#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:38:05 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179070 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/32/4303271.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_4303271
loop_
_publ_author_name
'Mrigendra Dubey'
'Rik Rani Koner'
'Manabendra Ray'
_publ_contact_author_address
;Department of Chemistry
Indian Institute of Technology Guwahati
Guwahati 781039
;
_publ_contact_author_email       manabray@iitg.ernet.in
_publ_contact_author_name        'Dr. Manabendra Ray'
_publ_section_title
;
Sodium and Potassium Ion Directed Self-Assembled Multinuclear Assembly of
Divalent Nickel or Copper and l-Leucine Derived Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9294
_journal_page_last               9302
_journal_paper_doi               10.1021/ic9011444
_journal_volume                  48
_journal_year                    2009
_chemical_absolute_configuration syn
_chemical_compound_source        Synthesized
_chemical_formula_moiety
'C78 H108 N6 Na Ni3 O18, C F3 O3 S, 4(C2 N), O'
_chemical_formula_sum            'C87 H108 F3 N10 Na Ni3 O22 S'
_chemical_formula_weight         1934.01
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      20
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5336(6)
_cell_length_b                   21.0148(6)
_cell_length_c                   27.5553(9)
_cell_measurement_reflns_used    8899
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.82
_cell_measurement_theta_min      2.44
_cell_volume                     10153.2(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Wingx
_computing_publication_material  Wingx
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            35518
_diffrn_reflns_theta_full        24.24
_diffrn_reflns_theta_max         24.24
_diffrn_reflns_theta_min         1.48
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.650
_exptl_absorpt_correction_T_max  0.8810
_exptl_absorpt_correction_T_min  0.7811
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Purple-Blue
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Diamond
_exptl_crystal_F_000             4056
_exptl_crystal_recrystallization_method 'CH3OH CH3CN'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.005(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         8146
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0604P)²+5.0973P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.1035
_reflns_number_gt                6939
_reflns_number_total             8146
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic9011444_si_002_3.cif
_cod_data_source_block           capsule3
_cod_database_code               4303271
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -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
Na Na 0.79599(11) 0.0000 0.5000 0.0497(5) Uani 1 2 d S . .
H H 0.5458(19) 0.0274(18) 0.6238(13) 0.037(10) Uiso 1 1 d . . .
H2N H 0.962(2) 0.1030(19) 0.4800(13) 0.031(13) Uiso 1 1 d . . .
H1N H 0.6428 0.1183 0.4692 0.12(2) Uiso 1 1 d . . .
H50Z H 0.7746 0.0025 0.3674 0.089(16) Uiso 1 1 d . . .
Ni1 Ni 0.59759(4) 0.0000 0.5000 0.04093(16) Uani 1 2 d S . .
C6A C 0.5534(2) 0.12680(19) 0.56943(14) 0.0476(10) Uani 1 1 d . . .
C1A C 0.6105(2) 0.13665(17) 0.53528(13) 0.0461(9) Uani 1 1 d . . .
C5A C 0.5564(3) 0.1627(2) 0.61151(17) 0.0672(13) Uani 1 1 d . . .
H18 H 0.5191 0.1567 0.6351 0.081 Uiso 1 1 calc R . .
C2A C 0.6687(3) 0.1794(2) 0.54322(16) 0.0579(11) Uani 1 1 d . . .
H15 H 0.7076 0.1840 0.5205 0.070 Uiso 1 1 calc R . .
C3A C 0.6689(3) 0.2154(2) 0.58513(18) 0.0720(13) Uani 1 1 d . . .
H16 H 0.7070 0.2455 0.5901 0.086 Uiso 1 1 calc R . .
C4A C 0.6131(3) 0.2071(2) 0.61958(18) 0.0788(14) Uani 1 1 d . . .
H17 H 0.6135 0.2311 0.6480 0.095 Uiso 1 1 calc R . .
O1A O 0.60670(15) 0.10040(11) 0.49387(9) 0.0475(6) Uani 1 1 d . . .
C7A C 0.4914(2) 0.0792(2) 0.56048(15) 0.0515(10) Uani 1 1 d . . .
H20A H 0.4544 0.0817 0.5866 0.062 Uiso 1 1 calc R . .
H20B H 0.4655 0.0898 0.5304 0.062 Uiso 1 1 calc R . .
N1A N 0.52132(17) 0.01273(15) 0.55734(12) 0.0476(8) Uani 1 1 d . . .
H3 H 0.4810 -0.0138 0.5526 0.057 Uiso 1 1 calc R . .
Ni2 Ni 0.89364(3) 0.07030(2) 0.405986(15) 0.03659(12) Uani 1 1 d . . .
O3B1 O 0.79451(13) 0.09225(11) 0.43998(8) 0.0389(6) Uani 1 1 d . . .
O2B1 O 0.68869(15) 0.15037(13) 0.43035(10) 0.0521(7) Uani 1 1 d . . .
