120880 0.120212 0.053 Uiso d 1 . .
H H1WB -0.206198 -0.172200 0.074282 0.053 Uiso d 1 . .
O O2W 0.12087(19) 1.07030(19) 0.40066(14) 0.0346(5) Uani d 1 . .
H H2WA 0.128744 1.141065 0.393885 0.042 Uiso d 1 . .
H H2WB 0.092074 1.020775 0.346545 0.042 Uiso d 1 . .
O O2 -0.1332(3) 0.7053(2) 0.53437(15) 0.0500(6) Uani d 1 . .
O O3 -0.018(3) 0.614(2) 0.1026(10) 0.103(6) Uani d 0.86(6) A 1
O O3A 0.048(5) 0.653(4) 0.127(4) 0.051(13) Uani d 0.14(6) A 2
O O4 0.126(7) 0.593(3) 0.145(4) 0.078(10) Uani d 0.43(16) A 1
O O4A 0.158(4) 0.587(3) 0.169(4) 0.083(6) Uani d 0.57(16) A 2
O O5 0.14968(18) 0.01671(18) 0.09383(13) 0.0309(4) Uani d 1 . .
O O6 0.05986(19) -0.07410(19) 0.21454(13) 0.0348(5) Uani d 1 . .
O O7 0.6737(6) 0.0451(8) 0.1233(5) 0.090(3) Uani d 0.594(9) B 1
O O7A 0.6954(13) 0.1306(13) 0.1786(10) 0.121(4) Uani d 0.406(9) B 2
O O8 0.6216(8) 0.1896(8) 0.1182(6) 0.130(3) Uani d 0.594(9) B 1
O O8A 0.5760(10) 0.0653(11) 0.0499(8) 0.117(4) Uani d 0.406(9) B 2
O O9 0.3862(10) 0.234(2) -0.0433(10) 0.075(4) Uani d 0.50(5) C 1
O O9A 0.3826(10) 0.281(2) -0.0539(7) 0.072(4) Uani d 0.50(5) C 2
O O10 0.6588(4) 0.2897(4) 0.5251(3) 0.1091(13) Uani d 1 . .
N N1 -0.0148(2) 0.1448(2) 0.09002(16) 0.0321(5) Uani d 1 . .
N N2 0.0442(5) 0.5906(3) 0.1650(3) 0.0653(12) Uani d 1 . .
N N3 0.8449(2) -0.0019(2) 0.41517(16) 0.0319(5) Uani d 1 . .
N N4 0.5990(4) 0.0777(5) 0.1351(3) 0.0905(14) Uani d 1 . .
N N5 0.5640(7) 0.3824(7) 0.0429(6) 0.161(3) Uani d 1 . .
N N6 0.5084(19) 0.3347(16) 0.5422(17) 0.108(6) Uani d 0.52(3) D 1
N N6A 0.5489(17) 0.3784(19) 0.5933(15) 0.095(6) Uani d 0.48(3) D 2
C C1 -0.0469(3) 0.2227(3) 0.0532(2) 0.0385(7) Uani d 1 . .
H H1A -0.060522 0.212539 -0.013183 0.046 Uiso calc 1 . .
C C2 -0.0610(3) 0.3169(3) 0.1069(2) 0.0406(8) Uani d 1 . .
H H2A -0.085650 0.366824 0.077048 0.049 Uiso calc 1 . .
C C3 -0.0381(3) 0.3371(3) 0.2068(2) 0.0353(7) Uani d 1 . .
C C4 -0.0045(4) 0.2575(3) 0.2452(2) 0.0466(9) Uani d 1 . .
H H4A 0.011571 0.266755 0.311364 0.056 Uiso calc 1 . .
C C5 0.0055(3) 0.1638(3) 0.1855(2) 0.0418(8) Uani d 1 . .
H H5A 0.027730 0.110977 0.213495 0.050 Uiso calc 1 . .
C C6 -0.0533(3) 0.4363(3) 0.2689(2) 0.0358(7) Uani d 1 . .
C C7 -0.0190(3) 0.5537(3) 0.2486(2) 0.0366(7) Uani d 1 . .
