#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/46/4314678.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_4314678
loop_
_publ_author_name
'Katarzyna Grubel'
'Amy L. Fuller'
'Bonnie M. Chambers'
'Atta M. Arif'
'Lisa M. Berreau'
_publ_section_title
;
 O2-Dependent Aliphatic Carbon-Carbon Bond Cleavage Reactivity in a Ni(II)
 Enolate Complex Having a Hydrogen Bond Donor Microenvironment; Comparison
 with a Hydrophobic Analogue
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1071
_journal_page_last               1081
_journal_paper_doi               10.1021/ic901981y
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C30 H44 N7 Ni O2, 1/4(C2 H5 N O2), Cl O4'
_chemical_formula_sum            'C30.5 H45.25 Cl N7.25 Ni O6.5'
_chemical_formula_weight         711.65
_chemical_name_systematic
; 
 ? 
;
_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                 93.1236(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.3396(8)
_cell_length_b                   11.4649(3)
_cell_length_c                   19.4692(3)
_cell_measurement_reflns_used    40506
_cell_measurement_temperature    103(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_volume                     7207.9(3)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'WinGX, Ortep3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      103(1)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method       'Phi and Omega scan'
_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  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0638
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15128
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_T_max  0.9070
_exptl_absorpt_correction_T_min  0.8787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         8259
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0620
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0736P)²+16.1441P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1452
_refine_ls_wR_factor_ref         0.1713
_reflns_number_gt                5348
_reflns_number_total             8259
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901981y_si_001_2.cif
_cod_data_source_block           usu186
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'C30.50 H45.25 Cl N7.25 Ni O6.50'
_cod_database_code               4314678
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_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
Ni1 Ni 0.831926(12) 0.48920(4) 0.94350(2) 0.03237(15) Uani 1 1 d . . .
Cl1 Cl 0.84419(3) 0.88416(9) 0.69380(5) 0.0521(3) Uani 1 1 d . . .
O1 O 0.85807(7) 0.4068(2) 1.02651(13) 0.0447(6) Uani 1 1 d . . .
O2 O 0.77839(7) 0.4391(2) 0.98785(13) 0.0415(6) Uani 1 1 d . . .
O3 O 0.86300(12) 0.7753(3) 0.67917(14) 0.0766(11) Uani 1 1 d . A 1
O4 O 0.82150(19) 0.8871(3) 0.7542(2) 0.0843(19) Uani 0.790(7) 1 d P A 1
O5 O 0.81496(13) 0.9122(5) 0.6367(2) 0.0710(15) Uani 0.790(7) 1 d P A 1
O6 O 0.87487(14) 0.9759(4) 0.6916(3) 0.0948(19) Uani 0.790(7) 1 d P A 1
O4A O 0.8630(4) 0.9001(12) 0.7651(7) 0.054(4) Uiso 0.210(7) 1 d P A 2
O5A O 0.8061(7) 0.829(2) 0.7082(12) 0.117(8) Uiso 0.210(7) 1 d P A 2
O6A O 0.8338(6) 0.9671(17) 0.6551(9) 0.069(5) Uiso 0.210(7) 1 d P A 2
N1 N 0.86825(9) 0.6340(3) 1.08261(15) 0.0504(8) Uani 1 1 d . . .
H1N H 0.8765 0.5692 1.0633 0.061 Uiso 1 1 calc R . .
N2 N 0.82568(8) 0.6599(2) 0.98586(14) 0.0355(6) Uani 1 1 d . . .
N3 N 0.80628(9) 0.5746(2) 0.85735(14) 0.0366(6) Uani 1 1 d . . .
N4 N 0.82678(9) 0.3477(3) 0.87237(16) 0.0395(7) Uani 1 1 d . . .
N5 N 0.86768(11) 0.2204(3) 0.9370(2) 0.0653(11) Uani 1 1 d . . .
H5N H 0.8772 0.2829 0.9589 0.078 Uiso 1 1 calc R B 1
N6 N 0.88712(8) 0.5445(2) 0.90821(14) 0.0338(6) Uani 1 1 d . . .
N7 N 0.82601(9) 0.3656(3) 1.06419(17) 0.0502(8) Uani 1 1 d . . .
H7N H 0.8315 0.3270 1.1026 0.060 Uiso 1 1 calc R . .
C1 C 0.95671(18) 0.6776(7) 1.1283(3) 0.111(3) Uani 1 1 d . . .
H1A H 0.9848 0.6508 1.1415 0.167 Uiso 1 1 calc R . .
H1B H 0.9549 0.7621 1.1351 0.167 Uiso 1 1 calc R . .
