#------------------------------------------------------------------------------
#$Date: 2024-07-05 18:34:34 +0300 (Fri, 05 Jul 2024) $
#$Revision: 292975 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/83/7248385.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_7248385
loop_
_publ_author_name
'Mendoza-Báez, Raúl'
'Molina-Renteria, Alan'
'Olguín, Juan'
_publ_section_title
;
 Nitro group and K+-based secondary building units for the self-assembly
 of 3D coordination polymers built on dinuclear dianionic helicate
 connectors
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              2346
_journal_page_last               2352
_journal_paper_doi               10.1039/D4CE00255E
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C83 H57 K2 N13 Ni2 O18'
_chemical_formula_sum            'C83 H57 K2 N13 Ni2 O18'
_chemical_formula_weight         1720.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2024-01-18 deposited with the CCDC.	2024-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.921(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7610(11)
_cell_length_b                   14.5644(9)
_cell_length_c                   36.558(3)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.8964
_cell_measurement_theta_min      2.2504
_cell_volume                     8311.8(10)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection
'Bruker Instrument Service (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'XP V 5.1 (Bruker, 1998)'
_computing_publication_material  'XP V 5.1 (Bruker, 1998)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2012 (Bruker, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 VENTURE diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1132
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            204178
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.250
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sheldrick, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3536
_exptl_crystal_size_max          0.384
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.056
_exptl_transmission_factor_max   0.7452
_exptl_transmission_factor_min   0.6704
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         7322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0642
_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)+(0.0984P)²+16.4832P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1671
_refine_ls_wR_factor_ref         0.1879
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5052
_reflns_number_total             7322
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00255e2.cif
_cod_data_source_block           JOAMR137B
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7248384--7248385.cif.
;
_cod_original_cell_volume        8311.7(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7248385
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.6704
_shelx_estimated_absorpt_t_max   0.7452
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+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
O3 O 0.4594(4) 0.9069(4) 0.06832(15) 0.139(2) Uani 1 1 d . . . . .
N3 N 0.6343(2) 0.4443(2) 0.38045(9) 0.0465(9) Uani 1 1 d . . . . .
C3 C 0.2396(3) 0.6066(3) 0.25193(11) 0.0461(10) Uani 1 1 d . . . . .
H3 H 0.1942 0.5915 0.2646 0.055 Uiso 1 1 calc R U . . .
O2 O 0.4335(3) 0.8713(3) 0.01154(12) 0.1052(15) Uani 1 1 d . . . . .
C2 C 0.3162(3) 0.6329(3) 0.27184(11) 0.0455(10) Uani 1 1 d . . . . .
N2 N 0.4260(3) 0.8567(3) 0.04348(15) 0.0811(14) Uani 1 1 d . . . . .
O4 O 0.81044(18) 0.3841(2) 0.40507(8) 0.0547(8) Uani 1 1 d . . . . .
C4 C 0.2277(3) 0.6018(3) 0.21402(11) 0.0472(10) Uani 1 1 d . . . . .
H4 H 0.1747 0.5849 0.2014 0.057 Uiso 1 1 calc R U . . .
N4 N 0.6626(4) 0.1077(3) 0.47874(14) 0.0852(15) Uani 1 1 d . . . . .
O6 O 0.7100(3) 0.0521(4) 0.49618(15) 0.1236(19) Uani 1 1 d . . . . .
N6 N -0.1497(3) 0.4139(3) 0.19663(16) 0.0757(13) Uani 1 1 d . . . . .
C6 C 0.3719(3) 0.6515(3) 0.21412(12) 0.0519(11) Uani 1 1 d . . . . .
H6 H 0.4172 0.6670 0.2015 0.062 Uiso 1 1 calc R U . . .
O5 O 0.5862(3) 0.1056(3) 0.47818(15) 0.1127(17) Uani 1 1 d . . . . .
N5 N 0.2245(2) 0.4077(2) 0.17347(9) 0.0450(8) Uani 1 1 d . . . . .
C5 C 0.2953(3) 0.6223(3) 0.19464(11) 0.0437(10) Uani 1 1 d . . . . .
O7 O 0.11817(19) 0.5352(2) 0.12581(8) 0.0530(8) Uani 1 1 d . . . . .
C7 C 0.3820(3) 0.6579(3) 0.25222(12) 0.0518(11) Uani 1 1 d . . . . .
H7 H 0.4335 0.6791 0.2649 0.062 Uiso 1 1 calc R U . . .
O8 O -0.2232(2) 0.4332(4) 0.18246(14) 0.1053(15) Uani 1 1 d . . . . .
C8 C 0.3138(3) 0.6819(3) 0.13812(12) 0.0532(11) Uani 1 1 d . . . . .
H8 H 0.3323 0.7320 0.1529 0.064 Uiso 1 1 calc R U . . .
C9 C 0.3197(3) 0.6919(3) 0.09918(11) 0.0498(11) Uani 1 1 d . . . . .
O9 O -0.1335(3) 0.3708(4) 0.22521(16) 0.1113(17) Uani 1 1 d . . . . .