O1B O 0.82782(13) 0.00844(12) 0.36010(9) 0.0462(6) Uani 1 1 d . . .
O1B1 O 0.95212(16) 0.12288(13) 0.46134(11) 0.0429(7) Uani 1 1 d . . .
N1B1 N 0.87121(16) 0.15564(14) 0.37061(10) 0.0381(7) Uani 1 1 d . . .
H1 H 0.8824 0.1502 0.3386 0.046 Uiso 1 1 calc R . .
N1B N 0.99042(17) 0.04209(14) 0.36823(11) 0.0425(7) Uani 1 1 d . . .
H2 H 1.0178 0.0777 0.3613 0.051 Uiso 1 1 calc R . .
C1B C 0.8572(2) -0.04987(18) 0.34735(13) 0.0463(9) Uani 1 1 d . . .
C7B C 0.9731(2) 0.0098(2) 0.32135(13) 0.0526(10) Uani 1 1 d . . .
H1A H 1.0205 0.0008 0.3045 0.063 Uiso 1 1 calc R . .
H1B H 0.9433 0.0383 0.3011 0.063 Uiso 1 1 calc R . .
C6B C 0.9297(3) -0.0512(2) 0.32831(13) 0.0521(10) Uani 1 1 d . . .
C4B C 0.9188(4) -0.1647(3) 0.3204(2) 0.0857(17) Uani 1 1 d . . .
H6 H 0.9394 -0.2035 0.3107 0.103 Uiso 1 1 calc R . .
C2B C 0.8154(3) -0.1052(2) 0.35423(16) 0.0614(12) Uani 1 1 d . . .
H4 H 0.7671 -0.1040 0.3682 0.074 Uiso 1 1 calc R . .
C3B C 0.8478(4) -0.1625(2) 0.33950(19) 0.0757(15) Uani 1 1 d . . .
H5 H 0.8201 -0.1999 0.3429 0.091 Uiso 1 1 calc R . .
C5B C 0.9604(3) -0.1095(2) 0.31529(15) 0.0668(13) Uani 1 1 d . . .
H7 H 1.0097 -0.1114 0.3029 0.080 Uiso 1 1 calc R . .
C6B1 C 0.9040(2) 0.22409(16) 0.44139(12) 0.0401(8) Uani 1 1 d . . .
C1B1 C 0.9220(2) 0.17930(17) 0.47671(13) 0.0411(9) Uani 1 1 d . . .
C4B1 C 0.8604(3) 0.2949(2) 0.50471(18) 0.0666(12) Uani 1 1 d . . .
H12 H 0.8408 0.3341 0.5141 0.080 Uiso 1 1 calc R . .
C5B1 C 0.8728(2) 0.2814(2) 0.45615(16) 0.0550(11) Uani 1 1 d . . .
H11 H 0.8598 0.3116 0.4329 0.066 Uiso 1 1 calc R . .
C7B1 C 0.9188(2) 0.20897(18) 0.38898(12) 0.0418(9) Uani 1 1 d . . .
H8A H 0.9088 0.2466 0.3696 0.050 Uiso 1 1 calc R . .
H8B H 0.9722 0.1981 0.3850 0.050 Uiso 1 1 calc R . .
C2B1 C 0.9082(3) 0.1917(2) 0.52585(14) 0.0551(11) Uani 1 1 d . . .
H13 H 0.9195 0.1615 0.5494 0.066 Uiso 1 1 calc R . .
C8B1 C 0.7891(2) 0.16845(18) 0.37450(14) 0.0439(9) Uani 1 1 d . . .
H22 H 0.7827 0.2143 0.3796 0.053 Uiso 1 1 calc R . .
C9B1 C 0.7553(2) 0.13435(17) 0.41851(12) 0.0415(9) Uani 1 1 d . . .
10B1 C 0.7464(3) 0.1508(2) 0.32764(15) 0.0587(11) Uani 1 1 d . . .
H23A H 0.7676 0.1115 0.3151 0.070 Uiso 1 1 calc R . .
H23B H 0.6933 0.1429 0.3356 0.070 Uiso 1 1 calc R . .
11B1 C 0.7498(4) 0.2010(3) 0.28789(19) 0.098(2) Uani 1 1 d . . .
H24 H 0.8025 0.2164 0.2855 0.118 Uiso 1 1 calc R . .
O2B O 0.91897(13) -0.00715(11) 0.44579(8) 0.0401(6) Uani 1 1 d . . .
O3B O 1.01729(15) -0.06803(13) 0.46676(9) 0.0502(6) Uani 1 1 d . . .
C8B C 1.03747(19) 0.00201(19) 0.40121(13) 0.0454(8) Uani 1 1 d . . .
H26 H 1.0582 -0.0332 0.3820 0.054 Uiso 1 1 calc R . .