H1C H 0.9502 0.6590 1.0798 0.167 Uiso 1 1 calc R . .
C2 C 0.92982(19) 0.4870(6) 1.1620(2) 0.091(2) Uani 1 1 d . . .
H2A H 0.9584 0.4626 1.1734 0.137 Uiso 1 1 calc R . .
H2B H 0.9224 0.4678 1.1138 0.137 Uiso 1 1 calc R . .
H2C H 0.9111 0.4461 1.1918 0.137 Uiso 1 1 calc R . .
C3 C 0.93513(16) 0.6446(6) 1.2492(2) 0.0899(19) Uani 1 1 d . . .
H3A H 0.9636 0.6217 1.2628 0.135 Uiso 1 1 calc R . .
H3B H 0.9158 0.6014 1.2769 0.135 Uiso 1 1 calc R . .
H3C H 0.9317 0.7285 1.2568 0.135 Uiso 1 1 calc R . .
C4 C 0.92601(13) 0.6167(5) 1.1725(2) 0.0640(13) Uani 1 1 d . . .
C5 C 0.88255(14) 0.6579(5) 1.1535(2) 0.0701(14) Uani 1 1 d . . .
H5A H 0.8634 0.6202 1.1846 0.084 Uiso 1 1 calc R . .
H5B H 0.8812 0.7431 1.1614 0.084 Uiso 1 1 calc R . .
C6 C 0.84292(10) 0.7064(3) 1.04513(18) 0.0392(8) Uani 1 1 d . . .
C7 C 0.83417(13) 0.8227(4) 1.0633(2) 0.0503(10) Uani 1 1 d . . .
H7 H 0.8458 0.8545 1.1051 0.060 Uiso 1 1 calc R . .
C8 C 0.80919(15) 0.8890(4) 1.0209(2) 0.0613(12) Uani 1 1 d . . .
H8 H 0.8030 0.9670 1.0332 0.074 Uiso 1 1 calc R . .
C9 C 0.79280(16) 0.8431(4) 0.9598(2) 0.0650(12) Uani 1 1 d . . .
H9 H 0.7758 0.8894 0.9292 0.078 Uiso 1 1 calc R . .
C10 C 0.80148(12) 0.7293(3) 0.9441(2) 0.0468(9) Uani 1 1 d . . .
C11 C 0.78149(13) 0.6715(4) 0.8823(2) 0.0565(11) Uani 1 1 d . . .
H11A H 0.7540 0.6417 0.8939 0.068 Uiso 1 1 calc R . .
H11B H 0.7772 0.7299 0.8452 0.068 Uiso 1 1 calc R . .
C12 C 0.78048(11) 0.4889(3) 0.81834(18) 0.0417(8) Uani 1 1 d . . .
H12A H 0.7744 0.5178 0.7710 0.050 Uiso 1 1 calc R . .
H12B H 0.7539 0.4789 0.8404 0.050 Uiso 1 1 calc R . .
C13 C 0.80231(11) 0.3737(3) 0.81583(19) 0.0423(9) Uani 1 1 d . . .
C14 C 0.79555(14) 0.2974(4) 0.7620(2) 0.0561(11) Uani 1 1 d . . .
H14 H 0.7784 0.3180 0.7227 0.067 Uiso 1 1 calc R . .
C15 C 0.81484(16) 0.1879(4) 0.7673(3) 0.0684(15) Uani 1 1 d . C .
H15 H 0.8110 0.1332 0.7309 0.082 Uiso 1 1 calc R . .
C16 C 0.83908(14) 0.1596(4) 0.8241(3) 0.0626(13) Uani 1 1 d . . .
H16 H 0.8519 0.0852 0.8277 0.075 Uiso 1 1 calc R C .
C17 C 0.84500(12) 0.2416(3) 0.8776(2) 0.0521(10) Uani 1 1 d . C .
C19 C 0.92561(12) 0.0902(4) 0.9767(2) 0.0492(10) Uani 1 1 d . . .
