#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/53/2215331.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_2215331
loop_
_publ_author_name
'Xia, Hai-Tao'
'Liu, Yu-Fen'
'Wang, Da-Qi'
'Yang, Shu-Ping'
_publ_section_title
;Bis{N-[2-(2-hydroxy-3-methoxybenzylamino)ethyl]-N'-(2-hydroxy-3-methoxybenzyl)ethane-1,2-diamine}nickel(II)
 dinitrate 1.25-hydrate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2512
_journal_page_last               m2513
_journal_paper_doi               10.1107/S160053680704353X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ni (C20 H29 N3 O4)2] (N O3)2, 1.25H2 O'
_chemical_formula_moiety
'4(C40 H58 N6 Ni O8 -), 8(N O3 2+), 4(H2 O), H2 O'
_chemical_formula_sum            'C160 H242 N32 Ni4 O61'
_chemical_formula_weight         3824.70
_chemical_name_systematic
;Bis{N-[2-(2-hydroxy-3-methoxybenzylamino)ethyl]-N'-(2-hydroxy-3-methoxybenzyl)
ethane-1,2-diamine}nickel(II)
 dinitrate 1.25-hydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 130.370(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   43.710(3)
_cell_length_b                   9.5091(16)
_cell_length_c                   28.476(3)
_cell_measurement_reflns_used    2390
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      18.192
_cell_measurement_theta_min      2.566
_cell_volume                     9017.5(19)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Siemens SMART 1000 CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0744
_diffrn_reflns_av_sigmaI/netI    0.1271
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            22092
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.43
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_T_max  0.9370
_exptl_absorpt_correction_T_min  0.8228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4052
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.393
_refine_diff_density_min         -1.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         7920
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1411
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0509P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1537
_reflns_number_gt                3683
_reflns_number_total             7920
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            at2393.cif
_cod_data_source_block           I
_cod_original_cell_volume        9017.5(18)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2215331
_cod_database_fobs_code          2215331
loop_
_symmetry_equiv_pos_as_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_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_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.641419(19) 0.66303(7) 0.83507(3) 0.0421(2) Uani d . 1 . .
N N1 0.67961(12) 0.5637(5) 0.92197(18) 0.0470(11) Uani d . 1 . .
H H1 0.6824 0.6245 0.9492 0.056 Uiso calc R 1 . .
N N2 0.60570(12) 0.4742(4) 0.81236(18) 0.0453(11) Uani d . 1 . .
H H2 0.5900 0.4979 0.8217 0.054 Uiso calc R 1 . .
N N3 0.59205(12) 0.5073(4) 0.68534(18) 0.0503(12) Uani d . 1 . .
H H3A 0.6004 0.5837 0.7095 0.060 Uiso calc R 1 . .
H H3B 0.6092 0.4943 0.6783 0.060 Uiso calc R 1 . .
N N4 0.60783(12) 0.7801(5) 0.85042(19) 0.0495(12) Uani d . 1 . .
H H4 0.6088 0.7336 0.8793 0.059 Uiso calc R 1 . .
N N5 0.67810(11) 0.8570(4) 0.87038(17) 0.0446(11) Uani d . 1 . .
H H5 0.7044 0.8311 0.8952 0.053 Uiso calc R 1 . .
N N6 0.67847(11) 0.7963(4) 0.76456(18) 0.0457(11) Uani d . 1 . .
H H6A 0.6527 0.8062 0.7299 0.055 Uiso calc R 1 . .
H H6B 0.6795 0.7251 0.7864 0.055 Uiso calc R 1 . .
N N7 0.79795(17) 0.8175(6) 0.9440(3) 0.0647(14) Uani d . 1 . .
N N8 0.5515(3) 0.4732(12) 0.3733(4) 0.166(3) Uani d DU 1 . .
O O1 0.67406(9) 0.5765(4) 0.81493(14) 0.0434(9) Uani d . 1 . .
O O2 0.68190(10) 0.4173(4) 0.74696(16) 0.0532(10) Uani d . 1 . .
O O3 0.59061(11) 0.4258(4) 0.58805(17) 0.0726(12) Uani d . 1 . .
H H3 0.6000 0.3898 0.5736 0.109 Uiso calc R 1 . .
O O4 0.56196(12) 0.2248(5) 0.50398(18) 0.0799(13) Uani d . 1 . .
O O5 0.60564(9) 0.7372(3) 0.74682(14) 0.0394(8) Uani d . 1 . .
O O6 0.59622(13) 0.8973(4) 0.66216(17) 0.0809(9) Uani d . 1 . .
O O7 0.64853(14) 0.6522(5) 0.62992(19) 0.1009(16) Uani d . 1 . .
H H7 0.6368 0.6205 0.5953 0.151 Uiso d R 1 . .
O O8 0.62619(13) 0.7786(4) 0.52971(19) 0.0809(9) Uani d . 1 . .
O O9 0.77001(13) 0.8176(6) 0.9444(2) 0.0993(17) Uani d . 1 . .
