#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:03:05 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180057 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/03/7050387.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_7050387
loop_
_publ_author_name
'Dariusz Pawlica'
'Marek Marszałek'
'Grzegorz Mynarczuk'
'Lesław Sieroń'
'Julita Eilmes'
_publ_section_title
;
 New unsymmetrical Schiff base Ni(II) complexes as scaffolds for
 dendritic and amino acid superstructures
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              1615
_journal_page_last               1621
_journal_paper_doi               10.1039/b409298h
_journal_volume                  28
_journal_year                    2004
_chemical_formula_moiety         'C37 H35 N3 Ni O6, 2(H2 O)'
_chemical_formula_sum            'C37 H39 N3 Ni O8'
_chemical_formula_weight         712.42
_chemical_name_systematic
;[8-(3'-Boc-(L)-phenylalanyloxy-2'-hydroxyphenyl)-(5,6)
-benzo-3-methyl-1-phenyl-4,7-diazaocta-2,7-dien-1
-onato(2-)]nickel(II) dihydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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
_cell_angle_beta                 114.2092(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.8152(3)
_cell_length_b                   7.57810(10)
_cell_length_c                   22.9560(4)
_cell_measurement_reflns_used    9776
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      64.81
_cell_measurement_theta_min      3.64
_cell_volume                     3461.28(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_type            CCD
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29857
_diffrn_reflns_theta_full        65.83
_diffrn_reflns_theta_max         65.83
_diffrn_reflns_theta_min         2.11
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.278
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         10952
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0683P)²+0.1116P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1205
_reflns_number_gt                8527
_reflns_number_total             10952
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b409298h.txt
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7050387
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.87274(3) 0.71981(8) 0.88595(3) 0.06288(19) Uani 1 1 d . . .
O1 O 0.78956(12) 0.6236(4) 0.87084(11) 0.0645(7) Uani 1 1 d . . .
O2 O 0.87163(12) 0.7844(4) 0.96308(11) 0.0707(8) Uani 1 1 d . . .
O3 O 0.67627(11) 0.4863(4) 0.87191(11) 0.0616(7) Uani 1 1 d . . .
O4 O 0.75244(13) 0.2751(4) 0.92155(12) 0.0725(7) Uani 1 1 d . . .
O5 O 0.60265(14) 0.1995(4) 0.93148(16) 0.0880(9) Uani 1 1 d . . .
O6 O 0.52580(12) 0.4098(4) 0.92455(13) 0.0749(8) Uani 1 1 d . . .
O7 O 0.6286(3) 0.8444(6) 0.9577(3) 0.185(2) Uani 1 1 d . . .
H71 H 0.6575 0.8665 0.9445 0.222 Uiso 1 1 d . . .
H72 H 0.6001 0.9202 0.9415 0.222 Uiso 1 1 d . . .
O8 O 0.71820(14) 0.8986(5) 0.90367(14) 0.0844(9) Uani 1 1 d . . .
H81 H 0.7394 0.9883 0.9189 0.101 Uiso 1 1 d . . .
H82 H 0.7457 0.8212 0.9067 0.101 Uiso 1 1 d . . .
N1 N 0.86863(14) 0.6709(4) 0.80668(15) 0.0605(8) Uani 1 1 d . . .
N2 N 0.96011(15) 0.7987(5) 0.90619(15) 0.0669(8) Uani 1 1 d . . .
N3 N 0.63307(15) 0.4775(5) 0.96671(14) 0.0615(8) Uani 1 1 d . . .
H30 H 0.6201 0.5779 0.9750 0.074 Uiso 1 1 calc R . .
C1 C 0.92479(19) 0.7428(6) 0.7963(2) 0.0678(11) Uani 1 1 d . . .
C2 C 0.9299(2) 0.7499(7) 0.7380(2) 0.0841(14) Uani 1 1 d . . .
H2 H 0.8975 0.6968 0.7020 0.101 Uiso 1 1 calc R . .
C3 C 0.9836(2) 0.8364(9) 0.7340(2) 0.0984(17) Uani 1 1 d . . .
H3 H 0.9889 0.8373 0.6958 0.118 Uiso 1 1 calc R . .
C4 C 1.0294(3) 0.9214(9) 0.7868(3) 0.1062(18) Uani 1 1 d . . .
H4 H 1.0644 0.9843 0.7833 0.127 Uiso 1 1 calc R . .
C5 C 1.0246(2) 0.9152(7) 0.8453(3) 0.0905(15) Uani 1 1 d . . .
H5 H 1.0553 0.9763 0.8802 0.109 Uiso 1 1 calc R . .
C6 C 0.97316(19) 0.8162(6) 0.8516(2) 0.0711(11) Uani 1 1 d . . .
C7 C 0.74843(18) 0.5468(6) 0.81845(17) 0.0590(10) Uani 1 1 d . . .
C8 C 0.68844(17) 0.4697(6) 0.81733(17) 0.0582(9) Uani 1 1 d . . .
C9 C 0.64178(18) 0.3906(6) 0.76408(18) 0.0662(11) Uani 1 1 d . . .