C18 C 0.87892(16) 0.1067(5) 0.9709(3) 0.0475(15) Uani 0.730(6) 1 d P C 1
H18A H 0.8661 0.0419 0.9437 0.057 Uiso 0.730(6) 1 calc PR C 1
H18B H 0.8679 0.1046 1.0174 0.057 Uiso 0.730(6) 1 calc PR C 1
C20 C 0.9470(2) 0.1795(6) 1.0233(4) 0.0671(19) Uani 0.730(6) 1 d P C 1
H20A H 0.9769 0.1641 1.0265 0.101 Uiso 0.730(6) 1 calc PR C 1
H20B H 0.9361 0.1745 1.0693 0.101 Uiso 0.730(6) 1 calc PR C 1
H20C H 0.9419 0.2577 1.0045 0.101 Uiso 0.730(6) 1 calc PR C 1
C21 C 0.9431(2) 0.0880(7) 0.9052(3) 0.074(2) Uani 0.730(6) 1 d P C 1
H21A H 0.9287 0.0283 0.8770 0.111 Uiso 0.730(6) 1 calc PR C 1
H21B H 0.9728 0.0698 0.9096 0.111 Uiso 0.730(6) 1 calc PR C 1
H21C H 0.9391 0.1644 0.8834 0.111 Uiso 0.730(6) 1 calc PR C 1
C22 C 0.9326(3) -0.0331(8) 1.0106(5) 0.076(3) Uani 0.730(6) 1 d P C 1
H22A H 0.9193 -0.0929 0.9810 0.113 Uiso 0.730(6) 1 calc PR C 1
H22B H 0.9205 -0.0343 1.0557 0.113 Uiso 0.730(6) 1 calc PR C 1
H22C H 0.9624 -0.0491 1.0162 0.113 Uiso 0.730(6) 1 calc PR C 1
C18A C 0.8907(4) 0.1041(11) 0.9192(7) 0.040(4) Uani 0.270(6) 1 d P C 2
H18C H 0.8715 0.0369 0.9190 0.048 Uiso 0.270(6) 1 calc PR C 2
H18D H 0.9026 0.1097 0.8735 0.048 Uiso 0.270(6) 1 calc PR C 2
C20A C 0.9095(6) 0.1290(15) 1.0450(7) 0.061(5) Uani 0.270(6) 1 d P C 2
H20D H 0.8983 0.2082 1.0404 0.092 Uiso 0.270(6) 1 calc PR C 2
H20E H 0.9321 0.1281 1.0805 0.092 Uiso 0.270(6) 1 calc PR C 2
H20F H 0.8876 0.0757 1.0582 0.092 Uiso 0.270(6) 1 calc PR C 2
C21A C 0.9595(4) 0.1866(13) 0.9598(11) 0.060(5) Uani 0.270(6) 1 d P C 2
H21D H 0.9466 0.2640 0.9592 0.090 Uiso 0.270(6) 1 calc PR C 2
H21E H 0.9702 0.1703 0.9147 0.090 Uiso 0.270(6) 1 calc PR C 2
H21F H 0.9822 0.1843 0.9951 0.090 Uiso 0.270(6) 1 calc PR C 2
C22A C 0.9416(6) -0.0261(16) 0.9741(10) 0.054(5) Uani 0.270(6) 1 d P C 2
H22D H 0.9641 -0.0355 1.0096 0.081 Uiso 0.270(6) 1 calc PR C 2
H22E H 0.9523 -0.0404 0.9287 0.081 Uiso 0.270(6) 1 calc PR C 2
H22F H 0.9195 -0.0819 0.9823 0.081 Uiso 0.270(6) 1 calc PR C 2
C23 C 0.84068(12) 0.6169(4) 0.8154(2) 0.0540(11) Uani 1 1 d . . .
H23A H 0.8346 0.6979 0.8005 0.065 Uiso 1 1 calc R . .
H23B H 0.8416 0.5681 0.7736 0.065 Uiso 1 1 calc R . .
C24 C 0.88293(11) 0.6143(3) 0.85329(17) 0.0378(8) Uani 1 1 d . . .
C25 C 0.91557(12) 0.6779(3) 0.82892(19) 0.0442(9) Uani 1 1 d . . .
H25 H 0.9115 0.7276 0.7901 0.053 Uiso 1 1 calc R . .
C26 C 0.95415(12) 0.6672(4) 0.8627(2) 0.0515(10) Uani 1 1 d . . .
H26 H 0.9771 0.7100 0.8475 0.062 Uiso 1 1 calc R . .
C27 C 0.95894(11) 0.5937(4) 0.9186(2) 0.0503(10) Uani 1 1 d . . .
H27 H 0.9853 0.5839 0.9419 0.060 Uiso 1 1 calc R . .
C28 C 0.92449(10) 0.5341(3) 0.94040(17) 0.0377(8) Uani 1 1 d . . .
H28 H 0.9277 0.4844 0.9794 0.045 Uiso 1 1 calc R . .
C29 C 0.78752(12) 0.3842(3) 1.0427(2) 0.0454(9) Uani 1 1 d . . .
C30 C 0.75409(13) 0.3368(4) 1.0860(2) 0.0594(11) Uani 1 1 d . . .
H30A H 0.7668 0.2959 1.1260 0.089 Uiso 1 1 calc R . .