C C8 -0.0360(3) 0.6443(3) 0.3054(2) 0.0347(7) Uani d 1 . .
H H8A -0.014840 0.720158 0.286946 0.042 Uiso calc 1 . .
C C9 -0.0849(3) 0.6216(3) 0.3905(2) 0.0317(6) Uani d 1 . .
C C10 -0.1219(3) 0.5042(3) 0.4127(2) 0.0437(8) Uani d 1 . .
H H10A -0.156807 0.486576 0.468700 0.052 Uiso calc 1 . .
C C11 -0.1076(4) 0.4137(3) 0.3527(2) 0.0453(8) Uani d 1 . .
H H11A -0.134992 0.335500 0.368555 0.054 Uiso calc 1 . .
C C12 -0.0921(3) 0.7248(3) 0.4567(2) 0.0314(6) Uani d 1 . .
C C13 0.7882(3) 0.0644(3) 0.4515(2) 0.0411(8) Uani d 1 . .
H H13A 0.823027 0.115928 0.511616 0.049 Uiso calc 1 . .
C C14 0.6810(3) 0.0598(3) 0.4041(2) 0.0468(8) Uani d 1 . .
H H14A 0.644975 0.107377 0.432262 0.056 Uiso calc 1 . .
C C15 0.6270(3) -0.0154(3) 0.3146(2) 0.0389(7) Uani d 1 . .
C C16 0.6863(3) -0.0830(3) 0.2753(2) 0.0448(8) Uani d 1 . .
H H16A 0.654125 -0.133978 0.214782 0.054 Uiso calc 1 . .
C C17 0.7933(3) -0.0731(3) 0.3273(2) 0.0391(7) Uani d 1 . .
H H17A 0.832160 -0.118437 0.300035 0.047 Uiso calc 1 . .
C C18 0.5050(3) -0.0252(3) 0.2689(2) 0.0404(7) Uani d 1 . .
C C19 0.4903(3) 0.0212(4) 0.1873(2) 0.0476(8) Uani d 1 . .
C C20 0.3777(3) 0.0192(3) 0.1540(2) 0.0461(8) Uani d 1 . .
H H20A 0.372086 0.050986 0.099502 0.055 Uiso calc 1 . .
C C21 0.2741(3) -0.0295(3) 0.2013(2) 0.0316(6) Uani d 1 . .
C C22 0.2845(3) -0.0781(3) 0.2814(2) 0.0418(8) Uani d 1 . .
H H22A 0.214577 -0.112297 0.313732 0.050 Uiso calc 1 . .
C C23 0.3974(3) -0.0763(3) 0.3138(2) 0.0457(8) Uani d 1 . .
H H23A 0.401564 -0.110336 0.367280 0.055 Uiso calc 1 . .
C C24 0.1510(3) -0.0289(2) 0.16763(19) 0.0284(6) Uani d 1 . .
C C25 0.3793(6) 0.3378(7) 0.1171(5) 0.129(3) Uani d 1 . .
H H25A 0.419866 0.326593 0.172686 0.194 Uiso calc 1 . .
H H25B 0.291278 0.274960 0.103292 0.194 Uiso calc 1 . .
H H25C 0.383888 0.418963 0.129210 0.194 Uiso calc 1 . .
C C26 0.4480(7) 0.3265(7) 0.0306(6) 0.124(2) Uani d 1 . .
C C27 0.6281(6) 0.3548(9) -0.0403(6) 0.172(4) Uani d 1 . .
H H27A 0.571320 0.329628 -0.099356 0.257 Uiso calc 1 . .
H H27B 0.647656 0.288870 -0.031087 0.257 Uiso calc 1 . .
H H27C 0.705581 0.428483 -0.042769 0.257 Uiso calc 1 . .
C C28 0.6440(8) 0.4610(10) 0.1384(7) 0.213(5) Uani d 1 . .
H H28A 0.611284 0.515905 0.164074 0.320 Uiso calc 1 . .
H H28B 0.731144 0.509412 0.129115 0.320 Uiso calc 1 . .