H9 H 0.6033 0.3414 0.7654 0.079 Uiso 1 1 calc R . .
C10 C 0.6515(2) 0.3833(6) 0.70744(19) 0.0699(11) Uani 1 1 d . . .
H10 H 0.6195 0.3317 0.6708 0.084 Uiso 1 1 calc R . .
C11 C 0.7088(2) 0.4534(6) 0.70729(19) 0.0680(11) Uani 1 1 d . . .
H11 H 0.7153 0.4487 0.6697 0.082 Uiso 1 1 calc R . .
C12 C 0.75913(18) 0.5332(5) 0.76181(18) 0.0611(10) Uani 1 1 d . . .
C13 C 0.8193(2) 0.5998(6) 0.75885(19) 0.0637(11) Uani 1 1 d . . .
H13 H 0.8232 0.5915 0.7201 0.076 Uiso 1 1 calc R . .
C14 C 0.9235(2) 0.8225(6) 1.0150(2) 0.0707(11) Uani 1 1 d . . .
C15 C 0.9877(2) 0.8256(7) 1.0179(2) 0.0747(11) Uani 1 1 d . . .
H15 H 1.0226 0.8359 1.0583 0.090 Uiso 1 1 calc R . .
C16 C 1.0057(2) 0.8147(7) 0.9658(2) 0.0749(11) Uani 1 1 d . . .
C17 C 1.08095(19) 0.8165(8) 0.9838(2) 0.0952(15) Uani 1 1 d . . .
H17A H 1.0900 0.7627 0.9503 0.114 Uiso 1 1 calc R . .
H17B H 1.1035 0.7517 1.0228 0.114 Uiso 1 1 calc R . .
H17C H 1.0968 0.9361 0.9897 0.114 Uiso 1 1 calc R . .
C21 C 0.9084(2) 0.8658(6) 1.0708(2) 0.0728(11) Uani 1 1 d . . .
C22 C 0.9583(3) 0.8883(9) 1.1324(2) 0.1019(18) Uani 1 1 d . . .
H22 H 1.0032 0.8733 1.1397 0.122 Uiso 1 1 calc R . .
C23 C 0.9423(3) 0.9314(9) 1.1815(2) 0.1102(19) Uani 1 1 d . . .
H23 H 0.9763 0.9448 1.2222 0.132 Uiso 1 1 calc R . .
C24 C 0.8764(3) 0.9558(8) 1.1721(2) 0.1085(18) Uani 1 1 d . . .
H24 H 0.8658 0.9891 1.2059 0.130 Uiso 1 1 calc R . .
C25 C 0.8274(3) 0.9310(8) 1.1133(2) 0.1125(19) Uani 1 1 d . . .
H25 H 0.7826 0.9442 1.1066 0.135 Uiso 1 1 calc R . .
C26 C 0.8435(2) 0.8858(8) 1.0628(2) 0.0931(15) Uani 1 1 d . . .
H26 H 0.8091 0.8688 1.0225 0.112 Uiso 1 1 calc R . .
C30 C 0.71439(19) 0.3882(6) 0.92291(19) 0.0589(9) Uani 1 1 d . . .
C31 C 0.70424(17) 0.4465(5) 0.98158(17) 0.0633(10) Uani 1 1 d . . .
H31 H 0.7269 0.5607 0.9944 0.076 Uiso 1 1 calc R . .
C32 C 0.5884(2) 0.3482(6) 0.9400(2) 0.0653(10) Uani 1 1 d . . .
C33 C 0.4676(2) 0.2872(7) 0.89888(18) 0.0768(12) Uani 1 1 d . . .
C34 C 0.4722(2) 0.1526(8) 0.9488(2) 0.1061(17) Uani 1 1 d . . .
H34A H 0.5037 0.0623 0.9502 0.127 Uiso 1 1 calc R . .
H34B H 0.4288 0.1007 0.9381 0.127 Uiso 1 1 calc R . .
H34C H 0.4871 0.2091 0.9897 0.127 Uiso 1 1 calc R . .
C35 C 0.4087(2) 0.4082(8) 0.8858(2) 0.1120(19) Uani 1 1 d . . .
H35A H 0.4139 0.4674 0.9246 0.134 Uiso 1 1 calc R . .
H35B H 0.3679 0.3404 0.8703 0.134 Uiso 1 1 calc R . .
H35C H 0.4066 0.4939 0.8543 0.134 Uiso 1 1 calc R . .
C36 C 0.4637(2) 0.2057(8) 0.83726(19) 0.0983(14) Uani 1 1 d . . .
H36A H 0.4614 0.2975 0.8076 0.118 Uiso 1 1 calc R . .
H36B H 0.4243 0.1331 0.8193 0.118 Uiso 1 1 calc R . .
H36C H 0.5029 0.1349 0.8458 0.118 Uiso 1 1 calc R . .
C40 C 0.73874(19) 0.3208(6) 1.03715(17) 0.0780(11) Uani 1 1 d . . .
H40A H 0.7176 0.2057 1.0260 0.094 Uiso 1 1 calc R . .