O O10 0.83138(14) 0.7824(5) 0.9913(2) 0.0956(16) Uani d . 1 . .
O O11 0.79332(12) 0.8545(5) 0.8982(2) 0.0886(15) Uani d . 1 . .
O O12 0.5796(2) 0.4142(10) 0.3996(3) 0.198(3) Uani d DU 1 A .
O O13 0.5197(4) 0.418(3) 0.3255(11) 0.239(8) Uani d PDU 0.360(10) A 1
O O14 0.5441(6) 0.554(3) 0.3961(9) 0.215(6) Uani d PDU 0.360(10) A 1
O O13' 0.5460(3) 0.5510(16) 0.3304(6) 0.224(5) Uani d PDU 0.640(10) A 2
O O14' 0.5220(3) 0.4543(18) 0.3637(6) 0.195(4) Uani d PDU 0.640(10) A 2
O O15 0.62322(12) 0.4501(5) 0.53586(19) 0.0917(15) Uani d . 1 . .
H H41 0.6075 0.4356 0.4972 0.138 Uiso d R 1 . .
H H42 0.6448 0.4093 0.5489 0.138 Uiso d R 1 . .
O O16 0.5000 0.2747(19) 0.7500 0.166(7) Uani d SPU 0.50 . .
H H43 0.4795 0.3158 0.7182 0.250 Uiso d PR 0.50 . .
C C1 0.72074(15) 0.5365(6) 0.9449(2) 0.0542(15) Uani d . 1 . .
H H1A 0.7367 0.4966 0.9860 0.065 Uiso calc R 1 . .
H H1B 0.7328 0.6256 0.9483 0.065 Uiso calc R 1 . .
C C2 0.72261(14) 0.4396(6) 0.9053(2) 0.0449(14) Uani d . 1 . .
C C3 0.70035(14) 0.4694(5) 0.8429(2) 0.0408(13) Uani d . 1 . .
C C4 0.70488(15) 0.3824(5) 0.8079(3) 0.0425(14) Uani d . 1 . .
C C5 0.73178(16) 0.2706(6) 0.8355(3) 0.0525(15) Uani d . 1 . .
H H5A 0.7351 0.2143 0.8124 0.063 Uiso calc R 1 . .
C C6 0.75355(17) 0.2434(6) 0.8974(3) 0.0651(17) Uani d . 1 . .
H H6 0.7713 0.1679 0.9158 0.078 Uiso calc R 1 . .
C C7 0.74916(15) 0.3271(6) 0.9317(3) 0.0580(16) Uani d . 1 . .
H H7A 0.7642 0.3084 0.9735 0.070 Uiso calc R 1 . .
C C8 0.68558(16) 0.3331(6) 0.7093(2) 0.0658(17) Uani d . 1 . .
H H8A 0.7133 0.3268 0.7281 0.099 Uiso calc R 1 . .
H H8B 0.6706 0.3754 0.6693 0.099 Uiso calc R 1 . .
H H8C 0.6753 0.2406 0.7052 0.099 Uiso calc R 1 . .
C C9 0.55143(15) 0.5370(6) 0.6253(2) 0.0548(15) Uani d . 1 . .
H H9A 0.5530 0.6196 0.6070 0.066 Uiso calc R 1 . .
H H9B 0.5333 0.5586 0.6330 0.066 Uiso calc R 1 . .
C C10 0.53406(16) 0.4178(6) 0.5800(2) 0.0466(14) Uani d . 1 . .
C C11 0.55433(15) 0.3678(6) 0.5615(2) 0.0492(15) Uani d . 1 . .
C C12 0.53789(18) 0.2648(6) 0.5165(2) 0.0553(16) Uani d . 1 . .
C C13 0.50100(19) 0.2091(6) 0.4911(3) 0.0640(17) Uani d . 1 . .
H H13 0.4899 0.1379 0.4618 0.077 Uiso calc R 1 . .
C C14 0.48067(18) 0.2600(7) 0.5094(3) 0.0665(18) Uani d . 1 . .
H H14 0.4554 0.2244 0.4913 0.080 Uiso calc R 1 . .
C C15 0.49687(17) 0.3610(7) 0.5532(3) 0.0558(16) Uani d . 1 . .
H H15 0.4828 0.3924 0.5655 0.067 Uiso calc R 1 . .
C C16 0.5453(2) 0.1424(7) 0.4510(3) 0.095(2) Uani d . 1 . .
H H16A 0.5380 0.0517 0.4559 0.143 Uiso calc R 1 . .
H H16B 0.5647 0.1312 0.4457 0.143 Uiso calc R 1 . .
H H16C 0.5219 0.1882 0.4155 0.143 Uiso calc R 1 . .
C C17 0.65999(16) 0.4377(6) 0.9215(2) 0.0588(16) Uani d . 1 . .
H H17A 0.6439 0.4638 0.9326 0.071 Uiso calc R 1 . .
H H17B 0.6803 0.3717 0.9522 0.071 Uiso calc R 1 . .
C C18 0.63343(16) 0.3673(6) 0.8591(2) 0.0545(15) Uani d . 1 . .