H30B H 0.7367 0.2823 1.0585 0.089 Uiso 1 1 calc R . .
H30C H 0.7371 0.4012 1.1016 0.089 Uiso 1 1 calc R . .
O7 O 0.96802(16) 0.8395(8) 0.7124(3) 0.0668(19) Uani 0.50 1 d PD D -1
C31 C 0.9758(5) 0.9227(14) 0.7315(10) 0.037(4) Uiso 0.25 1 d PD D -1
N8 N 1.0190(4) 0.9214(12) 0.7462(8) 0.041(4) Uiso 0.25 1 d PD D -1
H8A H 1.0295 0.9908 0.7551 0.049 Uiso 0.25 1 calc PR D -1
C32 C 0.9712(5) 1.0412(12) 0.7240(8) 0.042(4) Uani 0.25 1 d P D -1
H32A H 0.9879 1.0812 0.7603 0.064 Uiso 0.25 1 calc PR D -1
H32B H 0.9420 1.0620 0.7274 0.064 Uiso 0.25 1 calc PR D -1
H32C H 0.9804 1.0650 0.6790 0.064 Uiso 0.25 1 calc PR D -1
O7A O 1.05(4) 0.84(11) 0.75(3) 0.036 Uiso 0.00 1 d PD D -1
H7A H 1.0481 0.8066 0.7890 0.053 Uiso 0.25 1 calc PR 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'
Cl Cl 0.1484 0.1585 '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
O1 Ni1 N6 94.53(10) . . ?
O1 Ni1 O2 81.86(10) . . ?
N6 Ni1 O2 174.68(10) . . ?
O1 Ni1 N3 178.78(10) . . ?
N6 Ni1 N3 84.26(11) . . ?
O2 Ni1 N3 99.35(11) . . ?
O1 Ni1 N4 100.25(12) . . ?
N6 Ni1 N4 93.24(11) . . ?
O2 Ni1 N4 91.27(10) . . ?
N3 Ni1 N4 79.68(11) . . ?
O1 Ni1 N2 99.44(11) . . ?
N6 Ni1 N2 87.04(11) . . ?
O2 Ni1 N2 89.69(10) . . ?
N3 Ni1 N2 80.67(11) . . ?
N4 Ni1 N2 160.22(11) . . ?
O6A Cl1 O4 110.4(8) . . ?
O6A Cl1 O3 130.6(8) . . ?
O4 Cl1 O3 115.6(2) . . ?
O6A Cl1 O5A 104.4(13) . . ?
O4 Cl1 O5A 49.9(10) . . ?
O3 Cl1 O5A 92.1(10) . . ?
O6A Cl1 O6 65.8(10) . . ?
O4 Cl1 O6 113.1(3) . . ?
O3 Cl1 O6 109.3(3) . . ?
O5A Cl1 O6 158.0(11) . . ?
O6A Cl1 O5 39.5(9) . . ?
O4 Cl1 O5 106.5(3) . . ?
O3 Cl1 O5 107.9(2) . . ?
O5A Cl1 O5 73.4(10) . . ?
O6 Cl1 O5 103.6(3) . . ?
O6A Cl1 O4A 123.3(11) . . ?
O4 Cl1 O4A 55.3(5) . . ?
O3 Cl1 O4A 97.8(6) . . ?
O5A Cl1 O4A 100.6(11) . . ?
O6 Cl1 O4A 72.2(6) . . ?
O5 Cl1 O4A 153.6(6) . . ?
N7 O1 Ni1 106.90(19) . . ?
C29 O2 Ni1 109.4(2) . . ?
C6 N1 C5 123.1(4) . . ?
C6 N1 H1N 118.4 . . ?
C5 N1 H1N 118.4 . . ?
C10 N2 C6 118.3(3) . . ?
C10 N2 Ni1 111.7(2) . . ?
C6 N2 Ni1 130.0(2) . . ?
C11 N3 C12 111.8(3) . . ?
C11 N3 C23 111.8(3) . . ?
C12 N3 C23 110.6(3) . . ?
C11 N3 Ni1 106.9(2) . . ?
C12 N3 Ni1 107.0(2) . . ?
C23 N3 Ni1 108.5(2) . . ?
C17 N4 C13 119.5(3) . . ?
C17 N4 Ni1 128.0(3) . . ?
C13 N4 Ni1 112.4(2) . . ?
C17 N5 C18 129.6(4) . . ?
C17 N5 C18A 101.7(6) . . ?
C18 N5 C18A 41.7(5) . . ?
C17 N5 H5N 115.2 . . ?
C18 N5 H5N 115.2 . . ?
C18A N5 H5N 129.6 . . ?