C10B C 1.1047(2) 0.0391(2) 0.42195(14) 0.0539(10) Uani 1 1 d . . .
H27A H 1.1318 0.0119 0.4445 0.065 Uiso 1 1 calc R . .
H27B H 1.0851 0.0751 0.4401 0.065 Uiso 1 1 calc R . .
C9B C 0.9872(2) -0.02692(16) 0.44156(13) 0.0384(8) Uani 1 1 d . . .
C11B C 1.1613(3) 0.0637(3) 0.3839(2) 0.0801(15) Uani 1 1 d . . .
H28 H 1.1336 0.0935 0.3630 0.096 Uiso 1 1 calc R . .
O2A O 0.67447(13) -0.00642(12) 0.44536(9) 0.0415(6) Uani 1 1 d . . .
C3B1 C 0.8776(3) 0.2495(2) 0.53851(16) 0.0671(13) Uani 1 1 d . . .
H73 H 0.8682 0.2580 0.5711 0.081 Uiso 1 1 calc R . .
C8A C 0.5601(2) -0.0068(2) 0.60241(15) 0.0476(9) Uani 1 1 d . . .
C10A C 0.5400(2) -0.0753(2) 0.61781(15) 0.0583(11) Uani 1 1 d . . .
H71A H 0.5454 -0.1028 0.5897 0.070 Uiso 1 1 calc R . .
H71B H 0.5771 -0.0892 0.6417 0.070 Uiso 1 1 calc R . .
C11A C 0.4622(4) -0.0850(3) 0.6385(3) 0.107(2) Uani 1 1 d . . .
H72 H 0.4253 -0.0742 0.6131 0.129 Uiso 1 1 calc R . .
C13B C 1.2247(3) 0.1019(3) 0.4100(3) 0.116(2) Uani 1 1 d . . .
H75A H 1.2019 0.1336 0.4304 0.174 Uiso 1 1 calc R . .
H75B H 1.2566 0.1222 0.3863 0.174 Uiso 1 1 calc R . .
H75C H 1.2549 0.0736 0.4294 0.174 Uiso 1 1 calc R . .
13B1 C 0.7279(6) 0.1723(5) 0.2397(2) 0.166(4) Uani 1 1 d . . .
H74A H 0.7618 0.1378 0.2323 0.249 Uiso 1 1 calc R . .
H74B H 0.7315 0.2042 0.2149 0.249 Uiso 1 1 calc R . .
H74C H 0.6765 0.1567 0.2414 0.249 Uiso 1 1 calc R . .
S1 S 0.0000 0.16814(9) 0.2500 0.0923(7) Uani 1 2 d S . .
C76 C 0.0000 0.2535(4) 0.2500 0.078(2) Uani 1 2 d S . .
O21 O -0.0685(4) 0.1509(3) 0.2700(2) 0.130(3) Uani 0.75 1 d P . .
O23 O 0.0308(7) 0.1548(3) 0.3008(3) 0.183(4) Uani 0.75 1 d P . .
C12B C 1.1948(4) 0.0140(5) 0.3521(3) 0.141(3) Uani 1 1 d . . .
H78A H 1.2294 0.0334 0.3295 0.212 Uiso 1 1 calc R . .
H78B H 1.1547 -0.0071 0.3345 0.212 Uiso 1 1 calc R . .
H78C H 1.2217 -0.0165 0.3715 0.212 Uiso 1 1 calc R . .
C12A C 0.4517(5) -0.1552(3) 0.6506(3) 0.152(4) Uani 1 1 d . . .
H79A H 0.4019 -0.1616 0.6643 0.227 Uiso 1 1 calc R . .
H79B H 0.4898 -0.1681 0.6736 0.227 Uiso 1 1 calc R . .
H79C H 0.4566 -0.1800 0.6215 0.227 Uiso 1 1 calc R . .
12B1 C 0.6988(6) 0.2571(4) 0.3007(3) 0.181(4) Uani 1 1 d . . .
H77A H 0.7008 0.2881 0.2752 0.272 Uiso 1 1 calc R . .
H77B H 0.7161 0.2760 0.3305 0.272 Uiso 1 1 calc R . .
H77C H 0.6472 0.2425 0.3047 0.272 Uiso 1 1 calc R . .
F1 F 0.0065(6) 0.2792(2) 0.21076(16) 0.150(3) Uani 0.75 1 d P . .
C13A C 0.4441(6) -0.0473(5) 0.6803(5) 0.240(7) Uani 1 1 d . . .
H80A H 0.3937 -0.0578 0.6914 0.360 Uiso 1 1 calc R . .
H80B H 0.4462 -0.0030 0.6719 0.360 Uiso 1 1 calc R . .
H80C H 0.4803 -0.0560 0.7056 0.360 Uiso 1 1 calc R . .
C9A C 0.64641(19) 0.00068(18) 0.40343(14) 0.0431(8) Uani 1 1 d . . .