H40B H 0.7854 0.3077 1.0439 0.094 Uiso 1 1 calc R . .
C41 C 0.7360(2) 0.3813(7) 1.09872(19) 0.0785(12) Uani 1 1 d . . .
C42 C 0.7784(2) 0.5031(10) 1.1361(2) 0.1105(18) Uani 1 1 d . . .
H42 H 0.8115 0.5493 1.1249 0.133 Uiso 1 1 calc R . .
C43 C 0.7734(3) 0.5615(12) 1.1915(3) 0.137(3) Uani 1 1 d . . .
H43 H 0.8017 0.6503 1.2159 0.164 Uiso 1 1 calc R . .
C44 C 0.7278(3) 0.4898(10) 1.2095(2) 0.1145(19) Uani 1 1 d . . .
H44 H 0.7271 0.5228 1.2482 0.137 Uiso 1 1 calc R . .
C45 C 0.6841(3) 0.3734(10) 1.1733(3) 0.1095(18) Uani 1 1 d . . .
H45 H 0.6508 0.3305 1.1850 0.131 Uiso 1 1 calc R . .
C46 C 0.6878(2) 0.3142(8) 1.1167(2) 0.0962(14) Uani 1 1 d . . .
H46 H 0.6576 0.2297 1.0914 0.115 Uiso 1 1 calc R . .
Ni' Ni 0.62800(3) 0.81175(8) 0.61805(3) 0.06210(18) Uani 1 1 d . . .
O1' O 0.70895(12) 0.9171(4) 0.63205(11) 0.0644(7) Uani 1 1 d . . .
O2' O 0.63104(12) 0.7393(4) 0.54295(11) 0.0688(7) Uani 1 1 d . . .
O3' O 0.82349(12) 1.0632(4) 0.63062(12) 0.0652(7) Uani 1 1 d . . .
O4' O 0.75170(15) 1.2849(5) 0.58652(14) 0.0892(9) Uani 1 1 d . . .
O5' O 0.92307(16) 1.3559(5) 0.5644(2) 0.1155(12) Uani 1 1 d . . .
O6' O 0.98470(12) 1.1090(4) 0.58066(13) 0.0770(8) Uani 1 1 d . . .
O7' O 0.8781(3) 0.7086(7) 0.5583(3) 0.189(2) Uani 1 1 d . . .
H71' H 0.8482 0.6716 0.5677 0.227 Uiso 1 1 d . . .
H72' H 0.9039 0.6246 0.5648 0.227 Uiso 1 1 d . . .
O8' O 0.78447(18) 0.6512(6) 0.60379(17) 0.1082(12) Uani 1 1 d . . .
H81' H 0.7828 0.5450 0.5958 0.130 Uiso 1 1 d . . .
H82' H 0.7489 0.6710 0.6072 0.130 Uiso 1 1 d . . .
N1' N 0.63150(15) 0.8646(5) 0.69800(15) 0.0628(9) Uani 1 1 d . . .
N2' N 0.54191(15) 0.7238(5) 0.59895(15) 0.0674(9) Uani 1 1 d . . .
N3' N 0.87514(16) 1.0889(5) 0.54303(15) 0.0649(9) Uani 1 1 d . . .
H30' H 0.8810 0.9776 0.5400 0.078 Uiso 1 1 calc R . .
C1' C 0.57595(19) 0.7937(6) 0.7080(2) 0.0677(10) Uani 1 1 d . . .
C2' C 0.5704(2) 0.7932(8) 0.7666(2) 0.0809(13) Uani 1 1 d . . .
H2' H 0.6014 0.8531 0.8016 0.097 Uiso 1 1 calc R . .
C3' C 0.5177(2) 0.7018(8) 0.7714(3) 0.0976(16) Uani 1 1 d . . .
H3' H 0.5129 0.6992 0.8098 0.117 Uiso 1 1 calc R . .
C4' C 0.4732(3) 0.6161(8) 0.7196(3) 0.1014(18) Uani 1 1 d . . .
H4' H 0.4382 0.5543 0.7234 0.122 Uiso 1 1 calc R . .
C5' C 0.4774(2) 0.6166(7) 0.6618(3) 0.0901(15) Uani 1 1 d . . .
H5' H 0.4465 0.5533 0.6277 0.108 Uiso 1 1 calc R . .
C6' C 0.52831(19) 0.7125(6) 0.6544(2) 0.0714(11) Uani 1 1 d . . .
C7' C 0.75108(18) 0.9935(5) 0.68456(17) 0.0592(9) Uani 1 1 d . . .
C8' C 0.81031(18) 1.0741(6) 0.68627(17) 0.0600(10) Uani 1 1 d . . .
C9' C 0.8582(2) 1.1458(6) 0.73960(18) 0.0699(11) Uani 1 1 d . . .
H9' H 0.8974 1.1917 0.7388 0.084 Uiso 1 1 calc R . .
C10' C 0.8479(2) 1.1497(6) 0.79590(19) 0.0720(12) Uani 1 1 d . . .
H10' H 0.8803 1.1983 0.8329 0.086 Uiso 1 1 calc R . .