H H18A 0.6497 0.3279 0.8503 0.065 Uiso calc R 1 . .
H H18B 0.6183 0.2918 0.8586 0.065 Uiso calc R 1 . .
C C19 0.57708(16) 0.4114(6) 0.7500(2) 0.0612(16) Uani d . 1 . .
H H19A 0.5544 0.4744 0.7238 0.073 Uiso calc R 1 . .
H H19B 0.5671 0.3237 0.7529 0.073 Uiso calc R 1 . .
C C20 0.59466(17) 0.3830(6) 0.7197(2) 0.0562(16) Uani d . 1 . .
H H20A 0.6226 0.3562 0.7510 0.067 Uiso calc R 1 . .
H H20B 0.5805 0.3047 0.6914 0.067 Uiso calc R 1 . .
C C21 0.56470(15) 0.7916(6) 0.7938(2) 0.0550(16) Uani d . 1 . .
H H21A 0.5499 0.8349 0.8046 0.066 Uiso calc R 1 . .
H H21B 0.5539 0.6979 0.7784 0.066 Uiso calc R 1 . .
C C22 0.55834(14) 0.8767(5) 0.7434(2) 0.0420(14) Uani d . 1 . .
C C23 0.57919(14) 0.8421(6) 0.7233(2) 0.0376(12) Uani d . 1 . .
C C24 0.57242(15) 0.9306(6) 0.6775(2) 0.0412(13) Uani d . 1 . .
C C25 0.54597(14) 1.0401(6) 0.6519(2) 0.0483(14) Uani d . 1 . .
H H25 0.5420 1.0943 0.6212 0.058 Uiso calc R 1 . .
C C26 0.52528(15) 1.0701(6) 0.6717(3) 0.0543(16) Uani d . 1 . .
H H26 0.5069 1.1437 0.6541 0.065 Uiso calc R 1 . .
C C27 0.53190(15) 0.9910(6) 0.7175(3) 0.0563(16) Uani d . 1 . .
H H27 0.5185 1.0136 0.7319 0.068 Uiso calc R 1 . .
C C28 0.5962(2) 0.9959(8) 0.6247(3) 0.0952(16) Uani d . 1 . .
H H28A 0.5704 0.9957 0.5840 0.143 Uiso calc R 1 . .
H H28B 0.6165 0.9706 0.6224 0.143 Uiso calc R 1 . .
H H28C 0.6017 1.0881 0.6422 0.143 Uiso calc R 1 . .
C C29 0.70348(15) 0.7592(6) 0.7475(2) 0.0519(15) Uani d . 1 . .
H H29A 0.7009 0.6591 0.7391 0.062 Uiso calc R 1 . .
H H29B 0.7314 0.7781 0.7826 0.062 Uiso calc R 1 . .
C C30 0.69241(16) 0.8374(6) 0.6927(3) 0.0483(14) Uani d . 1 . .
C C31 0.66558(19) 0.7776(7) 0.6360(3) 0.0632(17) Uani d . 1 . .
C C32 0.6551(2) 0.8495(8) 0.5839(3) 0.0768(19) Uani d . 1 . .
C C33 0.6706(2) 0.9770(8) 0.5890(4) 0.080(2) Uani d . 1 . .
H H33 0.6627 1.0250 0.5542 0.095 Uiso calc R 1 . .
C C34 0.6981(2) 1.0331(7) 0.6462(4) 0.081(2) Uani d . 1 . .
H H34 0.7097 1.1194 0.6505 0.097 Uiso calc R 1 . .
C C35 0.70907(18) 0.9656(7) 0.6977(3) 0.0659(17) Uani d . 1 . .
H H35 0.7279 1.0065 0.7363 0.079 Uiso calc R 1 . .
C C36 0.6178(2) 0.8226(8) 0.4753(3) 0.0952(16) Uani d . 1 . .
H H36A 0.6071 0.9164 0.4654 0.143 Uiso calc R 1 . .
H H36B 0.5984 0.7603 0.4423 0.143 Uiso calc R 1 . .
H H36C 0.6420 0.8212 0.4811 0.143 Uiso calc R 1 . .
C C37 0.62605(16) 0.9192(6) 0.8758(3) 0.0600(16) Uani d . 1 . .
H H37A 0.6216 0.9490 0.9035 0.072 Uiso calc R 1 . .
H H37B 0.6133 0.9870 0.8425 0.072 Uiso calc R 1 . .
C C38 0.67043(16) 0.9163(6) 0.9101(2) 0.0590(16) Uani d . 1 . .
H H38A 0.6812 1.0109 0.9226 0.071 Uiso calc R 1 . .
H H38B 0.6839 0.8594 0.9470 0.071 Uiso calc R 1 . .
C C39 0.67105(15) 0.9631(6) 0.8263(2) 0.0516(15) Uani d . 1 . .
H H39A 0.6805 1.0538 0.8467 0.062 Uiso calc R 1 . .
H H39B 0.6424 0.9708 0.7922 0.062 Uiso calc R 1 . .