O3A O 0.68505(14) 0.00364(15) 0.36515(9) 0.0558(7) Uani 1 1 d . . .
F3 F 0.0735(5) 0.2729(3) 0.2527(5) 0.232(5) Uani 0.75 1 d P . .
C85 C 0.1382(7) 0.8173(6) 0.4477(6) 0.194(5) Uani 1 1 d DU . .
N100 N 0.1754(9) 0.4192(7) 0.2571(3) 0.287(7) Uani 1 1 d DU . .
C83 C 0.1545(8) 0.4048(6) 0.2155(4) 0.216(6) Uani 1 1 d DU . .
C84 C 0.1441(7) 0.3828(5) 0.1710(4) 0.175(4) Uani 1 1 d DU . .
O28 O 0.3599(3) 0.0000 0.5000 0.129(2) Uani 1 2 d S . .
N101 N 0.2446(7) 0.9095(5) 0.4558(5) 0.235(6) Uani 1 1 d DU . .
C86 C 0.1954(8) 0.8686(5) 0.4514(4) 0.165(4) Uani 1 1 d DU . .
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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
O3B1 Na O3B1 178.83(14) . 4_556 ?
O3B1 Na O2A 69.94(8) . . ?
O3B1 Na O2A 109.05(9) 4_556 . ?
O3B1 Na O2A 109.05(9) . 4_556 ?
O3B1 Na O2A 69.94(8) 4_556 4_556 ?
O2A Na O2A 70.71(11) . 4_556 ?
O3B1 Na O2B 109.50(9) . 4_556 ?
O3B1 Na O2B 71.51(8) 4_556 4_556 ?
O2A Na O2B 179.38(9) . 4_556 ?
O2A Na O2B 109.80(7) 4_556 4_556 ?
O3B1 Na O2B 71.51(8) . . ?
O3B1 Na O2B 109.50(9) 4_556 . ?
O2A Na O2B 109.80(7) . . ?
O2A Na O2B 179.38(9) 4_556 . ?
O2B Na O2B 69.70(11) 4_556 . ?
O3B1 Na Ni2 35.84(5) . . ?
O3B1 Na Ni2 145.16(8) 4_556 . ?
O2A Na Ni2 89.66(5) . . ?
O2A Na Ni2 144.89(7) 4_556 . ?
O2B Na Ni2 89.72(7) 4_556 . ?
O2B Na Ni2 35.67(5) . . ?
O3B1 Na Ni2 145.17(8) . 4_556 ?
O3B1 Na Ni2 35.84(5) 4_556 4_556 ?
O2A Na Ni2 144.89(7) . 4_556 ?
O2A Na Ni2 89.66(5) 4_556 4_556 ?
O2B Na Ni2 35.67(5) 4_556 4_556 ?
O2B Na Ni2 89.72(7) . 4_556 ?
Ni2 Na Ni2 120.28(6) . 4_556 ?
O3B1 Na Ni1 89.42(7) . . ?
O3B1 Na Ni1 89.42(7) 4_556 . ?
O2A Na Ni1 35.35(6) . . ?
O2A Na Ni1 35.35(6) 4_556 . ?
O2B Na Ni1 145.15(6) 4_556 . ?
O2B Na Ni1 145.15(6) . . ?
Ni2 Na Ni1 119.86(3) . . ?
Ni2 Na Ni1 119.86(3) 4_556 . ?
O2A Ni1 O2A 96.55(13) 4_556 . ?
O2A Ni1 N1A 81.67(10) 4_556 . ?
O2A Ni1 N1A 176.12(12) . . ?
O2A Ni1 N1A 176.12(12) 4_556 4_556 ?
O2A Ni1 N1A 81.67(10) . 4_556 ?
N1A Ni1 N1A 100.31(18) . 4_556 ?
O2A Ni1 O1A 86.72(10) 4_556 . ?
O2A Ni1 O1A 87.54(10) . . ?
N1A Ni1 O1A 88.91(11) . . ?
N1A Ni1 O1A 96.63(11) 4_556 . ?
O2A Ni1 O1A 87.54(10) 4_556 4_556 ?
O2A Ni1 O1A 86.72(10) . 4_556 ?
N1A Ni1 O1A 96.63(11) . 4_556 ?
N1A Ni1 O1A 88.91(11) 4_556 4_556 ?
O1A Ni1 O1A 171.37(15) . 4_556 ?
O2A Ni1 Na 48.27(7) 4_556 . ?
O2A Ni1 Na 48.27(7) . . ?
N1A Ni1 Na 129.85(9) . . ?
N1A Ni1 Na 129.85(9) 4_556 . ?
O1A Ni1 Na 85.68(7) . . ?
O1A Ni1 Na 85.68(7) 4_556 . ?
C5A C6A C1A 117.3(4) . . ?
C5A C6A C7A 122.0(4) . . ?
C1A C6A C7A 120.7(4) . . ?