C11' C 0.7904(2) 1.0825(6) 0.79643(18) 0.0649(10) Uani 1 1 d . . .
H11' H 0.7835 1.0877 0.8338 0.078 Uiso 1 1 calc R . .
C12' C 0.74133(18) 1.0054(6) 0.74170(16) 0.0583(10) Uani 1 1 d . . .
C13' C 0.68171(19) 0.9379(6) 0.74453(18) 0.0633(10) Uani 1 1 d . . .
H13' H 0.6783 0.9473 0.7835 0.076 Uiso 1 1 calc R . .
C14' C 0.5797(2) 0.6905(6) 0.49193(19) 0.0671(11) Uani 1 1 d . . .
C15' C 0.5155(2) 0.6813(6) 0.4884(2) 0.0771(12) Uani 1 1 d . . .
H15' H 0.4814 0.6613 0.4482 0.093 Uiso 1 1 calc R . .
C16' C 0.4961(2) 0.6985(6) 0.5383(2) 0.0750(12) Uani 1 1 d . . .
C17' C 0.4219(2) 0.6857(8) 0.5210(2) 0.0958(15) Uani 1 1 d . . .
H17D H 0.4100 0.5648 0.5234 0.115 Uiso 1 1 calc R . .
H17E H 0.3975 0.7289 0.4784 0.115 Uiso 1 1 calc R . .
H17F H 0.4108 0.7552 0.5503 0.115 Uiso 1 1 calc R . .
C21' C 0.5956(2) 0.6375(6) 0.4375(2) 0.0709(11) Uani 1 1 d . . .
C22' C 0.5471(3) 0.6426(8) 0.3745(2) 0.0897(15) Uani 1 1 d . . .
H22' H 0.5044 0.6873 0.3655 0.108 Uiso 1 1 calc R . .
C23' C 0.5629(3) 0.5808(10) 0.3255(3) 0.117(2) Uani 1 1 d . . .
H23' H 0.5305 0.5852 0.2837 0.140 Uiso 1 1 calc R . .
C24' C 0.6245(4) 0.5141(9) 0.3367(3) 0.120(2) Uani 1 1 d . . .
H24' H 0.6339 0.4729 0.3031 0.144 Uiso 1 1 calc R . .
C25' C 0.6725(3) 0.5081(8) 0.3979(3) 0.1142(18) Uani 1 1 d . . .
H25' H 0.7147 0.4616 0.4061 0.137 Uiso 1 1 calc R . .
C26' C 0.6584(2) 0.5716(7) 0.4484(2) 0.0905(14) Uani 1 1 d . . .
H26' H 0.6918 0.5693 0.4898 0.109 Uiso 1 1 calc R . .
C30' C 0.79157(19) 1.1807(6) 0.58395(19) 0.0637(10) Uani 1 1 d . . .
C31' C 0.80805(16) 1.1575(6) 0.52635(16) 0.0622(9) Uani 1 1 d . . .
H31' H 0.8062 1.2746 0.5076 0.075 Uiso 1 1 calc R . .
C32' C 0.92790(19) 1.1978(7) 0.56311(19) 0.0680(10) Uani 1 1 d . . .
C33' C 1.0497(2) 1.1987(9) 0.6013(2) 0.0906(15) Uani 1 1 d . . .
C36' C 1.0634(3) 1.3020(11) 0.6619(2) 0.126(2) Uani 1 1 d . . .
H36D H 1.0320 1.3978 0.6526 0.151 Uiso 1 1 calc R . .
H36E H 1.1083 1.3480 0.6783 0.151 Uiso 1 1 calc R . .
H36F H 1.0585 1.2257 0.6931 0.151 Uiso 1 1 calc R . .
C35' C 1.0971(2) 1.0428(11) 0.6137(3) 0.143(3) Uani 1 1 d . . .
H35D H 1.0929 0.9678 0.6456 0.171 Uiso 1 1 calc R . .
H35E H 1.1425 1.0847 0.6285 0.171 Uiso 1 1 calc R . .
H35F H 1.0858 0.9772 0.5749 0.171 Uiso 1 1 calc R . .
C34' C 1.0506(2) 1.3116(11) 0.5477(2) 0.131(2) Uani 1 1 d . . .
H34D H 1.0364 1.2426 0.5094 0.157 Uiso 1 1 calc R . .
H34E H 1.0953 1.3545 0.5586 0.157 Uiso 1 1 calc R . .
H34F H 1.0206 1.4096 0.5411 0.157 Uiso 1 1 calc R . .
C40' C 0.75427(18) 1.0460(6) 0.47667(17) 0.0764(11) Uani 1 1 d . . .
H40C H 0.7592 0.9256 0.4923 0.092 Uiso 1 1 calc R . .
H40D H 0.7108 1.0881 0.4728 0.092 Uiso 1 1 calc R . .
C41' C 0.75421(19) 1.0436(6) 0.41101(18) 0.0722(10) Uani 1 1 d . . .
C42' C 0.7111(3) 0.9321(8) 0.3665(2) 0.1021(16) Uani 1 1 d . . .