C24 N6 C28 118.6(3) . . ?
C24 N6 Ni1 113.7(2) . . ?
C28 N6 Ni1 126.7(2) . . ?
C29 N7 O1 120.1(3) . . ?
C29 N7 H7N 119.9 . . ?
O1 N7 H7N 119.9 . . ?
C4 C1 H1A 109.5 . . ?
C4 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C4 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C4 C2 H2A 109.5 . . ?
C4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 C5 111.0(4) . . ?
C2 C4 C1 108.4(5) . . ?
C5 C4 C1 110.2(5) . . ?
C2 C4 C3 108.9(4) . . ?
C5 C4 C3 107.4(4) . . ?
C1 C4 C3 110.9(4) . . ?
N1 C5 C4 114.6(4) . . ?
N1 C5 H5A 108.6 . . ?
C4 C5 H5A 108.6 . . ?
N1 C5 H5B 108.6 . . ?
C4 C5 H5B 108.6 . . ?
H5A C5 H5B 107.6 . . ?
N1 C6 N2 115.1(3) . . ?
N1 C6 C7 124.7(4) . . ?
N2 C6 C7 120.2(3) . . ?
C8 C7 C6 119.8(4) . . ?
C8 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
C7 C8 C9 120.0(4) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C10 C9 C8 118.8(4) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
N2 C10 C9 122.8(4) . . ?
N2 C10 C11 115.8(3) . . ?
C9 C10 C11 121.2(4) . . ?
N3 C11 C10 112.5(3) . . ?
N3 C11 H11A 109.1 . . ?
C10 C11 H11A 109.1 . . ?
N3 C11 H11B 109.1 . . ?
C10 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
N3 C12 C13 110.5(3) . . ?
N3 C12 H12A 109.5 . . ?
C13 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
N4 C13 C14 122.8(4) . . ?
N4 C13 C12 115.0(3) . . ?
C14 C13 C12 122.0(4) . . ?
C13 C14 C15 117.6(4) . . ?
C13 C14 H14 121.2 . . ?
C15 C14 H14 121.2 . . ?
C16 C15 C14 120.4(4) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C17 119.5(4) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
N4 C17 N5 116.0(4) . . ?
N4 C17 C16 120.2(4) . . ?
N5 C17 C16 123.8(4) . . ?
C22A C19 C20 119.8(9) . . ?
C22A C19 C18 118.2(9) . . ?
C20 C19 C18 112.4(4) . . ?
C22A C19 C20A 116.4(10) . . ?
C20 C19 C20A 56.3(8) . . ?
C18 C19 C20A 69.0(7) . . ?
C22A C19 C21 78.5(8) . . ?
C20 C19 C21 112.2(5) . . ?
C18 C19 C21 110.5(4) . . ?
C20A C19 C21 163.9(8) . . ?
C22A C19 C18A 108.7(10) . . ?
C20 C19 C18A 130.9(6) . . ?
C18 C19 C18A 41.8(5) . . ?
C20A C19 C18A 109.3(8) . . ?
C21 C19 C18A 68.7(6) . . ?
C22A C19 C22 29.9(7) . . ?
C20 C19 C22 107.9(5) . . ?
C18 C19 C22 105.3(4) . . ?
C20A C19 C22 86.8(7) . . ?
C21 C19 C22 108.3(5) . . ?
C18A C19 C22 118.5(7) . . ?
C22A C19 C21A 112.5(10) . . ?
C20 C19 C21A 50.3(8) . . ?
C18 C19 C21A 125.9(6) . . ?
C20A C19 C21A 104.4(11) . . ?
C21 C19 C21A 62.2(8) . . ?
C18A C19 C21A 105.0(8) . . ?
C22 C19 C21A 128.5(6) . . ?
N5 C18 C19 111.0(4) . . ?
N5 C18 H18A 109.4 . . ?
C19 C18 H18A 109.4 . . ?
N5 C18 H18B 109.4 . . ?
C19 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C18A N5 105.2(9) . . ?
C19 C18A H18C 110.7 . . ?
N5 C18A H18C 110.7 . . ?
C19 C18A H18D 110.7 . . ?
N5 C18A H18D 110.7 . . ?
H18C C18A H18D 108.8 . . ?
C19 C20A H20D 109.5 . . ?
C19 C20A H20E 109.5 . . ?
H20D C20A H20E 109.5 . . ?
C19 C20A H20F 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
C19 C21A H21D 109.5 . . ?
C19 C21A H21E 109.5 . . ?
H21D C21A H21E 109.5 . . ?
C19 C21A H21F 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?
C19 C22A H22D 109.5 . . ?