O1A C1A C2A 122.0(4) . . ?
O1A C1A C6A 116.4(3) . . ?
C2A C1A C6A 121.6(4) . . ?
C4A C5A C6A 122.0(4) . . ?
C4A C5A H18 119.0 . . ?
C6A C5A H18 119.0 . . ?
C1A C2A C3A 119.4(4) . . ?
C1A C2A H15 120.3 . . ?
C3A C2A H15 120.3 . . ?
C4A C3A C2A 120.5(5) . . ?
C4A C3A H16 119.7 . . ?
C2A C3A H16 119.7 . . ?
C3A C4A C5A 119.1(4) . . ?
C3A C4A H17 120.4 . . ?
C5A C4A H17 120.4 . . ?
C1A O1A Ni1 119.3(2) . . ?
C1A O1A H1N 109.0 . . ?
Ni1 O1A H1N 118.00 . . ?
N1A C7A C6A 112.3(3) . . ?
N1A C7A H20A 109.1 . . ?
C6A C7A H20A 109.1 . . ?
N1A C7A H20B 109.1 . . ?
C6A C7A H20B 109.1 . . ?
H20A C7A H20B 107.9 . . ?
C8A N1A C7A 111.9(3) . . ?
C8A N1A Ni1 107.9(2) . . ?
C7A N1A Ni1 112.8(2) . . ?
C8A N1A H3 108.0 . . ?
C7A N1A H3 108.0 . . ?
Ni1 N1A H3 108.0 . . ?
O2B Ni2 O3B1 96.98(9) . . ?
O2B Ni2 N1B 82.06(10) . . ?
O3B1 Ni2 N1B 175.39(11) . . ?
O2B Ni2 N1B1 174.36(11) . . ?
O3B1 Ni2 N1B1 81.85(10) . . ?
N1B Ni2 N1B1 99.55(11) . . ?
O2B Ni2 O1B1 85.62(11) . . ?
O3B1 Ni2 O1B1 87.94(10) . . ?
N1B Ni2 O1B1 96.47(12) . . ?
N1B1 Ni2 O1B1 88.82(11) . . ?
O2B Ni2 O1B 87.13(10) . . ?
O3B1 Ni2 O1B 87.08(9) . . ?
N1B Ni2 O1B 88.36(11) . . ?
N1B1 Ni2 O1B 98.30(11) . . ?
O1B1 Ni2 O1B 170.64(11) . . ?
O2B Ni2 Na 49.59(7) . . ?
O3B1 Ni2 Na 47.38(7) . . ?
N1B Ni2 Na 131.42(9) . . ?
N1B1 Ni2 Na 129.03(8) . . ?
O1B1 Ni2 Na 85.62(8) . . ?
O1B Ni2 Na 85.18(7) . . ?
C9B1 O3B1 Ni2 114.1(2) . . ?
C9B1 O3B1 Na 147.1(2) . . ?
Ni2 O3B1 Na 96.78(10) . . ?
C1B O1B Ni2 119.2(2) . . ?
C1B O1B H50Z 108.0 . . ?
Ni2 O1B H50Z 118.00 . . ?
C1B1 O1B1 Ni2 118.9(2) . . ?
C1B1 O1B1 H2N 113(3) . . ?
Ni2 O1B1 H2N 110(3) . . ?
C8B1 N1B1 C7B1 112.8(3) . . ?
C8B1 N1B1 Ni2 108.0(2) . . ?
C7B1 N1B1 Ni2 112.6(2) . . ?
C8B1 N1B1 H1 107.7 . . ?
C7B1 N1B1 H1 107.7 . . ?
Ni2 N1B1 H1 107.7 . . ?
C8B N1B C7B 112.6(3) . . ?
C8B N1B Ni2 108.0(2) . . ?
C7B N1B Ni2 113.4(2) . . ?
C8B N1B H2 107.5 . . ?
C7B N1B H2 107.5 . . ?
Ni2 N1B H2 107.5 . . ?
C6B C1B O1B 117.5(4) . . ?
C6B C1B C2B 121.6(4) . . ?
O1B C1B C2B 120.9(4) . . ?
N1B C7B C6B 112.4(3) . . ?
N1B C7B H1A 109.1 . . ?
C6B C7B H1A 109.1 . . ?
N1B C7B H1B 109.1 . . ?
C6B C7B H1B 109.1 . . ?
H1A C7B H1B 107.9 . . ?
C1B C6B C5B 118.4(4) . . ?
C1B C6B C7B 119.9(4) . . ?
C5B C6B C7B 121.7(4) . . ?
C3B C4B C5B 119.8(5) . . ?
C3B C4B H6 120.1 . . ?
C5B C4B H6 120.1 . . ?
C1B C2B C3B 118.0(5) . . ?
C1B C2B H4 121.0 . . ?
C3B C2B H4 121.0 . . ?
C4B C3B C2B 121.3(5) . . ?