C1 C 0.3313(3) 0.6334(3) 0.31375(11) 0.0508(11) Uani 1 1 d . . . . .
H1A H 0.2816 0.6067 0.3227 0.061 Uiso 1 1 calc R U . . .
H1B H 0.3358 0.6966 0.3222 0.061 Uiso 1 1 calc R U . . .
K1 K 0.08530(7) 0.51389(9) 0.04746(3) 0.0664(3) Uani 1 1 d . . . . .
Ni1 Ni 0.24122(3) 0.48984(4) 0.12729(2) 0.0435(2) Uani 1 1 d . . . . .
N1 N 0.2862(2) 0.6129(2) 0.15499(9) 0.0443(8) Uani 1 1 d . . . . .
O1 O 0.2407(2) 0.5586(2) 0.07873(8) 0.0561(8) Uani 1 1 d . . . . .
C20 C 0.4508(3) 0.5167(3) 0.31221(13) 0.0549(12) Uani 1 1 d . . . . .
H20 H 0.4277 0.5013 0.2882 0.066 Uiso 1 1 calc R U . . .
C21 C 0.6217(3) 0.3814(3) 0.40364(12) 0.0519(11) Uani 1 1 d . . . . .
H21 H 0.5657 0.3754 0.4086 0.062 Uiso 1 1 calc R U . . .
C22 C 0.6832(3) 0.3186(3) 0.42307(12) 0.0512(11) Uani 1 1 d . . . . .
C23 C 0.7734(3) 0.3230(3) 0.42216(12) 0.0516(11) Uani 1 1 d . . . . .
C24 C 0.8245(3) 0.2531(4) 0.44190(14) 0.0680(14) Uani 1 1 d . . . . .
H24 H 0.8836 0.2548 0.4424 0.082 Uiso 1 1 calc R U . . .
C25 C 0.7892(4) 0.1846(4) 0.45987(15) 0.0735(15) Uani 1 1 d . . . . .
H25 H 0.8241 0.1401 0.4725 0.088 Uiso 1 1 calc R U . . .
C26 C 0.7012(4) 0.1808(4) 0.45949(14) 0.0656(14) Uani 1 1 d . . . . .
C27 C 0.6505(3) 0.2478(3) 0.44196(13) 0.0613(13) Uani 1 1 d . . . . .
H27 H 0.5919 0.2457 0.4428 0.074 Uiso 1 1 calc R U . . .
C28 C 0.5000 0.1945(4) 0.2500 0.0563(17) Uani 1 2 d S T P . .
H28 H 0.475(3) 0.156(4) 0.2677(13) 0.076(15) Uiso 1 1 d . . . . .
C29 C 0.4281(3) 0.2505(3) 0.22963(13) 0.0484(11) Uani 1 1 d . . . . .
C30 C 0.3884(3) 0.3189(3) 0.24803(13) 0.0520(11) Uani 1 1 d . . . . .
H30 H 0.4073 0.3303 0.2728 0.062 Uiso 1 1 calc R U . . .
C31 C 0.3214(3) 0.3698(3) 0.22986(12) 0.0498(11) Uani 1 1 d . . . . .
H31 H 0.2950 0.4144 0.2426 0.060 Uiso 1 1 calc R U . . .
C32 C 0.2936(3) 0.3545(3) 0.19274(12) 0.0427(10) Uani 1 1 d . . . . .
C33 C 0.3313(3) 0.2866(3) 0.17430(12) 0.0456(10) Uani 1 1 d . . . . .
H33 H 0.3123 0.2750 0.1495 0.055 Uiso 1 1 calc R U . . .
C34 C 0.3976(3) 0.2358(3) 0.19299(13) 0.0484(11) Uani 1 1 d . . . . .
H34 H 0.4225 0.1900 0.1803 0.058 Uiso 1 1 calc R U . . .
C35 C 0.1523(3) 0.3968(3) 0.18551(12) 0.0487(11) Uani 1 1 d . . . . .
H35 H 0.1524 0.3569 0.2054 0.058 Uiso 1 1 calc R U . . .
C36 C 0.0706(3) 0.4392(3) 0.17186(12) 0.0488(11) Uani 1 1 d . . . . .
C37 C 0.0581(3) 0.5052(3) 0.14270(12) 0.0486(11) Uani 1 1 d . . . . .
C38 C -0.0280(3) 0.5378(4) 0.13211(14) 0.0594(12) Uani 1 1 d . . . . .
H38 H -0.0385 0.5809 0.1133 0.071 Uiso 1 1 calc R U . . .
C39 C -0.0938(3) 0.5073(4) 0.14888(15) 0.0634(14) Uani 1 1 d . . . . .
H39 H -0.1491 0.5282 0.1410 0.076 Uiso 1 1 calc R U . . .
C40 C -0.0798(3) 0.4460(3) 0.17746(15) 0.0582(12) Uani 1 1 d . . . . .
C41 C 0.0009(3) 0.4124(3) 0.18925(14) 0.0585(12) Uani 1 1 d . . . . .