H H28C 0.640022 0.407294 0.182255 0.320 Uiso calc 1 . .
C C29 0.4406(7) 0.2434(7) 0.4449(7) 0.184(4) Uani d 1 . .
H H29A 0.411841 0.159097 0.453619 0.276 Uiso calc 1 D 1
H H29B 0.499386 0.261492 0.399105 0.276 Uiso calc 1 D 1
H H29C 0.368502 0.253153 0.421972 0.276 Uiso calc 1 D 1
C C30 0.6183(16) 0.3516(13) 0.5725(12) 0.074(7) Uani d 0.52(3) D 1
C C30A 0.5519(16) 0.3027(12) 0.5188(15) 0.068(6) Uani d 0.48(3) D 2
C C31 0.6761(9) 0.4459(9) 0.6649(5) 0.164(4) Uani d 1 . .
H H31A 0.747637 0.439978 0.694320 0.246 Uiso calc 1 D 1
H H31B 0.613156 0.429598 0.707466 0.246 Uiso calc 1 D 1
H H31C 0.704344 0.528303 0.651906 0.246 Uiso calc 1 D 1
C C32 0.4347(7) 0.3936(9) 0.5959(7) 0.179(4) Uani d 1 . .
H H32A 0.486919 0.482495 0.612408 0.268 Uiso calc 1 D 1
H H32B 0.413581 0.360783 0.653234 0.268 Uiso calc 1 D 1
H H32C 0.357584 0.374089 0.555438 0.268 Uiso calc 1 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'
N N 0.0061 0.0033 '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'
Ni Ni 0.3393 1.1124 '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
O1W Ni1 O1W . 2 180.0
O1W Ni1 O5 . 2 90.13(9)
O1W Ni1 O5 2 2 89.87(9)
O1W Ni1 O5 . . 89.87(9)
O1W Ni1 O5 2 . 90.13(9)
O5 Ni1 O5 2 . 180.0
O1W Ni1 N1 . . 90.62(10)
O1W Ni1 N1 2 . 89.38(11)
O5 Ni1 N1 2 . 87.91(9)
O5 Ni1 N1 . . 92.09(9)
O1W Ni1 N1 . 2 89.38(10)
O1W Ni1 N1 2 2 90.62(10)
O5 Ni1 N1 2 2 92.09(9)
O5 Ni1 N1 . 2 87.91(9)
N1 Ni1 N1 . 2 180.0
O1 Ni2 O1 . 2_576 180.00(10)
O1 Ni2 O2W . 2_576 91.64(9)
O1 Ni2 O2W 2_576 2_576 88.36(9)
O1 Ni2 O2W . . 88.36(9)
O1 Ni2 O2W 2_576 . 91.64(9)
O2W Ni2 O2W 2_576 . 180.00(12)
O1 Ni2 N3 . 2_666 91.20(9)
O1 Ni2 N3 2_576 2_666 88.80(9)
O2W Ni2 N3 2_576 2_666 91.58(10)
O2W Ni2 N3 . 2_666 88.42(11)
O1 Ni2 N3 . 1_465 88.80(9)
O1 Ni2 N3 2_576 1_465 91.20(9)
O2W Ni2 N3 2_576 1_465 88.42(11)
O2W Ni2 N3 . 1_465 91.58(10)
N3 Ni2 N3 2_666 1_465 180.0
C12 O1 Ni2 . . 129.71(19)
Ni1 O1W H1WA . . 102.4
Ni1 O1W H1WB . . 145.4
H1WA O1W H1WB . . 108.8
Ni2 O2W H2WA . . 110.7
Ni2 O2W H2WB . . 110.6
H2WA O2W H2WB . . 108.8
C24 O5 Ni1 . . 131.40(18)
C5 N1 C1 . . 115.8(2)
C5 N1 Ni1 . . 123.15(19)