C4B C3B H5 119.3 . . ?
C2B C3B H5 119.3 . . ?
C4B C5B C6B 120.9(5) . . ?
C4B C5B H7 119.6 . . ?
C6B C5B H7 119.6 . . ?
C5B1 C6B1 C1B1 118.2(3) . . ?
C5B1 C6B1 C7B1 122.3(3) . . ?
C1B1 C6B1 C7B1 119.4(3) . . ?
O1B1 C1B1 C6B1 117.3(3) . . ?
O1B1 C1B1 C2B1 121.9(3) . . ?
C6B1 C1B1 C2B1 120.8(3) . . ?
C3B1 C4B1 C5B1 118.8(4) . . ?
C3B1 C4B1 H12 120.6 . . ?
C5B1 C4B1 H12 120.6 . . ?
C6B1 C5B1 C4B1 121.6(4) . . ?
C6B1 C5B1 H11 119.2 . . ?
C4B1 C5B1 H11 119.2 . . ?
N1B1 C7B1 C6B1 112.9(3) . . ?
N1B1 C7B1 H8A 109.0 . . ?
C6B1 C7B1 H8A 109.0 . . ?
N1B1 C7B1 H8B 109.0 . . ?
C6B1 C7B1 H8B 109.0 . . ?
H8A C7B1 H8B 107.8 . . ?
C3B1 C2B1 C1B1 118.6(4) . . ?
C3B1 C2B1 H13 120.7 . . ?
C1B1 C2B1 H13 120.7 . . ?
N1B1 C8B1 C9B1 110.6(3) . . ?
N1B1 C8B1 10B1 111.8(3) . . ?
C9B1 C8B1 10B1 111.4(3) . . ?
N1B1 C8B1 H22 107.6 . . ?
C9B1 C8B1 H22 107.6 . . ?
10B1 C8B1 H22 107.6 . . ?
O2B1 C9B1 O3B1 124.7(3) . . ?
O2B1 C9B1 C8B1 116.1(3) . . ?
O3B1 C9B1 C8B1 119.2(3) . . ?
11B1 10B1 C8B1 114.7(4) . . ?
11B1 10B1 H23A 108.6 . . ?
C8B1 10B1 H23A 108.6 . . ?
11B1 10B1 H23B 108.6 . . ?
C8B1 10B1 H23B 108.6 . . ?
H23A 10B1 H23B 107.6 . . ?
13B1 11B1 10B1 110.3(5) . . ?
13B1 11B1 12B1 111.4(6) . . ?
10B1 11B1 12B1 110.2(6) . . ?
13B1 11B1 H24 108.3 . . ?
10B1 11B1 H24 108.3 . . ?
12B1 11B1 H24 108.3 . . ?
C9B O2B Ni2 115.0(2) . . ?
C9B O2B Na 147.4(2) . . ?
Ni2 O2B Na 94.73(9) . . ?
N1B C8B C10B 111.6(3) . . ?
N1B C8B C9B 110.3(3) . . ?
C10B C8B C9B 111.9(3) . . ?
N1B C8B H26 107.6 . . ?
C10B C8B H26 107.6 . . ?
C9B C8B H26 107.6 . . ?
C8B C10B C11B 114.7(3) . . ?
C8B C10B H27A 108.6 . . ?
C11B C10B H27A 108.6 . . ?
C8B C10B H27B 108.6 . . ?
C11B C10B H27B 108.6 . . ?
H27A C10B H27B 107.6 . . ?
O3B C9B O2B 125.6(3) . . ?
O3B C9B C8B 116.1(3) . . ?
O2B C9B C8B 118.3(3) . . ?
C12B C11B C10B 115.0(5) . . ?
C12B C11B C13B 110.8(5) . . ?
C10B C11B C13B 108.9(5) . . ?
C12B C11B H28 107.3 . . ?
C10B C11B H28 107.3 . . ?
C13B C11B H28 107.3 . . ?
C9A O2A Ni1 114.4(2) . . ?
C9A O2A Na 146.9(2) . . ?
Ni1 O2A Na 96.37(9) . . ?
C4B1 C3B1 C2B1 122.0(4) . . ?
C4B1 C3B1 H73 119.0 . . ?
C2B1 C3B1 H73 119.0 . . ?
N1A C8A C9A 110.2(3) . 4_556 ?
N1A C8A C10A 112.7(3) . . ?
C9A C8A C10A 109.5(4) 4_556 . ?
N1A C8A H 101(2) . . ?
C9A C8A H 105(2) 4_556 . ?
C10A C8A H 118(2) . . ?
C11A C10A C8A 116.2(4) . . ?
C11A C10A H71A 108.2 . . ?
C8A C10A H71A 108.2 . . ?
C11A C10A H71B 108.2 . . ?
C8A C10A H71B 108.2 . . ?
H71A C10A H71B 107.4 . . ?