H41 H 0.0092 0.3715 0.2090 0.070 Uiso 1 1 calc R U . . .
C10 C 0.2838(3) 0.6280(3) 0.07158(11) 0.0499(11) Uani 1 1 d . . . . .
C11 C 0.3000(3) 0.6445(4) 0.03504(13) 0.0676(14) Uani 1 1 d . . . . .
H11 H 0.2786 0.6033 0.0166 0.081 Uiso 1 1 calc R U . . .
C12 C 0.3454(3) 0.7178(4) 0.02586(14) 0.0684(14) Uani 1 1 d . . . . .
H12 H 0.3553 0.7263 0.0016 0.082 Uiso 1 1 calc R U . . .
C13 C 0.3768(3) 0.7800(4) 0.05299(13) 0.0633(13) Uani 1 1 d . . . . .
C14 C 0.3645(3) 0.7673(3) 0.08892(13) 0.0592(12) Uani 1 1 d . . . . .
H14 H 0.3865 0.8098 0.1067 0.071 Uiso 1 1 calc R U . . .
C16 C 0.4447(3) 0.5985(4) 0.36706(13) 0.0609(13) Uani 1 1 d . . . . .
H16 H 0.4186 0.6417 0.3806 0.073 Uiso 1 1 calc R U . . .
C15 C 0.4106(3) 0.5817(3) 0.33092(11) 0.0431(10) Uani 1 1 d . . . . .
C17 C 0.5168(3) 0.5527(4) 0.38384(12) 0.0606(13) Uani 1 1 d . . . . .
H17 H 0.5372 0.5638 0.4085 0.073 Uiso 1 1 calc R U . . .
C19 C 0.5254(3) 0.4736(3) 0.32834(12) 0.0541(12) Uani 1 1 d . . . . .
H19 H 0.5531 0.4323 0.3146 0.065 Uiso 1 1 calc R U . . .
C18 C 0.5581(3) 0.4912(3) 0.36420(11) 0.0437(10) Uani 1 1 d . . . . .
C42 C 0.4049(8) 0.2464(11) 0.3943(4) 0.091(4) Uani 0.5 1 d . . P . .
C43 C 0.3909(8) 0.2811(10) 0.3596(4) 0.107(5) Uani 0.5 1 d . . P . .
H43A H 0.3447 0.2484 0.3455 0.160 Uiso 0.5 1 calc R U P . .
H43B H 0.4418 0.2746 0.3482 0.160 Uiso 0.5 1 calc R U P . .
H43C H 0.3763 0.3450 0.3607 0.160 Uiso 0.5 1 calc R U P . .
N7 N 0.4169(9) 0.2392(14) 0.4237(5) 0.157(7) Uani 0.5 1 d . . P . .
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'
K K 0.2009 0.2494 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 O3 K1 113.0(4) . 3 ?
C21 N3 C18 114.6(4) . . ?
C21 N3 Ni1 122.8(3) . 2_655 ?
C18 N3 Ni1 122.0(3) . 2_655 ?
C4 C3 C2 122.3(4) . . ?
C4 C3 H3 118.8 . . ?
C2 C3 H3 118.8 . . ?
N2 O2 K1 149.5(4) . 7_565 ?
N2 O2 K1 83.6(3) . 3 ?
K1 O2 K1 85.54(11) 7_565 3 ?
C3 C2 C7 117.6(4) . . ?
C3 C2 C1 122.6(4) . . ?
C7 C2 C1 119.7(4) . . ?
O2 N2 O3 121.4(5) . . ?
O2 N2 C13 120.1(5) . . ?
O3 N2 C13 118.5(5) . . ?
O2 N2 K1 75.6(3) . 3 ?
O3 N2 K1 47.5(3) . 3 ?
C13 N2 K1 160.3(4) . 3 ?
C23 O4 Ni1 129.6(3) . 2_655 ?
C23 O4 K1 114.8(3) . 2_655 ?
Ni1 O4 K1 90.16(11) 2_655 2_655 ?
C3 C4 C5 119.7(4) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
O5 N4 O6 122.1(5) . . ?
O5 N4 C26 119.7(5) . . ?
O6 N4 C26 118.1(6) . . ?
O5 N4 K1 62.8(3) . 8_556 ?
O6 N4 K1 61.9(3) . 8_556 ?
C26 N4 K1 161.1(4) . 8_556 ?
N4 O6 K1 97.5(4) . 8_556 ?
O9 N6 O8 123.5(5) . . ?
O9 N6 C40 119.6(5) . . ?
O8 N6 C40 116.8(6) . . ?
C5 C6 C7 120.7(4) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
N4 O5 K1 149.5(5) . 4_545 ?
N4 O5 K1 96.8(3) . 8_556 ?
K1 O5 K1 84.28(11) 4_545 8_556 ?
C35 N5 C32 114.3(4) . . ?
C35 N5 Ni1 123.8(3) . . ?
C32 N5 Ni1 121.7(2) . . ?
C6 C5 C4 118.7(4) . . ?