C1 N1 Ni1 . . 121.01(19)
O4 N2 O3 . . 114(5)
O3A N2 O4A . . 109(3)
O3A N2 C7 . . 130.9(18)
O4 N2 C7 . . 131(5)
O3 N2 C7 . . 114.9(10)
O4A N2 C7 . . 112(2)
C13 N3 C17 . . 116.5(3)
C13 N3 Ni2 . 1_645 119.8(2)
C17 N3 Ni2 . 1_645 123.50(19)
O7A N4 O8A . . 125.7(9)
O7 N4 O8 . . 119.0(6)
O7A N4 C19 . . 116.9(8)
O7 N4 C19 . . 125.8(5)
O8A N4 C19 . . 117.4(6)
O8 N4 C19 . . 113.8(5)
C26 N5 C28 . . 123.5(9)
C26 N5 C27 . . 115.7(7)
C28 N5 C27 . . 120.2(7)
C30 N6 C32 . . 125(2)
C30 N6 C29 . . 117.2(17)
C32 N6 C29 . . 117.7(16)
C30A N6A C32 . . 118(2)
C30A N6A C31 . . 113.2(14)
C32 N6A C31 . . 128.9(16)
N1 C1 C2 . . 124.3(3)
N1 C1 H1A . . 117.9
C2 C1 H1A . . 117.9
C1 C2 C3 . . 119.5(3)
C1 C2 H2A . . 120.3
C3 C2 H2A . . 120.3
C4 C3 C2 . . 116.5(3)
C4 C3 C6 . . 121.3(3)
C2 C3 C6 . . 122.1(3)
C3 C4 C5 . . 120.0(3)
C3 C4 H4A . . 120.0
C5 C4 H4A . . 120.0
N1 C5 C4 . . 123.8(3)
N1 C5 H5A . . 118.1
C4 C5 H5A . . 118.1
C7 C6 C11 . . 115.6(3)
C7 C6 C3 . . 124.1(3)
C11 C6 C3 . . 120.3(3)
C8 C7 C6 . . 123.8(3)
C8 C7 N2 . . 115.4(3)
C6 C7 N2 . . 120.7(3)
C7 C8 C9 . . 119.5(3)
C7 C8 H8A . . 120.2
C9 C8 H8A . . 120.2
C8 C9 C10 . . 118.3(3)
C8 C9 C12 . . 119.3(3)
C10 C9 C12 . . 122.4(3)
C11 C10 C9 . . 120.9(3)
C11 C10 H10A . . 119.6
C9 C10 H10A . . 119.6
C10 C11 C6 . . 121.8(3)
C10 C11 H11A . . 119.1
C6 C11 H11A . . 119.1
O2 C12 O1 . . 126.2(3)
O2 C12 C9 . . 119.3(3)
O1 C12 C9 . . 114.5(3)
N3 C13 C14 . . 123.1(3)
N3 C13 H13A . . 118.4
C14 C13 H13A . . 118.4
C13 C14 C15 . . 120.0(3)
C13 C14 H14A . . 120.0
C15 C14 H14A . . 120.0
C14 C15 C16 . . 117.5(3)
C14 C15 C18 . . 118.2(3)
C16 C15 C18 . . 124.3(3)
C17 C16 C15 . . 119.0(3)
C17 C16 H16A . . 120.5
C15 C16 H16A . . 120.5
N3 C17 C16 . . 123.9(3)
N3 C17 H17A . . 118.1
C16 C17 H17A . . 118.1
C23 C18 C19 . . 115.7(3)
C23 C18 C15 . . 118.3(3)
C19 C18 C15 . . 125.9(3)
C20 C19 C18 . . 122.8(3)
C20 C19 N4 . . 117.5(3)
C18 C19 N4 . . 119.7(3)
C21 C20 C19 . . 120.0(3)
C21 C20 H20A . . 120.0
C19 C20 H20A . . 120.0
C20 C21 C22 . . 118.8(3)
C20 C21 C24 . . 120.7(3)
C22 C21 C24 . . 120.5(3)
C23 C22 C21 . . 120.7(3)
C23 C22 H22A . . 119.6
C21 C22 H22A . . 119.6