C13A C11A C10A 115.7(7) . . ?
C13A C11A C12A 109.3(7) . . ?
C10A C11A C12A 109.1(6) . . ?
C13A C11A H72 107.5 . . ?
C10A C11A H72 107.5 . . ?
C12A C11A H72 107.5 . . ?
C11B C13B H75A 109.5 . . ?
C11B C13B H75B 109.5 . . ?
H75A C13B H75B 109.5 . . ?
C11B C13B H75C 109.5 . . ?
H75A C13B H75C 109.5 . . ?
H75B C13B H75C 109.5 . . ?
11B1 13B1 H74A 109.5 . . ?
11B1 13B1 H74B 109.5 . . ?
H74A 13B1 H74B 109.5 . . ?
11B1 13B1 H74C 109.5 . . ?
H74A 13B1 H74C 109.5 . . ?
H74B 13B1 H74C 109.5 . . ?
O21 S1 O21 149.3(6) 3 . ?
O21 S1 O23 90.6(5) 3 . ?
O21 S1 O23 83.8(5) . . ?
O21 S1 O23 83.8(5) 3 3 ?
O21 S1 O23 90.6(5) . 3 ?
O23 S1 O23 158.8(6) . 3 ?
O21 S1 C76 105.3(3) 3 . ?
O21 S1 C76 105.3(3) . . ?
O23 S1 C76 100.6(3) . . ?
O23 S1 C76 100.6(3) 3 . ?
F1 C76 F1 127.2(8) 3 . ?
F1 C76 F3 84.6(6) 3 . ?
F1 C76 F3 80.0(6) . . ?
F1 C76 F3 80.0(6) 3 3 ?
F1 C76 F3 84.6(6) . 3 ?
F3 C76 F3 144.9(9) . 3 ?
F1 C76 S1 116.4(4) 3 . ?
F1 C76 S1 116.4(4) . . ?
F3 C76 S1 107.5(5) . . ?
F3 C76 S1 107.5(5) 3 . ?
C11B C12B H78A 109.5 . . ?
C11B C12B H78B 109.5 . . ?
H78A C12B H78B 109.5 . . ?
C11B C12B H78C 109.5 . . ?
H78A C12B H78C 109.5 . . ?
H78B C12B H78C 109.5 . . ?
C11A C12A H79A 109.5 . . ?
C11A C12A H79B 109.5 . . ?
H79A C12A H79B 109.5 . . ?
C11A C12A H79C 109.5 . . ?
H79A C12A H79C 109.5 . . ?
H79B C12A H79C 109.5 . . ?
11B1 12B1 H77A 109.5 . . ?
11B1 12B1 H77B 109.5 . . ?
H77A 12B1 H77B 109.5 . . ?
11B1 12B1 H77C 109.5 . . ?
H77A 12B1 H77C 109.5 . . ?
H77B 12B1 H77C 109.5 . . ?
C76 F1 F3 51.1(5) . 3 ?
C11A C13A H80A 109.5 . . ?
C11A C13A H80B 109.5 . . ?
H80A C13A H80B 109.5 . . ?
C11A C13A H80C 109.5 . . ?
H80A C13A H80C 109.5 . . ?
H80B C13A H80C 109.5 . . ?
O3A C9A O2A 124.3(3) . . ?
O3A C9A C8A 116.2(4) . 4_556 ?
O2A C9A C8A 119.5(3) . 4_556 ?
C76 F3 F1 44.3(3) . 3 ?
N100 C83 C84 169.2(17) . . ?
N101 C86 C85 177.3(14) . . ?
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
Na O3B1 2.548(2) . ?
Na O3B1 2.548(2) 4_556 ?
Na O2A 2.612(3) . ?
Na O2A 2.612(3) 4_556 ?
Na O2B 2.627(3) 4_556 ?
Na O2B 2.627(3) . ?
Na Ni2 3.4387(11) . ?
Na Ni2 3.4387(11) 4_556 ?
Na Ni1 3.479(2) . ?
Ni1 O2A 2.025(2) 4_556 ?
Ni1 O2A 2.025(2) . ?
Ni1 N1A 2.087(3) . ?
Ni1 N1A 2.087(3) 4_556 ?
Ni1 O1A 2.123(2) . ?
Ni1 O1A 2.123(2) 4_556 ?
C6A C5A 1.384(6) . ?
C6A C1A 1.389(6) . ?
C6A C7A 1.497(6) . ?
C1A O1A 1.374(4) . ?
C1A C2A 1.378(6) . ?
C5A C4A 1.382(7) . ?
C5A H18 0.9300 . ?
C2A C3A 1.380(6) . ?
C2A H15 0.9300 . ?
C3A C4A 1.373(7) . ?
C3A H16 0.9300 . ?
C4A H17 0.9300 . ?
O1A H1N 1.000 . ?
C7A N1A 1.495(5) . ?
C7A H20A 0.9700 . ?