H42' H 0.6829 0.8600 0.3772 0.123 Uiso 1 1 calc R . .
C43' C 0.7089(3) 0.9247(10) 0.3044(3) 0.1190(19) Uani 1 1 d . . .
H43' H 0.6784 0.8497 0.2744 0.143 Uiso 1 1 calc R . .
C44' C 0.7491(3) 1.0215(10) 0.2882(2) 0.1067(18) Uani 1 1 d . . .
H44' H 0.7482 1.0113 0.2475 0.128 Uiso 1 1 calc R . .
C45' C 0.7923(3) 1.1375(9) 0.3308(2) 0.1060(17) Uani 1 1 d . . .
H45' H 0.8198 1.2093 0.3190 0.127 Uiso 1 1 calc R . .
C46' C 0.7945(2) 1.1470(7) 0.3931(2) 0.0879(13) Uani 1 1 d . . .
H46' H 0.8241 1.2253 0.4225 0.106 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N1 Ni O2 175.13(14) . . ?
N1 Ni O1 95.14(12) . . ?
O2 Ni O1 83.51(11) . . ?
N1 Ni N2 86.61(14) . . ?
O2 Ni N2 95.16(13) . . ?
O1 Ni N2 174.61(15) . . ?
C7 O1 Ni 126.8(2) . . ?
C14 O2 Ni 126.2(2) . . ?
C30 O3 C8 117.1(3) . . ?
C32 O6 C33 119.8(4) . . ?
H71 O7 H72 104.2 . . ?
H81 O8 H82 107.0 . . ?
C13 N1 C1 118.8(3) . . ?
C13 N1 Ni 127.8(3) . . ?
C1 N1 Ni 112.9(3) . . ?
C16 N2 C6 125.0(3) . . ?
C16 N2 Ni 122.9(3) . . ?
C6 N2 Ni 111.7(3) . . ?
C32 N3 C31 119.5(4) . . ?
C32 N3 H30 120.3 . . ?
C31 N3 H30 120.3 . . ?
C2 C1 C6 122.2(4) . . ?
C2 C1 N1 125.5(4) . . ?
C6 C1 N1 112.2(3) . . ?
C3 C2 C1 119.2(5) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C4 C3 C2 119.7(5) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 121.3(5) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
C4 C5 C6 119.8(5) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C1 C6 N2 114.9(4) . . ?
C1 C6 C5 117.3(4) . . ?
N2 C6 C5 127.3(4) . . ?
O1 C7 C12 124.6(3) . . ?
O1 C7 C8 118.6(3) . . ?
C12 C7 C8 116.8(4) . . ?
C9 C8 O3 119.9(3) . . ?
C9 C8 C7 122.5(3) . . ?
O3 C8 C7 117.5(3) . . ?
C8 C9 C10 120.4(4) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C11 C10 C9 118.4(4) . . ?
C11 C10 H10 120.8 . . ?
C9 C10 H10 120.8 . . ?
C10 C11 C12 123.0(4) . . ?
C10 C11 H11 118.5 . . ?
C12 C11 H11 118.5 . . ?
C7 C12 C11 118.8(4) . . ?
C7 C12 C13 121.1(4) . . ?
C11 C12 C13 120.0(4) . . ?
N1 C13 C12 124.3(4) . . ?
N1 C13 H13 117.8 . . ?
C12 C13 H13 117.8 . . ?
O2 C14 C15 122.5(4) . . ?
O2 C14 C21 115.1(4) . . ?
C15 C14 C21 122.4(4) . . ?
C14 C15 C16 126.2(4) . . ?
C14 C15 H15 116.9 . . ?
C16 C15 H15 116.9 . . ?
N2 C16 C15 122.1(3) . . ?
N2 C16 C17 123.4(4) . . ?
C15 C16 C17 114.5(4) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C26 C21 C22 117.4(4) . . ?
C26 C21 C14 119.7(4) . . ?
C22 C21 C14 122.9(4) . . ?
C23 C22 C21 120.9(5) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C22 C23 C24 120.8(5) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 H23 119.6 . . ?
C25 C24 C23 119.2(5) . . ?
C25 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
C24 C25 C26 120.2(5) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C21 C26 C25 121.4(5) . . ?
C21 C26 H26 119.3 . . ?
C25 C26 H26 119.3 . . ?
O4 C30 O3 123.9(4) . . ?
O4 C30 C31 125.8(4) . . ?
O3 C30 C31 110.3(3) . . ?
N3 C31 C30 111.5(3) . . ?
N3 C31 C40 114.1(3) . . ?
C30 C31 C40 111.1(3) . . ?
N3 C31 H31 106.6 . . ?
C30 C31 H31 106.6 . . ?
C40 C31 H31 106.6 . . ?
O5 C32 N3 124.8(4) . . ?
O5 C32 O6 125.6(4) . . ?
N3 C32 O6 109.7(4) . . ?
O6 C33 C34 110.0(3) . . ?
O6 C33 C35 102.6(4) . . ?
C34 C33 C35 110.4(4) . . ?