C22 C23 C18 . . 122.0(3)
C22 C23 H23A . . 119.0
C18 C23 H23A . . 119.0
O6 C24 O5 . . 126.1(3)
O6 C24 C21 . . 117.6(2)
O5 C24 C21 . . 116.3(2)
C26 C25 H25A . . 109.5
C26 C25 H25B . . 109.5
H25A C25 H25B . . 109.5
C26 C25 H25C . . 109.5
H25A C25 H25C . . 109.5
H25B C25 H25C . . 109.5
N5 C26 O9A . . 121.8(9)
N5 C26 O9 . . 120.1(9)
N5 C26 C25 . . 117.6(8)
O9A C26 C25 . . 119.1(8)
O9 C26 C25 . . 119.7(8)
N5 C27 H27A . . 109.5
N5 C27 H27B . . 109.5
H27A C27 H27B . . 109.5
N5 C27 H27C . . 109.5
H27A C27 H27C . . 109.5
H27B C27 H27C . . 109.5
N5 C28 H28A . . 109.5
N5 C28 H28B . . 109.5
H28A C28 H28B . . 109.5
N5 C28 H28C . . 109.5
H28A C28 H28C . . 109.5
H28B C28 H28C . . 109.5
N6 C29 H29A . . 109.5
N6 C29 H29B . . 109.5
H29A C29 H29B . . 109.5
N6 C29 H29C . . 109.5
H29A C29 H29C . . 109.5
H29B C29 H29C . . 109.5
O10 C30 N6 . . 117(2)
O10 C30 C31 . . 131.1(14)
N6 C30 C31 . . 112.1(15)
N6A C30A O10 . . 113.4(19)
N6A C30A C29 . . 116.7(16)
O10 C30A C29 . . 129.9(15)
C30 C31 H31A . . 109.5
C30 C31 H31B . . 109.5
H31A C31 H31B . . 109.5
C30 C31 H31C . . 109.5
H31A C31 H31C . . 109.5
H31B C31 H31C . . 109.5
N6 C32 H32A . . 109.5
N6 C32 H32B . . 109.5
H32A C32 H32B . . 109.5
N6 C32 H32C . . 109.5
H32A C32 H32C . . 109.5
H32B C32 H32C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ni1 O1W . 2.059(2)
Ni1 O1W 2 2.059(2)
Ni1 O5 2 2.068(2)
Ni1 O5 . 2.068(2)
Ni1 N1 . 2.116(2)
Ni1 N1 2 2.116(2)
Ni2 O1 . 2.016(2)
Ni2 O1 2_576 2.016(2)
Ni2 O2W 2_576 2.071(2)
Ni2 O2W . 2.071(2)
Ni2 N3 2_666 2.126(3)
Ni2 N3 1_465 2.126(2)
O1 C12 . 1.264(3)
O1W H1WA . 0.8499
O1W H1WB . 0.8501
O2W H2WA . 0.8499
O2W H2WB . 0.8499
O2 C12 . 1.248(4)
O3 N2 . 1.27(2)
O3A N2 . 0.99(4)
O4 N2 . 1.02(7)
O4A N2 . 1.36(5)
O5 C24 . 1.263(3)
O6 C24 . 1.256(3)
O7 N4 . 1.138(6)
O7A N4 . 1.109(13)
O8 N4 . 1.335(9)
O8A N4 . 1.200(11)
O9 C26 . 1.314(12)
O9A C26 . 1.288(11)
O10 C30 . 1.219(15)
O10 C30A . 1.348(16)
N1 C5 . 1.333(4)
N1 C1 . 1.336(4)
N2 C7 . 1.465(5)
N3 C13 . 1.342(4)
N3 C17 . 1.344(4)
N4 C19 . 1.467(5)
N5 C26 . 1.214(8)
N5 C28 . 1.519(9)
N5 C27 . 1.525(9)
N6 C30 . 1.26(3)
N6 C32 . 1.539(16)