C7A H20B 0.9700 . ?
N1A C8A 1.474(5) . ?
N1A H3 0.9100 . ?
Ni2 O2B 2.012(2) . ?
Ni2 O3B1 2.028(2) . ?
Ni2 N1B 2.077(3) . ?
Ni2 N1B1 2.079(3) . ?
Ni2 O1B1 2.145(3) . ?
Ni2 O1B 2.150(2) . ?
O3B1 C9B1 1.267(4) . ?
O2B1 C9B1 1.259(4) . ?
O1B C1B 1.375(5) . ?
O1B H50Z 0.9600 . ?
O1B1 C1B1 1.365(4) . ?
O1B1 H2N 0.68(4) . ?
N1B1 C8B1 1.469(5) . ?
N1B1 C7B1 1.486(5) . ?
N1B1 H1 0.9100 . ?
N1B C8B 1.489(5) . ?
N1B C7B 1.490(5) . ?
N1B H2 0.9100 . ?
C1B C6B 1.375(6) . ?
C1B C2B 1.388(6) . ?
C7B C6B 1.503(6) . ?
C7B H1A 0.9700 . ?
C7B H1B 0.9700 . ?
C6B C5B 1.384(6) . ?
C4B C3B 1.352(8) . ?
C4B C5B 1.379(8) . ?
C4B H6 0.9300 . ?
C2B C3B 1.392(7) . ?
C2B H4 0.9300 . ?
C3B H5 0.9300 . ?
C5B H7 0.9300 . ?
C6B1 C5B1 1.385(5) . ?
C6B1 C1B1 1.390(5) . ?
C6B1 C7B1 1.501(5) . ?
C1B1 C2B1 1.400(5) . ?
C4B1 C3B1 1.367(7) . ?
C4B1 C5B1 1.385(6) . ?
C4B1 H12 0.9300 . ?
C5B1 H11 0.9300 . ?
C7B1 H8A 0.9700 . ?
C7B1 H8B 0.9700 . ?
C2B1 C3B1 1.372(6) . ?
C2B1 H13 0.9300 . ?
C8B1 C9B1 1.528(5) . ?
C8B1 10B1 1.538(6) . ?
C8B1 H22 0.9800 . ?
10B1 11B1 1.521(7) . ?
10B1 H23A 0.9700 . ?
10B1 H23B 0.9700 . ?
11B1 13B1 1.507(9) . ?
11B1 12B1 1.522(11) . ?
11B1 H24 0.9800 . ?
O2B C9B 1.272(4) . ?
O3B C9B 1.227(4) . ?
C8B C10B 1.524(6) . ?
C8B C9B 1.543(5) . ?
C8B H26 0.9800 . ?
C10B C11B 1.533(6) . ?
C10B H27A 0.9700 . ?
C10B H27B 0.9700 . ?
C11B C12B 1.486(10) . ?
C11B C13B 1.547(8) . ?
C11B H28 0.9800 . ?
O2A C9A 1.265(4) . ?
C3B1 H73 0.9300 . ?
C8A C9A 1.528(5) 4_556 ?
C8A C10A 1.543(6) . ?
C8A H 0.96(4) . ?
C10A C11A 1.491(7) . ?
C10A H71A 0.9700 . ?
C10A H71B 0.9700 . ?
C11A C13A 1.435(11) . ?
C11A C12A 1.523(9) . ?
C11A H72 0.9800 . ?
C13B H75A 0.9600 . ?
C13B H75B 0.9600 . ?
C13B H75C 0.9600 . ?
13B1 H74A 0.9600 . ?
13B1 H74B 0.9600 . ?
13B1 H74C 0.9600 . ?
S1 O21 1.370(6) 3 ?
S1 O21 1.370(6) . ?
S1 O23 1.526(9) . ?
S1 O23 1.526(9) 3 ?
S1 C76 1.795(8) . ?
C76 F1 1.214(6) 3 ?
C76 F1 1.214(6) . ?
C76 F3 1.353(9) . ?
C76 F3 1.353(9) 3 ?
C12B H78A 0.9600 . ?
C12B H78B 0.9600 . ?
C12B H78C 0.9600 . ?
C12A H79A 0.9600 . ?
C12A H79B 0.9600 . ?
C12A H79C 0.9600 . ?
12B1 H77A 0.9600 . ?
12B1 H77B 0.9600 . ?
12B1 H77C 0.9600 . ?
F1 F3 1.731(10) 3 ?
C13A H80A 0.9600 . ?
C13A H80B 0.9600 . ?
C13A H80C 0.9600 . ?
C9A O3A 1.255(4) . ?
C9A C8A 1.528(5) 4_556 ?
F3 F1 1.731(10) 3 ?
C85 C86 1.477(13) . ?
N100 C83 1.239(9) . ?
C83 C84 1.325(9) . ?
N101 C86 1.223(11) . ?