C6 C5 N1 120.4(4) . . ?
C4 C5 N1 120.9(4) . . ?
C37 O7 Ni1 129.9(3) . . ?
C37 O7 K1 113.8(3) . . ?
Ni1 O7 K1 91.81(11) . . ?
C6 C7 C2 120.8(4) . . ?
C6 C7 H7 119.6 . . ?
C2 C7 H7 119.6 . . ?
N1 C8 C9 128.5(4) . . ?
N1 C8 H8 115.8 . . ?
C9 C8 H8 115.8 . . ?
C14 C9 C10 119.4(4) . . ?
C14 C9 C8 116.8(4) . . ?
C10 C9 C8 123.8(4) . . ?
C2 C1 C15 114.9(3) . . ?
C2 C1 H1A 108.6 . . ?
C15 C1 H1A 108.6 . . ?
C2 C1 H1B 108.6 . . ?
C15 C1 H1B 108.6 . . ?
H1A C1 H1B 107.5 . . ?
O1 K1 O2 100.71(13) . 7_565 ?
O1 K1 O3 133.72(15) . 3_445 ?
O2 K1 O3 124.97(17) 7_565 3_445 ?
O1 K1 O7 60.61(9) . . ?
O2 K1 O7 135.64(13) 7_565 . ?
O3 K1 O7 79.59(13) 3_445 . ?
O1 K1 O4 59.23(9) . 2_655 ?
O2 K1 O4 149.76(13) 7_565 2_655 ?
O3 K1 O4 80.47(16) 3_445 2_655 ?
O7 K1 O4 57.60(9) . 2_655 ?
O1 K1 O5 139.21(12) . 4 ?
O2 K1 O5 59.32(15) 7_565 4 ?
O3 K1 O5 71.68(18) 3_445 4 ?
O7 K1 O5 106.95(11) . 4 ?
O4 K1 O5 150.61(13) 2_655 4 ?
O1 K1 O6 72.89(11) . 8_455 ?
O2 K1 O6 73.44(16) 7_565 8_455 ?
O3 K1 O6 123.33(17) 3_445 8_455 ?
O7 K1 O6 127.36(12) . 8_455 ?
O4 K1 O6 78.67(13) 2_655 8_455 ?
O5 K1 O6 124.66(15) 4 8_455 ?
O1 K1 O5 112.77(13) . 8_455 ?
O2 K1 O5 72.93(15) 7_565 8_455 ?
O3 K1 O5 89.61(16) 3_445 8_455 ?
O7 K1 O5 150.08(13) . 8_455 ?
O4 K1 O5 93.27(13) 2_655 8_455 ?
O5 K1 O5 95.72(11) 4 8_455 ?
O6 K1 O5 40.47(12) 8_455 8_455 ?
O1 K1 O2 155.01(13) . 3_445 ?
O2 K1 O2 94.46(11) 7_565 3_445 ?
O3 K1 O2 39.87(13) 3_445 3_445 ?
O7 K1 O2 119.25(10) . 3_445 ?
O4 K1 O2 98.44(11) 2_655 3_445 ?
O5 K1 O2 65.77(13) 4 3_445 ?
O6 K1 O2 92.88(12) 8_455 3_445 ?
O5 K1 O2 53.25(13) 8_455 3_445 ?
O1 K1 N2 145.49(12) . 3_445 ?
O2 K1 N2 112.55(14) 7_565 3_445 ?
O3 K1 N2 19.49(13) 3_445 3_445 ?
O7 K1 N2 98.49(11) . 3_445 ?
O4 K1 N2 86.60(11) 2_655 3_445 ?
O5 K1 N2 70.24(13) 4 3_445 ?
O6 K1 N2 107.28(13) 8_455 3_445 ?
O5 K1 N2 70.70(14) 8_455 3_445 ?
O2 K1 N2 20.77(10) 3_445 3_445 ?
O1 K1 N4 92.44(12) . 8_455 ?
O2 K1 N4 75.36(14) 7_565 8_455 ?
O3 K1 N4 104.86(16) 3_445 8_455 ?
O7 K1 N4 139.16(12) . 8_455 ?
O4 K1 N4 82.71(11) 2_655 8_455 ?
O5 K1 N4 113.01(14) 4 8_455 ?
O6 K1 N4 20.65(12) 8_455 8_455 ?
O5 K1 N4 20.34(11) 8_455 8_455 ?
O2 K1 N4 72.24(13) 3_445 8_455 ?
N2 K1 N4 87.44(14) 3_445 8_455 ?
O1 K1 N7 71.4(2) . 4 ?
O2 K1 N7 69.6(3) 7_565 4 ?
O3 K1 N7 114.9(3) 3_445 4 ?
O7 K1 N7 66.3(3) . 4 ?
O4 K1 N7 117.6(3) 2_655 4 ?
O5 K1 N7 68.3(2) 4 4 ?
O6 K1 N7 121.5(3) 8_455 4 ?
O5 K1 N7 142.4(3) 8_455 4 ?
O2 K1 N7 133.1(2) 3_445 4 ?