O6 C33 C36 109.7(3) . . ?
C34 C33 C36 113.3(5) . . ?
C35 C33 C36 110.2(4) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C41 C40 C31 113.5(3) . . ?
C41 C40 H40A 108.9 . . ?
C31 C40 H40A 108.9 . . ?
C41 C40 H40B 108.9 . . ?
C31 C40 H40B 108.9 . . ?
H40A C40 H40B 107.7 . . ?
C42 C41 C46 118.3(4) . . ?
C42 C41 C40 121.8(4) . . ?
C46 C41 C40 119.8(5) . . ?
C41 C42 C43 120.9(5) . . ?
C41 C42 H42 119.6 . . ?
C43 C42 H42 119.6 . . ?
C44 C43 C42 119.9(6) . . ?
C44 C43 H43 120.0 . . ?
C42 C43 H43 120.0 . . ?
C45 C44 C43 121.0(6) . . ?
C45 C44 H44 119.5 . . ?
C43 C44 H44 119.5 . . ?
C44 C45 C46 119.7(5) . . ?
C44 C45 H45 120.2 . . ?
C46 C45 H45 120.2 . . ?
C41 C46 C45 120.0(5) . . ?
C41 C46 H46 120.0 . . ?
C45 C46 H46 120.0 . . ?
O2' Ni' O1' 83.82(11) . . ?
O2' Ni' N1' 173.65(14) . . ?
O1' Ni' N1' 94.96(13) . . ?
O2' Ni' N2' 95.33(13) . . ?
O1' Ni' N2' 174.45(15) . . ?
N1' Ni' N2' 86.49(14) . . ?
C7' O1' Ni' 127.7(2) . . ?
C14' O2' Ni' 125.5(2) . . ?
C30' O3' C8' 116.6(3) . . ?
C32' O6' C33' 121.6(4) . . ?
H71' O7' H72' 104.3 . . ?
H81' O8' H82' 104.0 . . ?
C13' N1' C1' 120.9(3) . . ?
C13' N1' Ni' 125.9(3) . . ?
C1' N1' Ni' 112.7(3) . . ?
C16' N2' C6' 125.1(3) . . ?
C16' N2' Ni' 122.6(3) . . ?
C6' N2' Ni' 111.7(3) . . ?
C32' N3' C31' 120.3(4) . . ?
C32' N3' H30' 119.9 . . ?
C31' N3' H30' 119.9 . . ?
C6' C1' C2' 121.5(4) . . ?
C6' C1' N1' 113.6(3) . . ?
C2' C1' N1' 124.7(4) . . ?
C3' C2' C1' 118.7(5) . . ?
C3' C2' H2' 120.7 . . ?
C1' C2' H2' 120.7 . . ?
C4' C3' C2' 119.4(5) . . ?
C4' C3' H3' 120.3 . . ?
C2' C3' H3' 120.3 . . ?
C3' C4' C5' 122.8(5) . . ?
C3' C4' H4' 118.6 . . ?
C5' C4' H4' 118.6 . . ?
C4' C5' C6' 119.6(5) . . ?
C4' C5' H5' 120.2 . . ?
C6' C5' H5' 120.2 . . ?
C1' C6' C5' 117.8(4) . . ?
C1' C6' N2' 114.3(3) . . ?
C5' C6' N2' 127.6(4) . . ?
O1' C7' C8' 120.2(3) . . ?
O1' C7' C12' 124.3(4) . . ?
C8' C7' C12' 115.4(3) . . ?
C9' C8' C7' 123.7(3) . . ?
C9' C8' O3' 118.0(3) . . ?
C7' C8' O3' 118.0(3) . . ?
C8' C9' C10' 119.0(4) . . ?
C8' C9' H9' 120.5 . . ?
C10' C9' H9' 120.5 . . ?
C11' C10' C9' 120.0(4) . . ?
C11' C10' H10' 120.0 . . ?
C9' C10' H10' 120.0 . . ?
C10' C11' C12' 121.1(4) . . ?
C10' C11' H11' 119.4 . . ?
C12' C11' H11' 119.4 . . ?
C11' C12' C7' 120.5(4) . . ?
C11' C12' C13' 119.0(3) . . ?
C7' C12' C13' 120.5(4) . . ?
N1' C13' C12' 126.4(4) . . ?
N1' C13' H13' 116.8 . . ?
C12' C13' H13' 116.8 . . ?
O2' C14' C15' 123.4(4) . . ?
O2' C14' C21' 115.0(3) . . ?
C15' C14' C21' 121.5(4) . . ?
C14' C15' C16' 126.8(4) . . ?
C14' C15' H15' 116.6 . . ?
C16' C15' H15' 116.6 . . ?
N2' C16' C15' 121.3(3) . . ?
N2' C16' C17' 122.7(4) . . ?
C15' C16' C17' 116.0(4) . . ?
C16' C17' H17D 109.5 . . ?
C16' C17' H17E 109.5 . . ?
H17D C17' H17E 109.5 . . ?
C16' C17' H17F 109.5 . . ?
H17D C17' H17F 109.5 . . ?