N6 C29 . 1.55(2)
N6A C30A . 1.32(4)
N6A C32 . 1.451(17)
N6A C31 . 1.56(2)
C1 C2 . 1.371(4)
C1 H1A . 0.9300
C2 C3 . 1.395(4)
C2 H2A . 0.9300
C3 C4 . 1.375(4)
C3 C6 . 1.484(4)
C4 C5 . 1.382(4)
C4 H4A . 0.9300
C5 H5A . 0.9300
C6 C7 . 1.388(4)
C6 C11 . 1.396(4)
C7 C8 . 1.375(4)
C8 C9 . 1.387(4)
C8 H8A . 0.9300
C9 C10 . 1.392(4)
C9 C12 . 1.504(4)
C10 C11 . 1.380(4)
C10 H10A . 0.9300
C11 H11A . 0.9300
C13 C14 . 1.376(4)
C13 H13A . 0.9300
C14 C15 . 1.380(5)
C14 H14A . 0.9300
C15 C16 . 1.392(5)
C15 C18 . 1.496(4)
C16 C17 . 1.375(4)
C16 H16A . 0.9300
C17 H17A . 0.9300
C18 C23 . 1.387(5)
C18 C19 . 1.401(5)
C19 C20 . 1.377(4)
C20 C21 . 1.370(4)
C20 H20A . 0.9300
C21 C22 . 1.385(4)
C21 C24 . 1.512(4)
C22 C23 . 1.378(4)
C22 H22A . 0.9300
C23 H23A . 0.9300
C25 C26 . 1.544(8)
C25 H25A . 0.9600
C25 H25B . 0.9600
C25 H25C . 0.9600
C27 H27A . 0.9600
C27 H27B . 0.9600
C27 H27C . 0.9600
C28 H28A . 0.9600
C28 H28B . 0.9600
C28 H28C . 0.9600
C29 C30A . 1.45(2)
C29 H29A . 0.9600
C29 H29B . 0.9600
C29 H29C . 0.9600
C30 C31 . 1.51(2)
C31 H31A . 0.9600
C31 H31B . 0.9600
C31 H31C . 0.9600
C32 H32A . 0.9600
C32 H32B . 0.9600
C32 H32C . 0.9600
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
O1W H1WA O6 . 0.85 1.89 2.717(4) 163 yes
O1W H1WB O9 2_555 0.85 1.91 2.707(18) 156 yes
O2W H2WA O2 2_576 0.85 1.98 2.706(4) 142 yes
O2W H2WB O6 1_565 0.85 1.98 2.815(4) 168 yes
C1 H1A O3 2_565 0.93 2.48 3.104(19) 125 yes
C4 H4A O2 2_566 0.93 2.44 3.317(5) 157 yes
C5 H5A O6 . 0.93 2.47 3.334(4) 155 yes
C14 H14A O10 . 0.93 2.36 3.210(7) 153 yes
C16 H16A O9 2_655 0.93 2.48 3.393(15) 167 yes
C27 H27B O8 . 0.96 2.57 3.227(13) 126 yes
C28 H28C O8 . 0.96 2.60 3.183(15) 120 yes
C32 H32C O2 2_566 0.96 2.56 3.505(11) 170 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
C5 N1 C1 C2 . -0.9(5)
Ni1 N1 C1 C2 . 178.5(3)
N1 C1 C2 C3 . 1.6(5)
C1 C2 C3 C4 . -1.2(5)
C1 C2 C3 C6 . -179.2(3)
C2 C3 C4 C5 . 0.2(5)
C6 C3 C4 C5 . 178.2(3)
C1 N1 C5 C4 . -0.2(5)
Ni1 N1 C5 C4 . -179.6(3)
C3 C4 C5 N1 . 0.6(6)
C4 C3 C6 C7 . 143.6(4)
C2 C3 C6 C7 . -38.5(5)
C4 C3 C6 C11 . -37.9(5)
C2 C3 C6 C11 . 140.0(4)
C11 C6 C7 C8 . 0.0(5)