N2 K1 N7 128.2(3) 3_445 4 ?
N4 K1 N7 137.3(3) 8_455 4 ?
O1 Ni1 O4 84.97(12) . 2_655 ?
O1 Ni1 O7 85.87(12) . . ?
O4 Ni1 O7 85.84(12) 2_655 . ?
O1 Ni1 N5 170.94(12) . . ?
O4 Ni1 N5 87.24(13) 2_655 . ?
O7 Ni1 N5 88.95(13) . . ?
O1 Ni1 N3 86.02(13) . 2_655 ?
O4 Ni1 N3 89.37(12) 2_655 2_655 ?
O7 Ni1 N3 170.91(12) . 2_655 ?
N5 Ni1 N3 98.55(13) . 2_655 ?
O1 Ni1 N1 87.83(12) . . ?
O4 Ni1 N1 171.72(13) 2_655 . ?
O7 Ni1 N1 89.58(13) . . ?
N5 Ni1 N1 99.58(13) . . ?
N3 Ni1 N1 94.21(13) 2_655 . ?
O1 Ni1 K1 47.03(8) . . ?
O4 Ni1 K1 54.89(9) 2_655 . ?
O7 Ni1 K1 53.24(8) . . ?
N5 Ni1 K1 124.15(9) . . ?
N3 Ni1 K1 117.79(9) 2_655 . ?
N1 Ni1 K1 116.94(10) . . ?
C8 N1 C5 114.5(3) . . ?
C8 N1 Ni1 122.8(3) . . ?
C5 N1 Ni1 122.5(3) . . ?
C10 O1 Ni1 129.4(3) . . ?
C10 O1 K1 126.9(3) . . ?
Ni1 O1 K1 98.55(12) . . ?
C15 C20 C19 121.5(4) . . ?
C15 C20 H20 119.3 . . ?
C19 C20 H20 119.3 . . ?
N3 C21 C22 128.4(4) . . ?
N3 C21 H21 115.8 . . ?
C22 C21 H21 115.8 . . ?
C27 C22 C23 119.1(4) . . ?
C27 C22 C21 116.5(4) . . ?
C23 C22 C21 124.2(4) . . ?
O4 C23 C22 124.6(4) . . ?
O4 C23 C24 118.6(4) . . ?
C22 C23 C24 116.7(4) . . ?
C25 C24 C23 121.9(5) . . ?
C25 C24 H24 119.1 . . ?
C23 C24 H24 119.1 . . ?
C24 C25 C26 120.1(5) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C27 C26 C25 119.7(5) . . ?
C27 C26 N4 119.6(5) . . ?
C25 C26 N4 120.6(5) . . ?
C26 C27 C22 122.3(5) . . ?
C26 C27 H27 118.8 . . ?
C22 C27 H27 118.8 . . ?
C29 C28 C29 114.5(5) 2_655 . ?
C29 C28 H28 109(3) 2_655 . ?
C29 C28 H28 107(3) . . ?
C34 C29 C30 117.4(4) . . ?
C34 C29 C28 122.4(4) . . ?
C30 C29 C28 120.2(4) . . ?
C31 C30 C29 120.9(4) . . ?
C31 C30 H30 119.5 . . ?
C29 C30 H30 119.5 . . ?
C30 C31 C32 120.1(4) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
C33 C32 C31 119.7(4) . . ?
C33 C32 N5 119.7(4) . . ?
C31 C32 N5 120.6(4) . . ?
C32 C33 C34 119.4(4) . . ?
C32 C33 H33 120.3 . . ?
C34 C33 H33 120.3 . . ?
C29 C34 C33 122.5(4) . . ?
C29 C34 H34 118.7 . . ?
C33 C34 H34 118.7 . . ?
N5 C35 C36 127.9(4) . . ?
N5 C35 H35 116.0 . . ?
C36 C35 H35 116.0 . . ?
C41 C36 C37 119.5(4) . . ?
C41 C36 C35 116.0(4) . . ?
C37 C36 C35 124.5(4) . . ?
O7 C37 C36 123.8(4) . . ?
O7 C37 C38 119.4(4) . . ?
C36 C37 C38 116.8(4) . . ?
C39 C38 C37 121.6(5) . . ?
C39 C38 H38 119.2 . . ?
C37 C38 H38 119.2 . . ?
C38 C39 C40 120.5(5) . . ?
C38 C39 H39 119.8 . . ?
C40 C39 H39 119.8 . . ?
C39 C40 C41 121.1(4) . . ?
C39 C40 N6 121.4(5) . . ?
C41 C40 N6 117.5(5) . . ?
C40 C41 C36 120.5(5) . . ?
C40 C41 H41 119.7 . . ?
C36 C41 H41 119.7 . . ?
O1 C10 C11 120.2(4) . . ?
O1 C10 C9 123.0(4) . . ?
C11 C10 C9 116.8(4) . . ?
C12 C11 C10 122.6(5) . . ?
C12 C11 H11 118.7 . . ?
C10 C11 H11 118.7 . . ?