H17E C17' H17F 109.5 . . ?
C26' C21' C22' 118.0(4) . . ?
C26' C21' C14' 120.3(4) . . ?
C22' C21' C14' 121.7(4) . . ?
C23' C22' C21' 119.7(5) . . ?
C23' C22' H22' 120.2 . . ?
C21' C22' H22' 120.2 . . ?
C24' C23' C22' 121.9(5) . . ?
C24' C23' H23' 119.1 . . ?
C22' C23' H23' 119.1 . . ?
C23' C24' C25' 119.3(6) . . ?
C23' C24' H24' 120.3 . . ?
C25' C24' H24' 120.3 . . ?
C24' C25' C26' 120.3(6) . . ?
C24' C25' H25' 119.9 . . ?
C26' C25' H25' 119.9 . . ?
C21' C26' C25' 120.9(5) . . ?
C21' C26' H26' 119.6 . . ?
C25' C26' H26' 119.6 . . ?
O4' C30' O3' 123.2(4) . . ?
O4' C30' C31' 123.9(4) . . ?
O3' C30' C31' 112.8(3) . . ?
N3' C31' C40' 112.7(3) . . ?
N3' C31' C30' 112.7(3) . . ?
C40' C31' C30' 109.5(3) . . ?
N3' C31' H31' 107.2 . . ?
C40' C31' H31' 107.2 . . ?
C30' C31' H31' 107.2 . . ?
O5' C32' O6' 125.5(4) . . ?
O5' C32' N3' 123.5(4) . . ?
O6' C32' N3' 111.0(4) . . ?
O6' C33' C34' 109.5(4) . . ?
O6' C33' C36' 109.8(4) . . ?
C34' C33' C36' 113.1(6) . . ?
O6' C33' C35' 101.2(5) . . ?
C34' C33' C35' 111.1(5) . . ?
C36' C33' C35' 111.6(5) . . ?
C33' C36' H36D 109.5 . . ?
C33' C36' H36E 109.5 . . ?
H36D C36' H36E 109.5 . . ?
C33' C36' H36F 109.5 . . ?
H36D C36' H36F 109.5 . . ?
H36E C36' H36F 109.5 . . ?
C33' C35' H35D 109.5 . . ?
C33' C35' H35E 109.5 . . ?
H35D C35' H35E 109.5 . . ?
C33' C35' H35F 109.5 . . ?
H35D C35' H35F 109.5 . . ?
H35E C35' H35F 109.5 . . ?
C33' C34' H34D 109.5 . . ?
C33' C34' H34E 109.5 . . ?
H34D C34' H34E 109.5 . . ?
C33' C34' H34F 109.5 . . ?
H34D C34' H34F 109.5 . . ?
H34E C34' H34F 109.5 . . ?
C41' C40' C31' 116.3(3) . . ?
C41' C40' H40C 108.2 . . ?
C31' C40' H40C 108.2 . . ?
C41' C40' H40D 108.2 . . ?
C31' C40' H40D 108.2 . . ?
H40C C40' H40D 107.4 . . ?
C46' C41' C42' 117.6(4) . . ?
C46' C41' C40' 124.0(4) . . ?
C42' C41' C40' 118.4(4) . . ?
C41' C42' C43' 120.8(5) . . ?
C41' C42' H42' 119.6 . . ?
C43' C42' H42' 119.6 . . ?
C44' C43' C42' 121.1(6) . . ?
C44' C43' H43' 119.5 . . ?
C42' C43' H43' 119.5 . . ?
C43' C44' C45' 120.3(5) . . ?
C43' C44' H44' 119.9 . . ?
C45' C44' H44' 119.9 . . ?
C44' C45' C46' 119.1(5) . . ?
C44' C45' H45' 120.5 . . ?
C46' C45' H45' 120.5 . . ?
C41' C46' C45' 121.2(5) . . ?
C41' C46' H46' 119.4 . . ?
C45' C46' H46' 119.4 . . ?
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
Ni N1 1.823(3) . ?
Ni O2 1.847(2) . ?
Ni O1 1.852(2) . ?
Ni N2 1.865(3) . ?
O1 C7 1.306(4) . ?
O2 C14 1.295(4) . ?
O3 C30 1.348(5) . ?
O3 C8 1.389(4) . ?
O4 C30 1.202(4) . ?
O5 C32 1.206(5) . ?
O6 C32 1.346(4) . ?
O6 C33 1.486(5) . ?
O7 H71 0.8225 . ?
O7 H72 0.8153 . ?
O8 H81 0.8164 . ?
O8 H82 0.8218 . ?
N1 C13 1.298(5) . ?
N1 C1 1.447(5) . ?
N2 C16 1.327(5) . ?
N2 C6 1.401(5) . ?
N3 C32 1.340(5) . ?
N3 C31 1.465(4) . ?
N3 H30 0.8600 . ?
C1 C2 1.390(5) . ?
C1 C6 1.391(6) . ?
C2 C3 1.378(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.374(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.390(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.406(6) . ?
C5 H5 0.9300 . ?