C C40 0.69177(15) 0.9282(6) 0.8014(2) 0.0524(15) Uani d . 1 . .
H H40A 0.6877 1.0058 0.7758 0.063 Uiso calc R 1 . .
H H40B 0.7204 0.9212 0.8358 0.063 Uiso calc R 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
_geom_angle_publ_flag
O1 Ni1 O5 84.85(12) y
O1 Ni1 N4 171.59(16) y
O5 Ni1 N4 89.52(15) y
O1 Ni1 N1 89.02(14) y
O5 Ni1 N1 172.66(15) y
N4 Ni1 N1 97.00(16) y
O1 Ni1 N2 94.69(14) y
O5 Ni1 N2 95.09(14) y
N4 Ni1 N2 92.02(17) y
N1 Ni1 N2 81.37(16) y
O1 Ni1 N5 91.79(14) y
O5 Ni1 N5 91.33(14) y
N4 Ni1 N5 82.08(16) y
N1 Ni1 N5 92.89(16) y
N2 Ni1 N5 171.25(15) y
C17 N1 C1 113.3(4) ?
C17 N1 Ni1 110.0(3) ?
C1 N1 Ni1 114.0(3) ?
C17 N1 H1 106.3 ?
C1 N1 H1 106.3 ?
Ni1 N1 H1 106.3 ?
C18 N2 C19 111.4(4) ?
C18 N2 Ni1 106.7(3) ?
C19 N2 Ni1 124.9(3) ?
C18 N2 H2 103.9 ?
C19 N2 H2 103.9 ?
Ni1 N2 H2 103.9 ?
C9 N3 C20 115.5(4) ?
C9 N3 H3A 108.4 ?
C20 N3 H3A 108.4 ?
C9 N3 H3B 108.4 ?
C20 N3 H3B 108.4 ?
H3A N3 H3B 107.5 ?
C37 N4 C21 111.6(4) ?
C37 N4 Ni1 110.5(3) ?
C21 N4 Ni1 112.2(3) ?
C37 N4 H4 107.4 ?
C21 N4 H4 107.4 ?
Ni1 N4 H4 107.4 ?
C39 N5 C38 111.3(4) ?
C39 N5 Ni1 119.4(3) ?
C38 N5 Ni1 102.0(3) ?
C39 N5 H5 107.9 ?
C38 N5 H5 107.9 ?
Ni1 N5 H5 107.9 ?
C40 N6 C29 113.1(4) ?
C40 N6 H6A 109.0 ?
C29 N6 H6A 109.0 ?
C40 N6 H6B 109.0 ?
C29 N6 H6B 109.0 ?
H6A N6 H6B 107.8 ?
O9 N7 O10 118.3(6) ?
O9 N7 O11 121.7(6) ?
O10 N7 O11 120.0(5) ?
O12 N8 O14' 132.4(14) ?
O12 N8 O14 123.0(13) ?
O14' N8 O14 64.3(11) ?
O12 N8 O13 119.4(14) ?
O14' N8 O13 53.0(13) ?
O14 N8 O13 111.0(12) ?
O12 N8 O13' 112.0(9) ?
O14' N8 O13' 111.7(11) ?
O14 N8 O13' 101(2) ?
O13 N8 O13' 79.6(19) ?
C3 O1 Ni1 128.9(3) ?
C4 O2 C8 118.0(4) ?
C11 O3 H3 109.5 ?
C12 O4 C16 118.8(5) ?
C23 O5 Ni1 126.9(3) ?
C24 O6 C28 116.5(5) ?
C31 O7 H7 109.8 ?
C32 O8 C36 119.0(5) ?
H41 O15 H42 103.3 ?
N1 C1 C2 114.6(4) ?
N1 C1 H1A 108.6 ?
C2 C1 H1A 108.6 ?
N1 C1 H1B 108.6 ?
C2 C1 H1B 108.6 ?
H1A C1 H1B 107.6 ?
C7 C2 C3 119.8(5) ?
C7 C2 C1 120.0(5) ?
C3 C2 C1 120.0(5) ?
O1 C3 C2 122.2(5) ?
O1 C3 C4 119.0(5) ?
C2 C3 C4 118.7(5) ?
O2 C4 C5 124.1(5) ?
O2 C4 C3 115.6(5) ?
C5 C4 C3 120.4(5) ?
C6 C5 C4 119.8(5) ?
C6 C5 H5A 120.1 ?
C4 C5 H5A 120.1 ?
C7 C6 C5 120.2(6) ?
C7 C6 H6 119.9 ?
C5 C6 H6 119.9 ?
C6 C7 C2 121.1(5) ?
C6 C7 H7A 119.5 ?
C2 C7 H7A 119.5 ?
O2 C8 H8A 109.5 ?
O2 C8 H8B 109.5 ?
H8A C8 H8B 109.5 ?
O2 C8 H8C 109.5 ?
H8A C8 H8C 109.5 ?
H8B C8 H8C 109.5 ?
N3 C9 C10 114.0(4) ?