C11 C12 C13 119.2(5) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
C14 C13 C12 121.1(4) . . ?
C14 C13 N2 119.5(5) . . ?
C12 C13 N2 119.3(5) . . ?
C13 C14 C9 120.9(4) . . ?
C13 C14 H14 119.6 . . ?
C9 C14 H14 119.6 . . ?
C15 C16 C17 121.8(4) . . ?
C15 C16 H16 119.1 . . ?
C17 C16 H16 119.1 . . ?
C20 C15 C16 117.0(4) . . ?
C20 C15 C1 123.1(4) . . ?
C16 C15 C1 119.9(4) . . ?
C18 C17 C16 120.2(4) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C18 C19 C20 120.5(4) . . ?
C18 C19 H19 119.7 . . ?
C20 C19 H19 119.7 . . ?
C19 C18 C17 118.9(4) . . ?
C19 C18 N3 119.4(4) . . ?
C17 C18 N3 121.7(4) . . ?
N7 C42 C43 164(2) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 N7 K1 113.1(15) . 4_545 ?
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
O3 N2 1.227(6) . ?
O3 K1 2.713(5) 3 ?
N3 C21 1.282(5) . ?
N3 C18 1.437(5) . ?
N3 Ni1 2.126(3) 2_655 ?
C3 C4 1.374(6) . ?
C3 C2 1.375(6) . ?
C3 H3 0.9300 . ?
O2 N2 1.209(6) . ?
O2 K1 2.713(4) 7_565 ?
O2 K1 3.301(5) 3 ?
C2 C7 1.389(6) . ?
C2 C1 1.518(6) . ?
N2 C13 1.430(7) . ?
N2 K1 3.386(5) 3 ?
O4 C23 1.275(5) . ?
O4 Ni1 2.042(3) 2_655 ?
O4 K1 2.916(3) 2_655 ?
C4 C5 1.391(6) . ?
C4 H4 0.9300 . ?
N4 O5 1.201(6) . ?
N4 O6 1.221(6) . ?
N4 C26 1.454(7) . ?
N4 K1 3.432(5) 8_556 ?
O6 K1 3.052(5) 8_556 ?
N6 O9 1.215(6) . ?
N6 O8 1.234(6) . ?
N6 C40 1.461(7) . ?
C6 C5 1.381(6) . ?
C6 C7 1.383(6) . ?
C6 H6 0.9300 . ?
O5 K1 3.045(6) 4_545 ?
O5 K1 3.075(4) 8_556 ?
N5 C35 1.285(5) . ?
N5 C32 1.439(5) . ?
N5 Ni1 2.116(4) . ?
C5 N1 1.443(5) . ?
O7 C37 1.277(5) . ?
O7 Ni1 2.043(3) . ?
O7 K1 2.857(3) . ?
C7 H7 0.9300 . ?
C8 N1 1.286(5) . ?
C8 C9 1.446(6) . ?
C8 H8 0.9300 . ?
C9 C14 1.385(6) . ?
C9 C10 1.431(6) . ?
C1 C15 1.519(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
K1 O1 2.637(3) . ?
K1 O2 2.713(4) 7_565 ?
K1 O3 2.713(5) 3_445 ?
K1 O4 2.916(3) 2_655 ?
K1 O5 3.045(6) 4 ?
K1 O6 3.052(5) 8_455 ?
K1 O5 3.075(4) 8_455 ?
K1 O2 3.301(5) 3_445 ?
K1 N2 3.386(5) 3_445 ?
K1 N4 3.432(5) 8_455 ?
K1 N7 3.449(19) 4 ?
Ni1 O1 2.037(3) . ?
Ni1 O4 2.042(3) 2_655 ?
Ni1 N3 2.126(3) 2_655 ?
Ni1 N1 2.132(3) . ?
O1 C10 1.266(5) . ?
C20 C15 1.373(6) . ?
C20 C19 1.390(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.446(6) . ?
C21 H21 0.9300 . ?
C22 C27 1.380(6) . ?
C22 C23 1.427(6) . ?
C23 C24 1.430(6) . ?
C24 C25 1.355(7) . ?
C24 H24 0.9300 . ?
C25 C26 1.386(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.364(7) . ?
C27 H27 0.9300 . ?
C28 C29 1.507(6) 2_655 ?
C28 C29 1.507(6) . ?
C28 H28 0.98(5) . ?
C29 C34 1.376(6) . ?
C29 C30 1.397(6) . ?
C30 C31 1.384(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.385(6) . ?
C31 H31 0.9300 . ?
C32 C33 1.378(6) . ?
C33 C34 1.381(6) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 C36 1.454(6) . ?
C35 H35 0.9300 . ?
C36 C41 1.398(6) . ?
C36 C37 1.428(6) . ?
C37 C38 1.439(6) . ?
C38 C39 1.352(7) . ?
C38 H38 0.9300 . ?
C39 C40 1.369(7) . ?
C39 H39 0.9300 . ?
C40 C41 1.376(7) . ?
C41 H41 0.9300 . ?