C3 C6 C7 C8 . 178.5(3)
C11 C6 C7 N2 . 177.2(4)
C3 C6 C7 N2 . -4.3(5)
O3A N2 C7 C8 . -27(5)
O4 N2 C7 C8 . 122(3)
O3 N2 C7 C8 . -65.1(12)
O4A N2 C7 C8 . 117.4(14)
O3A N2 C7 C6 . 156(5)
O4 N2 C7 C6 . -56(3)
O3 N2 C7 C6 . 117.4(11)
O4A N2 C7 C6 . -60.1(15)
C6 C7 C8 C9 . 2.9(5)
N2 C7 C8 C9 . -174.5(3)
C7 C8 C9 C10 . -3.6(5)
C7 C8 C9 C12 . 174.5(3)
C8 C9 C10 C11 . 1.5(5)
C12 C9 C10 C11 . -176.5(3)
C9 C10 C11 C6 . 1.4(6)
C7 C6 C11 C10 . -2.2(5)
C3 C6 C11 C10 . 179.3(3)
Ni2 O1 C12 O2 . 14.6(5)
Ni2 O1 C12 C9 . -163.34(19)
C8 C9 C12 O2 . -178.3(3)
C10 C9 C12 O2 . -0.3(5)
C8 C9 C12 O1 . -0.2(4)
C10 C9 C12 O1 . 177.8(3)
C17 N3 C13 C14 . 1.4(5)
Ni2 N3 C13 C14 1_645 -174.5(3)
N3 C13 C14 C15 . -0.2(5)
C13 C14 C15 C16 . -1.0(5)
C13 C14 C15 C18 . 175.4(3)
C14 C15 C16 C17 . 0.9(5)
C18 C15 C16 C17 . -175.2(3)
C13 N3 C17 C16 . -1.5(5)
Ni2 N3 C17 C16 1_645 174.3(3)
C15 C16 C17 N3 . 0.3(5)
C14 C15 C18 C23 . -63.1(4)
C16 C15 C18 C23 . 113.0(4)
C14 C15 C18 C19 . 112.0(4)
C16 C15 C18 C19 . -71.9(5)
C23 C18 C19 C20 . 1.3(6)
C15 C18 C19 C20 . -173.8(3)
C23 C18 C19 N4 . 179.7(4)
C15 C18 C19 N4 . 4.5(6)
O7A N4 C19 C20 . 144.0(11)
O7 N4 C19 C20 . -144.7(8)
O8A N4 C19 C20 . -34.3(9)
O8 N4 C19 C20 . 48.8(7)
O7A N4 C19 C18 . -34.5(12)
O7 N4 C19 C18 . 36.9(10)
O8A N4 C19 C18 . 147.3(8)
O8 N4 C19 C18 . -129.6(5)
C18 C19 C20 C21 . 0.0(6)
N4 C19 C20 C21 . -178.3(4)
C19 C20 C21 C22 . -1.1(5)
C19 C20 C21 C24 . 178.2(3)
C20 C21 C22 C23 . 0.7(5)
C24 C21 C22 C23 . -178.5(3)
C21 C22 C23 C18 . 0.7(5)
C19 C18 C23 C22 . -1.7(5)
C15 C18 C23 C22 . 173.9(3)
Ni1 O5 C24 O6 . -17.5(4)
Ni1 O5 C24 C21 . 162.00(18)
C20 C21 C24 O6 . -179.4(3)
C22 C21 C24 O6 . -0.2(4)
C20 C21 C24 O5 . 1.0(4)
C22 C21 C24 O5 . -179.7(3)
C28 N5 C26 O9A . 166.6(17)
C27 N5 C26 O9A . -21.9(19)
C28 N5 C26 O9 . -161.0(17)
C27 N5 C26 O9 . 10.5(19)
C28 N5 C26 C25 . 0.7(13)
C27 N5 C26 C25 . 172.2(7)
C32 N6 C30 O10 . 173.9(13)
C29 N6 C30 O10 . -3.7(19)
C32 N6 C30 C31 . -5(2)
C29 N6 C30 C31 . 177.5(11)
C32 N6A C30A O10 . -176.8(10)
C31 N6A C30A O10 . 6.5(15)
C32 N6A C30A C29 . 1.2(17)
C31 N6A C30A C29 . -175.5(10)

_cod_database_fobs_code 2021446