N3 C9 H9A 108.8 ?
C10 C9 H9A 108.8 ?
N3 C9 H9B 108.8 ?
C10 C9 H9B 108.8 ?
H9A C9 H9B 107.7 ?
C11 C10 C15 118.3(5) ?
C11 C10 C9 119.8(5) ?
C15 C10 C9 121.8(5) ?
O3 C11 C10 117.2(5) ?
O3 C11 C12 121.5(5) ?
C10 C11 C12 121.3(5) ?
O4 C12 C13 126.4(6) ?
O4 C12 C11 114.3(5) ?
C13 C12 C11 119.3(6) ?
C12 C13 C14 119.3(6) ?
C12 C13 H13 120.4 ?
C14 C13 H13 120.4 ?
C15 C14 C13 121.2(6) ?
C15 C14 H14 119.4 ?
C13 C14 H14 119.4 ?
C14 C15 C10 120.7(6) ?
C14 C15 H15 119.7 ?
C10 C15 H15 119.7 ?
O4 C16 H16A 109.5 ?
O4 C16 H16B 109.5 ?
H16A C16 H16B 109.5 ?
O4 C16 H16C 109.5 ?
H16A C16 H16C 109.5 ?
H16B C16 H16C 109.5 ?
N1 C17 C18 111.8(4) ?
N1 C17 H17A 109.3 ?
C18 C17 H17A 109.3 ?
N1 C17 H17B 109.3 ?
C18 C17 H17B 109.3 ?
H17A C17 H17B 107.9 ?
N2 C18 C17 108.2(5) ?
N2 C18 H18A 110.1 ?
C17 C18 H18A 110.1 ?
N2 C18 H18B 110.1 ?
C17 C18 H18B 110.1 ?
H18A C18 H18B 108.4 ?
N2 C19 C20 114.3(4) ?
N2 C19 H19A 108.7 ?
C20 C19 H19A 108.7 ?
N2 C19 H19B 108.7 ?
C20 C19 H19B 108.7 ?
H19A C19 H19B 107.6 ?
N3 C20 C19 112.5(5) ?
N3 C20 H20A 109.1 ?
C19 C20 H20A 109.1 ?
N3 C20 H20B 109.1 ?
C19 C20 H20B 109.1 ?
H20A C20 H20B 107.8 ?
N4 C21 C22 113.1(4) ?
N4 C21 H21A 109.0 ?
C22 C21 H21A 109.0 ?
N4 C21 H21B 109.0 ?
C22 C21 H21B 109.0 ?
H21A C21 H21B 107.8 ?
C23 C22 C27 120.3(5) ?
C23 C22 C21 119.9(5) ?
C27 C22 C21 119.8(5) ?
O5 C23 C22 123.7(5) ?
O5 C23 C24 120.4(4) ?
C22 C23 C24 115.9(5) ?
C25 C24 O6 123.3(5) ?
C25 C24 C23 123.1(5) ?
O6 C24 C23 113.5(5) ?
C24 C25 C26 119.7(5) ?
C24 C25 H25 120.1 ?
C26 C25 H25 120.1 ?
C27 C26 C25 119.4(5) ?
C27 C26 H26 120.3 ?
C25 C26 H26 120.3 ?
C26 C27 C22 121.5(5) ?
C26 C27 H27 119.2 ?
C22 C27 H27 119.2 ?
O6 C28 H28A 109.5 ?
O6 C28 H28B 109.5 ?
H28A C28 H28B 109.5 ?
O6 C28 H28C 109.5 ?
H28A C28 H28C 109.5 ?
H28B C28 H28C 109.5 ?
N6 C29 C30 114.2(4) ?
N6 C29 H29A 108.7 ?
C30 C29 H29A 108.7 ?
N6 C29 H29B 108.7 ?
C30 C29 H29B 108.7 ?
H29A C29 H29B 107.6 ?
C31 C30 C35 118.9(6) ?
C31 C30 C29 118.5(6) ?
C35 C30 C29 122.6(6) ?
O7 C31 C30 120.0(6) ?
O7 C31 C32 120.9(6) ?
C30 C31 C32 119.2(6) ?
C33 C32 O8 126.2(7) ?
C33 C32 C31 121.6(6) ?
O8 C32 C31 112.1(6) ?
C32 C33 C34 118.3(7) ?
C32 C33 H33 120.9 ?
C34 C33 H33 120.9 ?
C33 C34 C35 121.5(7) ?
C33 C34 H34 119.2 ?
C35 C34 H34 119.2 ?
C34 C35 C30 120.5(6) ?
C34 C35 H35 119.7 ?
C30 C35 H35 119.7 ?
O8 C36 H36A 109.5 ?
O8 C36 H36B 109.5 ?
H36A C36 H36B 109.5 ?
O8 C36 H36C 109.5 ?
H36A C36 H36C 109.5 ?
H36B C36 H36C 109.5 ?
N4 C37 C38 111.3(5) ?
N4 C37 H37A 109.4 ?
C38 C37 H37A 109.4 ?