C19 C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
C19 C22A H22F 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
N3 C23 C24 113.9(3) . . ?
N3 C23 H23A 108.8 . . ?
C24 C23 H23A 108.8 . . ?
N3 C23 H23B 108.8 . . ?
C24 C23 H23B 108.8 . . ?
H23A C23 H23B 107.7 . . ?
N6 C24 C25 122.8(3) . . ?
N6 C24 C23 116.7(3) . . ?
C25 C24 C23 120.3(3) . . ?
C26 C25 C24 118.3(3) . . ?
C26 C25 H25 120.9 . . ?
C24 C25 H25 120.9 . . ?
C27 C26 C25 119.3(3) . . ?
C27 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
C26 C27 C28 118.9(4) . . ?
C26 C27 H27 120.6 . . ?
C28 C27 H27 120.6 . . ?
N6 C28 C27 122.1(3) . . ?
N6 C28 H28 118.9 . . ?
C27 C28 H28 118.9 . . ?
O2 C29 N7 121.8(3) . . ?
O2 C29 C30 120.8(4) . . ?
N7 C29 C30 117.5(4) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O7 C31 C32 147(2) . . ?
O7 C31 N8 106.2(16) . . ?
C32 C31 N8 97.7(15) . . ?
O7A N8 C31 133(10) . . ?
O7A N8 H8A 113.5 . . ?
C31 N8 H8A 113.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.018(2) . ?
Ni1 N6 2.048(3) . ?
Ni1 O2 2.058(2) . ?
Ni1 N3 2.076(3) . ?
Ni1 N4 2.134(3) . ?
Ni1 N2 2.137(3) . ?
Cl1 O6A 1.247(18) . ?
Cl1 O4 1.420(4) . ?
Cl1 O3 1.424(3) . ?
Cl1 O5A 1.42(2) . ?
Cl1 O6 1.448(5) . ?
Cl1 O5 1.455(4) . ?
Cl1 O4A 1.497(13) . ?
O1 N7 1.385(4) . ?
O2 C29 1.261(4) . ?
N1 C6 1.352(5) . ?
N1 C5 1.457(5) . ?
N1 H1N 0.8800 . ?
N2 C10 1.356(5) . ?
N2 C6 1.363(4) . ?
N3 C11 1.468(5) . ?
N3 C12 1.473(4) . ?
N3 C23 1.496(5) . ?
N4 C17 1.353(5) . ?
N4 C13 1.353(5) . ?
N5 C17 1.357(6) . ?
N5 C18 1.497(6) . ?
N5 C18A 1.576(13) . ?
N5 H5N 0.8800 . ?
N6 C24 1.336(4) . ?
N6 C28 1.336(4) . ?
N7 C29 1.309(5) . ?
N7 H7N 0.8800 . ?
C1 C4 1.518(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C4 1.507(8) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.540(6) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.510(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.412(5) . ?
C7 C8 1.356(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.379(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.373(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.488(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.500(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.373(5) . ?
C14 C15 1.403(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.360(7) . ?
C15 H15 0.9500 . ?
C16 C17 1.408(6) . ?
C16 H16 0.9500 . ?
C19 C22A 1.432(18) . ?
C19 C20 1.510(8) . ?
C19 C18 1.520(6) . ?
C19 C20A 1.522(16) . ?
C19 C21 1.532(7) . ?
C19 C18A 1.554(14) . ?
C19 C22 1.571(9) . ?
C19 C21A 1.602(15) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C18A H18C 0.9900 . ?
C18A H18D 0.9900 . ?
C20A H20D 0.9800 . ?
C20A H20E 0.9800 . ?
C20A H20F 0.9800 . ?
C21A H21D 0.9800 . ?
C21A H21E 0.9800 . ?
C21A H21F 0.9800 . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?
C23 C24 1.517(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.388(5) . ?
C25 C26 1.383(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.380(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.392(5) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C30 1.508(5) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
O7 C31 1.050(14) . ?
C31 C32 1.37(2) . ?
C31 N8 1.408(19) . ?
N8 O7A 1.33(2) . ?
N8 H8A 0.8800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
O7A H7A 0.8400 . ?
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
N1 H1N O1 0.88 2.07 2.837(4) 144.9 .
N5 H5N O1 0.88 2.05 2.784(5) 139.7 .
N7 H7N O3 0.88 2.11 2.960(4) 161.3 6_566
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
N6 Ni1 O1 N7 175.9(2) . . . . ?
O2 Ni1 O1 N7 -0.1(2) . . . . ?
N3 Ni1 O1 N7 -177(62) . . . . ?
N4 Ni1 O1 N7 -89.9(2) . . . . ?