C10 C11 1.414(6) . ?
C11 C12 1.354(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.383(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.366(6) . ?
C14 H14 0.9300 . ?
C16 C15 1.378(6) . ?
C16 C17 1.386(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.367(6) . ?
C17 H17 0.9300 . ?
C19 C18 1.366(6) . ?
C19 H19 0.9300 . ?
C42 N7 1.070(16) . ?
C42 C43 1.354(17) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
N7 K1 3.449(19) 4_545 ?
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
C35 H35 O9 0.93 2.60 3.339(7) 136.5 2
C11 H11 O6 0.93 2.57 3.416(7) 150.8 8_455
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 C3 C2 C7 2.0(6) . . . . ?
C4 C3 C2 C1 -176.6(4) . . . . ?
K1 O2 N2 O3 -56.4(11) 7_565 . . . ?
K1 O2 N2 O3 13.4(6) 3 . . . ?
K1 O2 N2 C13 123.0(7) 7_565 . . . ?
K1 O2 N2 C13 -167.2(5) 3 . . . ?
K1 O2 N2 K1 -69.8(7) 7_565 . . 3 ?
K1 O3 N2 O2 -17.7(8) 3 . . . ?
K1 O3 N2 C13 162.8(4) 3 . . . ?
C2 C3 C4 C5 1.3(6) . . . . ?
O5 N4 O6 K1 -18.7(7) . . . 8_556 ?
C26 N4 O6 K1 158.6(4) . . . 8_556 ?
O6 N4 O5 K1 -71.8(10) . . . 4_545 ?
C26 N4 O5 K1 111.0(7) . . . 4_545 ?
K1 N4 O5 K1 -90.3(6) 8_556 . . 4_545 ?
O6 N4 O5 K1 18.6(7) . . . 8_556 ?
C26 N4 O5 K1 -158.7(5) . . . 8_556 ?
C7 C6 C5 C4 1.7(6) . . . . ?
C7 C6 C5 N1 -178.0(4) . . . . ?
C3 C4 C5 C6 -3.1(6) . . . . ?
C3 C4 C5 N1 176.5(4) . . . . ?
C5 C6 C7 C2 1.7(7) . . . . ?
C3 C2 C7 C6 -3.5(6) . . . . ?
C1 C2 C7 C6 175.2(4) . . . . ?
N1 C8 C9 C14 -169.9(5) . . . . ?
N1 C8 C9 C10 8.8(8) . . . . ?
C3 C2 C1 C15 127.6(4) . . . . ?
C7 C2 C1 C15 -50.9(6) . . . . ?
C9 C8 N1 C5 175.2(4) . . . . ?
C9 C8 N1 Ni1 0.5(7) . . . . ?
C6 C5 N1 C8 -47.3(6) . . . . ?
C4 C5 N1 C8 133.0(4) . . . . ?
C6 C5 N1 Ni1 127.4(4) . . . . ?
C4 C5 N1 Ni1 -52.3(5) . . . . ?
C18 N3 C21 C22 176.2(4) . . . . ?
Ni1 N3 C21 C22 -12.8(7) 2_655 . . . ?
N3 C21 C22 C27 -169.9(5) . . . . ?
N3 C21 C22 C23 6.8(8) . . . . ?
Ni1 O4 C23 C22 -2.5(7) 2_655 . . . ?
K1 O4 C23 C22 110.2(4) 2_655 . . . ?
Ni1 O4 C23 C24 177.3(3) 2_655 . . . ?
K1 O4 C23 C24 -70.0(5) 2_655 . . . ?
C27 C22 C23 O4 178.6(5) . . . . ?
C21 C22 C23 O4 2.1(8) . . . . ?
C27 C22 C23 C24 -1.1(7) . . . . ?
C21 C22 C23 C24 -177.7(5) . . . . ?
O4 C23 C24 C25 -178.2(5) . . . . ?
C22 C23 C24 C25 1.6(8) . . . . ?
C23 C24 C25 C26 0.0(9) . . . . ?
C24 C25 C26 C27 -2.1(9) . . . . ?
C24 C25 C26 N4 -179.8(5) . . . . ?
O5 N4 C26 C27 2.1(9) . . . . ?
O6 N4 C26 C27 -175.3(6) . . . . ?
K1 N4 C26 C27 -90.4(13) 8_556 . . . ?
O5 N4 C26 C25 179.8(6) . . . . ?
O6 N4 C26 C25 2.4(9) . . . . ?
K1 N4 C26 C25 87.3(13) 8_556 . . . ?
C25 C26 C27 C22 2.6(8) . . . . ?
N4 C26 C27 C22 -179.7(5) . . . . ?
C23 C22 C27 C26 -0.9(8) . . . . ?
C21 C22 C27 C26 175.9(5) . . . . ?
C29 C28 C29 C34 128.8(4) 2_655 . . . ?
C29 C28 C29 C30 -52.7(3) 2_655 . . . ?
C34 C29 C30 C31 -0.3(6) . . . . ?
C28 C29 C30 C31 -178.9(4) . . . . ?