N4 C37 H37B 109.4 ?
C38 C37 H37B 109.4 ?
H37A C37 H37B 108.0 ?
N5 C38 C37 110.1(4) ?
N5 C38 H38A 109.6 ?
C37 C38 H38A 109.6 ?
N5 C38 H38B 109.6 ?
C37 C38 H38B 109.6 ?
H38A C38 H38B 108.1 ?
N5 C39 C40 113.0(4) ?
N5 C39 H39A 109.0 ?
C40 C39 H39A 109.0 ?
N5 C39 H39B 109.0 ?
C40 C39 H39B 109.0 ?
H39A C39 H39B 107.8 ?
N6 C40 C39 115.9(4) ?
N6 C40 H40A 108.3 ?
C39 C40 H40A 108.3 ?
N6 C40 H40B 108.3 ?
C39 C40 H40B 108.3 ?
H40A C40 H40B 107.4 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 O1 2.025(3) y
Ni1 O5 2.041(3) y
Ni1 N4 2.102(4) y
Ni1 N1 2.110(4) y
Ni1 N2 2.184(4) y
Ni1 N5 2.212(4) y
N1 C17 1.468(6) ?
N1 C1 1.485(6) ?
N1 H1 0.9100 ?
N2 C18 1.478(6) ?
N2 C19 1.483(6) ?
N2 H2 0.9100 ?
N3 C9 1.491(6) ?
N3 C20 1.491(6) ?
N3 H3A 0.9000 ?
N3 H3B 0.9000 ?
N4 C37 1.470(7) ?
N4 C21 1.492(6) ?
N4 H4 0.9100 ?
N5 C39 1.480(6) ?
N5 C38 1.485(6) ?
N5 H5 0.9100 ?
N6 C40 1.489(6) ?
N6 C29 1.497(5) ?
N6 H6A 0.9000 ?
N6 H6B 0.9000 ?
N7 O9 1.229(11) ?
N7 O10 1.229(5) ?
N7 O11 1.235(6) ?
N8 O12 1.093(10) ?
N8 O14' 1.148(10) ?
N8 O14 1.178(12) ?
N8 O13 1.266(13) ?
N8 O13' 1.310(12) ?
O1 C3 1.344(5) ?
O2 C4 1.369(6) ?
O2 C8 1.428(6) ?
O3 C11 1.355(6) ?
O3 H3 0.8200 ?
O4 C12 1.367(6) ?
O4 C16 1.413(6) ?
O5 C23 1.333(5) ?
O6 C24 1.402(6) ?
O6 C28 1.421(7) ?
O7 C31 1.357(7) ?
O7 H7 0.8200 ?
O8 C32 1.381(7) ?
O8 C36 1.403(6) ?
O15 H41 0.8501 ?
O15 H42 0.8501 ?
O16 H43 0.8500 ?
C1 C2 1.500(7) ?
C1 H1A 0.9700 ?
C1 H1B 0.9700 ?
C2 C7 1.388(7) ?
C2 C3 1.393(6) ?
C3 C4 1.405(6) ?
C4 C5 1.390(7) ?
C5 C6 1.379(7) ?
C5 H5A 0.9300 ?
C6 C7 1.367(7) ?
C6 H6 0.9300 ?
C7 H7A 0.9300 ?
C8 H8A 0.9600 ?
C8 H8B 0.9600 ?
C8 H8C 0.9600 ?
C9 C10 1.503(7) ?
C9 H9A 0.9700 ?
C9 H9B 0.9700 ?
C10 C11 1.376(7) ?
C10 C15 1.382(7) ?
C11 C12 1.386(7) ?
C12 C13 1.375(7) ?
C13 C14 1.376(7) ?
C13 H13 0.9300 ?
C14 C15 1.356(8) ?
C14 H14 0.9300 ?
C15 H15 0.9300 ?
C16 H16A 0.9600 ?
C16 H16B 0.9600 ?
C16 H16C 0.9600 ?
C17 C18 1.510(7) ?
C17 H17A 0.9700 ?
C17 H17B 0.9700 ?
C18 H18A 0.9700 ?
C18 H18B 0.9700 ?
C19 C20 1.504(7) ?
C19 H19A 0.9700 ?
C19 H19B 0.9700 ?
C20 H20A 0.9700 ?
C20 H20B 0.9700 ?
C21 C22 1.510(7) ?
C21 H21A 0.9700 ?
C21 H21B 0.9700 ?
C22 C23 1.393(6) ?
C22 C27 1.399(7) ?
C23 C24 1.412(7) ?
C24 C25 1.364(6) ?
C25 C26 1.370(6) ?
C25 H25 0.9300 ?
C26 C27 1.364(7) ?
C26 H26 0.9300 ?
C27 H27 0.9300 ?
C28 H28A 0.9600 ?
C28 H28B 0.9600 ?
C28 H28C 0.9600 ?
C29 C30 1.499(7) ?
C29 H29A 0.9700 ?
C29 H29B 0.9700 ?
C30 C31 1.361(7) ?
C30 C35 1.379(7) ?