N2 Ni1 O1 N7 88.2(2) . . . . ?
O1 Ni1 O2 C29 0.2(2) . . . . ?
N6 Ni1 O2 C29 -47.5(12) . . . . ?
N3 Ni1 O2 C29 -179.9(2) . . . . ?
N4 Ni1 O2 C29 100.3(3) . . . . ?
N2 Ni1 O2 C29 -99.4(2) . . . . ?
O1 Ni1 N2 C10 -168.4(2) . . . . ?
N6 Ni1 N2 C10 97.5(3) . . . . ?
O2 Ni1 N2 C10 -86.7(3) . . . . ?
N3 Ni1 N2 C10 12.8(3) . . . . ?
N4 Ni1 N2 C10 6.2(5) . . . . ?
O1 Ni1 N2 C6 13.7(3) . . . . ?
N6 Ni1 N2 C6 -80.4(3) . . . . ?
O2 Ni1 N2 C6 95.4(3) . . . . ?
N3 Ni1 N2 C6 -165.1(3) . . . . ?
N4 Ni1 N2 C6 -171.7(3) . . . . ?
O1 Ni1 N3 C11 -123(5) . . . . ?
N6 Ni1 N3 C11 -115.3(3) . . . . ?
O2 Ni1 N3 C11 60.7(3) . . . . ?
N4 Ni1 N3 C11 150.3(3) . . . . ?
N2 Ni1 N3 C11 -27.4(2) . . . . ?
O1 Ni1 N3 C12 117(5) . . . . ?
N6 Ni1 N3 C12 124.7(2) . . . . ?
O2 Ni1 N3 C12 -59.2(2) . . . . ?
N4 Ni1 N3 C12 30.4(2) . . . . ?
N2 Ni1 N3 C12 -147.3(2) . . . . ?
O1 Ni1 N3 C23 -2(5) . . . . ?
N6 Ni1 N3 C23 5.4(2) . . . . ?
O2 Ni1 N3 C23 -178.6(2) . . . . ?
N4 Ni1 N3 C23 -89.0(2) . . . . ?
N2 Ni1 N3 C23 93.3(2) . . . . ?
O1 Ni1 N4 C17 -13.6(3) . . . . ?
N6 Ni1 N4 C17 81.6(3) . . . . ?
O2 Ni1 N4 C17 -95.6(3) . . . . ?
N3 Ni1 N4 C17 165.2(3) . . . . ?
N2 Ni1 N4 C17 171.8(3) . . . . ?
O1 Ni1 N4 C13 167.4(2) . . . . ?
N6 Ni1 N4 C13 -97.4(2) . . . . ?
O2 Ni1 N4 C13 85.4(2) . . . . ?
N3 Ni1 N4 C13 -13.8(2) . . . . ?
N2 Ni1 N4 C13 -7.2(4) . . . . ?
O1 Ni1 N6 C24 -174.9(2) . . . . ?
O2 Ni1 N6 C24 -127.7(11) . . . . ?
N3 Ni1 N6 C24 5.2(2) . . . . ?
N4 Ni1 N6 C24 84.5(2) . . . . ?
N2 Ni1 N6 C24 -75.7(2) . . . . ?
O1 Ni1 N6 C28 -6.8(3) . . . . ?
O2 Ni1 N6 C28 40.4(13) . . . . ?
N3 Ni1 N6 C28 173.3(3) . . . . ?
N4 Ni1 N6 C28 -107.4(3) . . . . ?
N2 Ni1 N6 C28 92.4(3) . . . . ?
Ni1 O1 N7 C29 0.1(4) . . . . ?
C6 N1 C5 C4 -145.3(4) . . . . ?
C2 C4 C5 N1 -58.8(6) . . . . ?
C1 C4 C5 N1 61.3(6) . . . . ?
C3 C4 C5 N1 -177.7(5) . . . . ?
C5 N1 C6 N2 -166.7(4) . . . . ?
C5 N1 C6 C7 13.9(6) . . . . ?
C10 N2 C6 N1 -176.9(3) . . . . ?
Ni1 N2 C6 N1 0.8(4) . . . . ?
C10 N2 C6 C7 2.5(5) . . . . ?
Ni1 N2 C6 C7 -179.7(3) . . . . ?
N1 C6 C7 C8 178.1(4) . . . . ?
N2 C6 C7 C8 -1.3(6) . . . . ?
C6 C7 C8 C9 -0.7(7) . . . . ?
C7 C8 C9 C10 1.5(7) . . . . ?
C6 N2 C10 C9 -1.7(6) . . . . ?
Ni1 N2 C10 C9 -179.9(4) . . . . ?
C6 N2 C10 C11 -176.4(3) . . . . ?