C7 C12 1.416(5) . ?
C7 C8 1.424(5) . ?
C8 C9 1.367(5) . ?
C9 C10 1.402(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.360(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.418(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.433(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.375(6) . ?
C14 C21 1.486(6) . ?
C15 C16 1.405(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.520(5) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C21 C26 1.360(6) . ?
C21 C22 1.396(6) . ?
C22 C23 1.350(7) . ?
C22 H22 0.9300 . ?
C23 C24 1.376(7) . ?
C23 H23 0.9300 . ?
C24 C25 1.348(7) . ?
C24 H24 0.9300 . ?
C25 C26 1.385(6) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C30 C31 1.518(5) . ?
C31 C40 1.521(5) . ?
C31 H31 0.9800 . ?
C33 C34 1.505(6) . ?
C33 C35 1.506(6) . ?
C33 C36 1.513(6) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C40 C41 1.510(5) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C42 1.339(7) . ?
C41 C46 1.375(6) . ?
C42 C43 1.391(7) . ?
C42 H42 0.9300 . ?
C43 C44 1.339(8) . ?
C43 H43 0.9300 . ?
C44 C45 1.315(8) . ?
C44 H44 0.9300 . ?
C45 C46 1.408(7) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?
Ni' O2' 1.836(2) . ?
Ni' O1' 1.842(3) . ?
Ni' N1' 1.849(3) . ?
Ni' N2' 1.868(3) . ?
O1' C7' 1.313(4) . ?
O2' C14' 1.299(4) . ?
O3' C30' 1.346(5) . ?
O3' C8' 1.422(4) . ?
O4' C30' 1.194(5) . ?
O5' C32' 1.204(6) . ?
O6' C32' 1.320(5) . ?
O6' C33' 1.465(5) . ?
O7' H71' 0.8172 . ?
O7' H72' 0.8214 . ?
O8' H81' 0.8236 . ?
O8' H82' 0.8252 . ?
N1' C13' 1.300(5) . ?
N1' C1' 1.428(5) . ?
N2' C16' 1.354(5) . ?
N2' C6' 1.422(5) . ?
N3' C32' 1.335(5) . ?
N3' C31' 1.449(4) . ?
N3' H30' 0.8600 . ?
C1' C6' 1.387(6) . ?
C1' C2' 1.400(5) . ?
C2' C3' 1.384(6) . ?
C2' H2' 0.9300 . ?
C3' C4' 1.354(7) . ?
C3' H3' 0.9300 . ?
C4' C5' 1.365(7) . ?
C4' H4' 0.9300 . ?
C5' C6' 1.396(6) . ?
C5' H5' 0.9300 . ?
C7' C8' 1.415(5) . ?
C7' C12' 1.415(5) . ?
C8' C9' 1.356(5) . ?
C9' C10' 1.401(5) . ?
C9' H9' 0.9300 . ?
C10' C11' 1.358(5) . ?
C10' H10' 0.9300 . ?
C11' C12' 1.401(5) . ?
C11' H11' 0.9300 . ?
C12' C13' 1.423(5) . ?
C13' H13' 0.9300 . ?
C14' C15' 1.371(5) . ?
C14' C21' 1.482(5) . ?
C15' C16' 1.379(5) . ?
C15' H15' 0.9300 . ?
C16' C17' 1.504(5) . ?
C17' H17D 0.9600 . ?
C17' H17E 0.9600 . ?
C17' H17F 0.9600 . ?
C21' C26' 1.382(6) . ?
C21' C22' 1.401(5) . ?
C22' C23' 1.387(7) . ?
C22' H22' 0.9300 . ?
C23' C24' 1.357(8) . ?
C23' H23' 0.9300 . ?
C24' C25' 1.365(7) . ?
C24' H24' 0.9300 . ?
C25' C26' 1.400(6) . ?
C25' H25' 0.9300 . ?
C26' H26' 0.9300 . ?
C30' C31' 1.516(5) . ?
C31' C40' 1.514(5) . ?
C31' H31' 0.9800 . ?
C33' C34' 1.505(7) . ?
C33' C36' 1.514(7) . ?
C33' C35' 1.518(8) . ?
C36' H36D 0.9600 . ?
C36' H36E 0.9600 . ?
C36' H36F 0.9600 . ?
C35' H35D 0.9600 . ?
C35' H35E 0.9600 . ?
C35' H35F 0.9600 . ?
C34' H34D 0.9600 . ?
C34' H34E 0.9600 . ?
C34' H34F 0.9600 . ?
C40' C41' 1.507(5) . ?
C40' H40C 0.9700 . ?
C40' H40D 0.9700 . ?
C41' C46' 1.360(6) . ?
C41' C42' 1.362(6) . ?
C42' C43' 1.408(7) . ?
C42' H42' 0.9300 . ?
C43' C44' 1.308(8) . ?
C43' H43' 0.9300 . ?
C44' C45' 1.364(8) . ?
C44' H44' 0.9300 . ?
C45' C46' 1.414(6) . ?
C45' H45' 0.9300 . ?
C46' H46' 0.9300 . ?