C31 C32 1.414(8) ?
C32 C33 1.350(8) ?
C33 C34 1.359(8) ?
C33 H33 0.9300 ?
C34 C35 1.372(8) ?
C34 H34 0.9300 ?
C35 H35 0.9300 ?
C36 H36A 0.9600 ?
C36 H36B 0.9600 ?
C36 H36C 0.9600 ?
C37 C38 1.504(7) ?
C37 H37A 0.9700 ?
C37 H37B 0.9700 ?
C38 H38A 0.9700 ?
C38 H38B 0.9700 ?
C39 C40 1.506(6) ?
C39 H39A 0.9700 ?
C39 H39B 0.9700 ?
C40 H40A 0.9700 ?
C40 H40B 0.9700 ?
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
N1 H1 O9 7_667 0.91 2.38 3.122(6) 139.1
N1 H1 O10 7_667 0.91 2.31 3.163(6) 156.1
N2 H2 O13' 6_566 0.91 2.14 2.976(11) 152.0
N4 H4 O12 6_566 0.91 2.21 3.021(8) 147.9
O15 H42 O10 4_646 0.85 2.32 3.013(6) 138.3
O15 H42 O11 4_646 0.85 2.14 2.965(6) 163.0
C9 H9B O14' 5_666 0.97 2.48 3.420(10) 162.7
C17 H17A O12 6_566 0.97 2.59 3.445(9) 147.2
C34 H34 O11 4_656 0.93 2.59 3.419(8) 148.9
O16 H43 O13' 5_666 0.85 1.66 2.464(17) 155.8
O3 H3 O15 . 0.82 1.98 2.653(5) 138.5
O3 H3 O4 . 0.82 2.21 2.659(5) 114.7
N3 H3A O5 . 0.90 1.73 2.617(5) 167.9
N3 H3B O2 . 0.90 2.53 3.211(5) 132.6
N3 H3B O3 . 0.90 2.23 2.838(5) 124.2
N5 H5 O9 . 0.91 2.24 3.123(6) 164.6
N6 H6A O5 . 0.90 2.49 2.936(5) 111.3
N6 H6A O6 . 0.90 2.10 2.961(6) 160.5
N6 H6B O1 . 0.90 1.72 2.612(5) 169.3
O7 H7 O8 . 0.82 2.20 2.633(6) 113.3
O7 H7 O15 . 0.82 2.13 2.872(6) 150.5
O15 H41 O12 . 0.85 2.21 3.037(8) 165.8
C1 H1B O9 . 0.97 2.49 3.438(7) 164.6
C29 H29A O2 . 0.97 2.50 3.382(6) 150.5
C29 H29A O7 . 0.97 2.39 2.757(7) 102.1
C40 H40B O9 . 0.97 2.56 3.369(7) 140.9
C40 H40B O11 . 0.97 2.53 3.456(7) 160.3
C39 H39B O5 . 0.97 2.55 3.087(6) 115.0
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
O1 Ni1 N1 C17 -101.5(3)
N4 Ni1 N1 C17 84.4(3)
N2 Ni1 N1 C17 -6.6(3)
N5 Ni1 N1 C17 166.8(3)
O1 Ni1 N1 C1 27.1(4)
N4 Ni1 N1 C1 -147.0(4)
N2 Ni1 N1 C1 122.0(4)
N5 Ni1 N1 C1 -64.7(4)
O1 Ni1 N2 C18 67.5(3)
O5 Ni1 N2 C18 152.8(3)
N4 Ni1 N2 C18 -117.5(3)
N1 Ni1 N2 C18 -20.7(3)
O1 Ni1 N2 C19 -64.8(4)
O5 Ni1 N2 C19 20.4(4)
N4 Ni1 N2 C19 110.1(4)
N1 Ni1 N2 C19 -153.1(4)
O5 Ni1 N4 C37 -92.2(3)
N1 Ni1 N4 C37 91.1(4)
N2 Ni1 N4 C37 172.7(3)
N5 Ni1 N4 C37 -0.8(3)
O5 Ni1 N4 C21 33.0(3)
N1 Ni1 N4 C21 -143.6(3)
N2 Ni1 N4 C21 -62.0(3)
N5 Ni1 N4 C21 124.5(3)
O1 Ni1 N5 C39 78.0(3)
O5 Ni1 N5 C39 -6.9(3)
N4 Ni1 N5 C39 -96.2(4)
N1 Ni1 N5 C39 167.1(3)
O1 Ni1 N5 C38 -158.9(3)
O5 Ni1 N5 C38 116.2(3)
N4 Ni1 N5 C38 26.9(3)
N1 Ni1 N5 C38 -69.8(3)
O5 Ni1 O1 C3 -159.8(4)
N1 Ni1 O1 C3 16.1(4)
N2 Ni1 O1 C3 -65.1(4)
N5 Ni1 O1 C3 109.0(4)