C29 C30 C31 C32 -1.1(7) . . . . ?
C30 C31 C32 C33 1.9(6) . . . . ?
C30 C31 C32 N5 -179.4(4) . . . . ?
C35 N5 C32 C33 115.2(4) . . . . ?
Ni1 N5 C32 C33 -61.3(4) . . . . ?
C35 N5 C32 C31 -63.5(5) . . . . ?
Ni1 N5 C32 C31 119.9(4) . . . . ?
C31 C32 C33 C34 -1.3(6) . . . . ?
N5 C32 C33 C34 -180.0(4) . . . . ?
C30 C29 C34 C33 0.9(6) . . . . ?
C28 C29 C34 C33 179.5(4) . . . . ?
C32 C33 C34 C29 -0.2(6) . . . . ?
C32 N5 C35 C36 -179.1(4) . . . . ?
Ni1 N5 C35 C36 -2.7(6) . . . . ?
N5 C35 C36 C41 177.6(4) . . . . ?
N5 C35 C36 C37 -2.8(7) . . . . ?
Ni1 O7 C37 C36 10.8(6) . . . . ?
K1 O7 C37 C36 125.2(4) . . . . ?
Ni1 O7 C37 C38 -168.6(3) . . . . ?
K1 O7 C37 C38 -54.2(4) . . . . ?
C41 C36 C37 O7 178.4(4) . . . . ?
C35 C36 C37 O7 -1.2(7) . . . . ?
C41 C36 C37 C38 -2.2(6) . . . . ?
C35 C36 C37 C38 178.2(4) . . . . ?
O7 C37 C38 C39 179.3(4) . . . . ?
C36 C37 C38 C39 -0.2(7) . . . . ?
C37 C38 C39 C40 2.0(7) . . . . ?
C38 C39 C40 C41 -1.4(7) . . . . ?
C38 C39 C40 N6 178.4(4) . . . . ?
O9 N6 C40 C39 -168.8(5) . . . . ?
O8 N6 C40 C39 10.8(7) . . . . ?
O9 N6 C40 C41 11.0(7) . . . . ?
O8 N6 C40 C41 -169.4(5) . . . . ?
C39 C40 C41 C36 -1.0(7) . . . . ?
N6 C40 C41 C36 179.2(4) . . . . ?
C37 C36 C41 C40 2.8(7) . . . . ?
C35 C36 C41 C40 -177.6(4) . . . . ?
Ni1 O1 C10 C11 155.5(4) . . . . ?
K1 O1 C10 C11 -55.4(6) . . . . ?
Ni1 O1 C10 C9 -23.3(7) . . . . ?
K1 O1 C10 C9 125.8(4) . . . . ?
C14 C9 C10 O1 -178.6(4) . . . . ?
C8 C9 C10 O1 2.7(7) . . . . ?
C14 C9 C10 C11 2.6(7) . . . . ?
C8 C9 C10 C11 -176.1(5) . . . . ?
O1 C10 C11 C12 179.7(5) . . . . ?
C9 C10 C11 C12 -1.5(8) . . . . ?
C10 C11 C12 C13 -0.7(9) . . . . ?
C11 C12 C13 C14 1.6(8) . . . . ?
C11 C12 C13 N2 178.9(5) . . . . ?
O2 N2 C13 C14 -176.2(5) . . . . ?
O3 N2 C13 C14 3.3(9) . . . . ?
K1 N2 C13 C14 43.7(14) 3 . . . ?
O2 N2 C13 C12 6.5(8) . . . . ?
O3 N2 C13 C12 -174.0(6) . . . . ?
K1 N2 C13 C12 -133.7(9) 3 . . . ?
C12 C13 C14 C9 -0.4(8) . . . . ?
N2 C13 C14 C9 -177.7(5) . . . . ?
C10 C9 C14 C13 -1.8(8) . . . . ?
C8 C9 C14 C13 177.0(5) . . . . ?
C19 C20 C15 C16 -3.5(7) . . . . ?
C19 C20 C15 C1 177.3(4) . . . . ?
C17 C16 C15 C20 0.6(7) . . . . ?
C17 C16 C15 C1 179.8(5) . . . . ?
C2 C1 C15 C20 -19.5(6) . . . . ?
C2 C1 C15 C16 161.4(4) . . . . ?
C15 C16 C17 C18 2.3(8) . . . . ?
C15 C20 C19 C18 3.6(8) . . . . ?
C20 C19 C18 C17 -0.6(7) . . . . ?
C20 C19 C18 N3 178.8(4) . . . . ?
C16 C17 C18 C19 -2.3(7) . . . . ?
C16 C17 C18 N3 178.4(4) . . . . ?
C21 N3 C18 C19 -106.4(5) . . . . ?
Ni1 N3 C18 C19 82.5(5) 2_655 . . . ?
C21 N3 C18 C17 73.0(6) . . . . ?
Ni1 N3 C18 C17 -98.1(4) 2_655 . . . ?
C43 C42 N7 K1 176(5) . . . 4_545 ?