Ni1 N2 C10 C11 5.4(4) . . . . ?
C8 C9 C10 N2 -0.3(7) . . . . ?
C8 C9 C10 C11 174.1(4) . . . . ?
C12 N3 C11 C10 155.4(3) . . . . ?
C23 N3 C11 C10 -80.0(4) . . . . ?
Ni1 N3 C11 C10 38.6(4) . . . . ?
N2 C10 C11 N3 -30.2(5) . . . . ?
C9 C10 C11 N3 155.1(4) . . . . ?
C11 N3 C12 C13 -159.3(3) . . . . ?
C23 N3 C12 C13 75.4(4) . . . . ?
Ni1 N3 C12 C13 -42.6(3) . . . . ?
C17 N4 C13 C14 -1.3(5) . . . . ?
Ni1 N4 C13 C14 177.8(3) . . . . ?
C17 N4 C13 C12 174.4(3) . . . . ?
Ni1 N4 C13 C12 -6.5(4) . . . . ?
N3 C12 C13 N4 33.2(4) . . . . ?
N3 C12 C13 C14 -151.0(3) . . . . ?
N4 C13 C14 C15 0.6(5) . . . . ?
C12 C13 C14 C15 -174.8(3) . . . . ?
C13 C14 C15 C16 0.3(6) . . . . ?
C14 C15 C16 C17 -0.6(6) . . . . ?
C13 N4 C17 N5 -177.4(3) . . . . ?
Ni1 N4 C17 N5 3.6(5) . . . . ?
C13 N4 C17 C16 1.1(5) . . . . ?
Ni1 N4 C17 C16 -177.9(3) . . . . ?
C18 N5 C17 N4 155.8(4) . . . . ?
C18A N5 C17 N4 -169.1(6) . . . . ?
C18 N5 C17 C16 -22.7(7) . . . . ?
C18A N5 C17 C16 12.5(7) . . . . ?
C15 C16 C17 N4 -0.1(6) . . . . ?
C15 C16 C17 N5 178.2(4) . . . . ?
C17 N5 C18 C19 118.8(5) . . . . ?
C18A N5 C18 C19 60.9(8) . . . . ?
C22A C19 C18 N5 -149.1(10) . . . . ?
C20 C19 C18 N5 64.7(6) . . . . ?
C20A C19 C18 N5 101.4(8) . . . . ?
C21 C19 C18 N5 -61.5(6) . . . . ?
C18A C19 C18 N5 -62.3(8) . . . . ?
C22 C19 C18 N5 -178.2(5) . . . . ?
C21A C19 C18 N5 8.4(12) . . . . ?
C22A C19 C18A N5 166.3(10) . . . . ?
C20 C19 C18A N5 -23.3(12) . . . . ?
C18 C19 C18A N5 54.4(7) . . . . ?
C20A C19 C18A N5 38.3(11) . . . . ?
C21 C19 C18A N5 -124.7(9) . . . . ?
C22 C19 C18A N5 135.3(6) . . . . ?
C21A C19 C18A N5 -73.2(10) . . . . ?
C17 N5 C18A C19 166.0(6) . . . . ?
C18 N5 C18A C19 -55.8(7) . . . . ?
C11 N3 C23 C24 103.4(4) . . . . ?
C12 N3 C23 C24 -131.2(3) . . . . ?
Ni1 N3 C23 C24 -14.2(4) . . . . ?
C28 N6 C24 C25 -1.1(5) . . . . ?
Ni1 N6 C24 C25 168.0(3) . . . . ?
C28 N6 C24 C23 175.9(3) . . . . ?
Ni1 N6 C24 C23 -15.0(4) . . . . ?
N3 C23 C24 N6 20.0(5) . . . . ?
N3 C23 C24 C25 -162.9(3) . . . . ?
N6 C24 C25 C26 0.8(6) . . . . ?
C23 C24 C25 C26 -176.1(4) . . . . ?
C24 C25 C26 C27 0.4(6) . . . . ?
C25 C26 C27 C28 -1.3(6) . . . . ?
C24 N6 C28 C27 0.2(5) . . . . ?
Ni1 N6 C28 C27 -167.4(3) . . . . ?
C26 C27 C28 N6 1.0(6) . . . . ?
Ni1 O2 C29 N7 -0.2(5) . . . . ?
Ni1 O2 C29 C30 -179.9(3) . . . . ?
O1 N7 C29 O2 0.1(6) . . . . ?
O1 N7 C29 C30 179.8(3) . . . . ?
O7 C31 N8 O7A -11(14) . . . . ?
C32 C31 N8 O7A -168(14) . . . . ?