O1 Ni1 O5 C23 -161.8(4)
N4 Ni1 O5 C23 12.0(4)
N2 Ni1 O5 C23 104.0(4)
N5 Ni1 O5 C23 -70.1(4)
C17 N1 C1 C2 64.7(6)
Ni1 N1 C1 C2 -62.1(5)
N1 C1 C2 C7 -130.7(5)
N1 C1 C2 C3 55.0(7)
Ni1 O1 C3 C2 -29.2(6)
Ni1 O1 C3 C4 149.2(4)
C7 C2 C3 O1 179.6(4)
C1 C2 C3 O1 -6.1(7)
C7 C2 C3 C4 1.2(7)
C1 C2 C3 C4 175.5(5)
C8 O2 C4 C5 0.5(7)
C8 O2 C4 C3 179.4(4)
O1 C3 C4 O2 1.1(7)
C2 C3 C4 O2 179.6(4)
O1 C3 C4 C5 -179.9(4)
C2 C3 C4 C5 -1.4(7)
O2 C4 C5 C6 -179.8(5)
C3 C4 C5 C6 1.3(8)
C4 C5 C6 C7 -0.9(9)
C5 C6 C7 C2 0.7(9)
C3 C2 C7 C6 -0.9(8)
C1 C2 C7 C6 -175.2(5)
C20 N3 C9 C10 -58.8(6)
N3 C9 C10 C11 -58.7(7)
N3 C9 C10 C15 125.1(5)
C15 C10 C11 O3 179.6(5)
C9 C10 C11 O3 3.2(7)
C15 C10 C11 C12 1.0(8)
C9 C10 C11 C12 -175.4(5)
C16 O4 C12 C13 15.4(9)
C16 O4 C12 C11 -167.4(5)
O3 C11 C12 O4 2.4(8)
C10 C11 C12 O4 -179.0(5)
O3 C11 C12 C13 179.8(5)
C10 C11 C12 C13 -1.6(8)
O4 C12 C13 C14 179.1(5)
C11 C12 C13 C14 2.0(9)
C12 C13 C14 C15 -1.9(9)
C13 C14 C15 C10 1.3(9)
C11 C10 C15 C14 -0.8(8)
C9 C10 C15 C14 175.5(5)
C1 N1 C17 C18 -95.6(5)
Ni1 N1 C17 C18 33.3(5)
C19 N2 C18 C17 -177.0(4)
Ni1 N2 C18 C17 43.6(5)
N1 C17 C18 N2 -52.6(6)
C18 N2 C19 C20 -77.6(6)
Ni1 N2 C19 C20 53.0(6)
C9 N3 C20 C19 -75.2(5)
N2 C19 C20 N3 -87.0(6)
C37 N4 C21 C22 58.1(6)
Ni1 N4 C21 C22 -66.5(5)
N4 C21 C22 C23 53.5(6)
N4 C21 C22 C27 -125.7(5)
Ni1 O5 C23 C22 -30.3(6)
Ni1 O5 C23 C24 146.3(4)
C27 C22 C23 O5 178.1(4)
C21 C22 C23 O5 -1.1(7)
C27 C22 C23 C24 1.4(7)
C21 C22 C23 C24 -177.8(4)
C28 O6 C24 C25 9.0(7)
C28 O6 C24 C23 -169.4(5)
O5 C23 C24 C25 -179.6(4)
C22 C23 C24 C25 -2.8(7)
O5 C23 C24 O6 -1.1(6)
C22 C23 C24 O6 175.7(4)
O6 C24 C25 C26 -176.7(5)
C23 C24 C25 C26 1.6(8)
C24 C25 C26 C27 1.0(8)
C25 C26 C27 C22 -2.2(8)
C23 C22 C27 C26 1.0(8)
C21 C22 C27 C26 -179.8(5)
C40 N6 C29 C30 -81.1(6)
N6 C29 C30 C31 -92.7(6)
N6 C29 C30 C35 88.9(6)
C35 C30 C31 O7 -179.4(5)
C29 C30 C31 O7 2.2(8)
C35 C30 C31 C32 -1.1(9)
C29 C30 C31 C32 -179.5(5)
C36 O8 C32 C33 15.4(10)
C36 O8 C32 C31 -168.7(5)
O7 C31 C32 C33 177.4(6)
C30 C31 C32 C33 -1.0(10)
O7 C31 C32 O8 1.3(9)
C30 C31 C32 O8 -177.1(5)
O8 C32 C33 C34 178.1(6)
C31 C32 C33 C34 2.5(10)
C32 C33 C34 C35 -2.1(10)
C33 C34 C35 C30 0.1(10)
C31 C30 C35 C34 1.5(9)
C29 C30 C35 C34 179.8(5)
C21 N4 C37 C38 -152.0(4)
Ni1 N4 C37 C38 -26.4(5)
C39 N5 C38 C37 79.4(5)
Ni1 N5 C38 C37 -49.1(5)
N4 C37 C38 N5 53.2(6)
C38 N5 C39 C40 159.5(4)
Ni1 N5 C39 C40 -82.1(5)
C29 N6 C40 C39 -173.2(4)
N5 C39 C40 N6 63.0(6)
