#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:29:39 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180184 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/80/7108024.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_7108024
loop_
_publ_author_name
'Radu Custelcean'
'Peter V. Bonnesen'
'Benjamin D. Roach'
'Nathan C. Duncan'
_publ_section_title
;
 Ion-pair triple helicates and mesocates self-assembled from ditopic
 2,2'-bipyridine-bis(urea) ligands and Ni(II) or Fe(II) sulfate salts
;
_journal_name_full               Chem.Commun.
_journal_page_first              7438
_journal_paper_doi               10.1039/c2cc33062h
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C87 H89 N23 Ni O21 S'
_chemical_formula_weight         1883.58
_chemical_name_common            H1b
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.997(2)
_cell_angle_beta                 104.132(2)
_cell_angle_gamma                108.688(2)
_cell_formula_units_Z            2
_cell_length_a                   13.7888(11)
_cell_length_b                   19.1350(15)
_cell_length_c                   19.5872(16)
_cell_measurement_temperature    173(2)
_cell_volume                     4652.6(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45983
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_T_max  0.9545
_exptl_absorpt_correction_T_min  0.9400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.901
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1200
_refine_ls_number_reflns         16391
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0667
_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)+(0.1363P)²+0.4837P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1967
_refine_ls_wR_factor_ref         0.2147
_reflns_number_gt                11542
_reflns_number_total             16391
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc33062h.txt
_cod_data_source_block           c:\frames\470\work\470sq
_cod_original_cell_volume        4652.6(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7108024
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Ni1 Ni 0.67727(3) 0.86281(2) 0.66305(2) 0.04498(15) Uani 1 1 d .
S1 S 0.96397(7) 1.26277(5) 0.78205(4) 0.0428(2) Uani 1 1 d .
O1 O 1.04155(18) 1.22723(13) 0.81316(12) 0.0460(5) Uani 1 1 d .
N1 N 0.7010(2) 0.79271(17) 0.58501(16) 0.0514(7) Uani 1 1 d .
C1 C 0.7192(3) 0.8218(2) 0.52789(19) 0.0493(8) Uani 1 1 d .
O2 O 0.8641(2) 1.22709(18) 0.80002(16) 0.0731(8) Uani 1 1 d .
N2 N 0.7017(2) 0.93074(16) 0.58803(14) 0.0471(7) Uani 1 1 d .
C2 C 0.7336(3) 0.7819(2) 0.4701(2) 0.0641(10) Uani 1 1 d .
H2 H 0.7454 0.8038 0.4301 0.077 Uiso 1 1 calc R
O3 O 0.9398(2) 1.24827(15) 0.70447(13) 0.0578(6) Uani 1 1 d .
N3 N 0.7174(3) 1.15615(18) 0.61594(17) 0.0594(8) Uani 1 1 d .
H3 H 0.7787 1.1824 0.6487 0.071 Uiso 1 1 calc R
C3 C 0.7300(3) 0.7092(3) 0.4728(3) 0.0772(13) Uani 1 1 d .
H3A H 0.7384 0.6799 0.4339 0.093 Uiso 1 1 calc R
O4 O 1.0078(2) 1.34257(15) 0.81225(17) 0.0787(9) Uani 1 1 d .
N4 N 0.6396(2) 1.1819(2) 0.70013(18) 0.0642(9) Uani 1 1 d .
H4 H 0.7056 1.2112 0.7243 0.077 Uiso 1 1 calc R
C4 C 0.7144(4) 0.6793(3) 0.5320(3) 0.0725(12) Uani 1 1 d .
H4A H 0.7135 0.6299 0.5351 0.087 Uiso 1 1 calc R
O5 O 0.93383(19) 1.07868(13) 0.99019(13) 0.0512(6) Uani 1 1 d .
N5 N 0.7045(2) 1.26992(16) 0.83587(17) 0.0527(7) Uani 1 1 d .
H5 H 0.7572 1.2527 0.8395 0.063 Uiso 1 1 calc R
C5 C 0.7001(3) 0.7232(2) 0.5871(2) 0.0639(10) Uani 1 1 d .
H5A H 0.6892 0.7028 0.6279 0.077 Uiso 1 1 calc R
O6 O 1.3323(2) 1.38750(14) 1.02230(14) 0.0584(7) Uani 1 1 d .
N6 N 0.8367(2) 1.38517(15) 0.87151(15) 0.0449(6) Uani 1 1 d .
H6 H 0.8764 1.3592 0.8632 0.054 Uiso 1 1 calc R
C6 C 0.7225(2) 0.9001(2) 0.53019(17) 0.0468(8) Uani 1 1 d .
O7 O 1.3505(4) 1.7196(2) 0.8479(2) 0.1246(16) Uani 1 1 d .
N7 N 1.0704(4) 1.6945(2) 0.9731(2) 0.0726(10) Uani 1 1 d .
C7 C 0.7450(3) 0.9408(2) 0.47766(18) 0.0548(9) Uani 1 1 d .
H7 H 0.7607 0.9189 0.4379 0.066 Uiso 1 1 calc R
O8 O 1.4138(3) 1.74955(17) 0.9628(2) 0.0835(9) Uani 1 1 d .
N8 N 0.5113(2) 0.82509(16) 0.62035(15) 0.0486(7) Uani 1 1 d .
C8 C 0.7444(3) 1.0127(2) 0.48323(19) 0.0566(9) Uani 1 1 d .
H8 H 0.7596 1.0408 0.4474 0.068 Uiso 1 1 calc R
O9 O 1.1037(2) 1.07238(16) 0.62220(15) 0.0659(7) Uani 1 1 d .
N9 N 0.6378(2) 0.93471(15) 0.73042(14) 0.0430(6) Uani 1 1 d .
C9 C 0.7215(3) 1.0441(2) 0.54175(19) 0.0536(9) Uani 1 1 d .
O10 O 0.9278(2) 1.35638(16) 0.51822(15) 0.0738(8) Uani 1 1 d .
N10 N 0.8605(2) 1.11668(15) 0.88999(14) 0.0459(7) Uani 1 1 d .
H10 H 0.8725 1.1361 0.8527 0.055 Uiso 1 1 calc R
C10 C 0.7013(3) 1.0011(2) 0.59238(18) 0.0521(9) Uani 1 1 d .
H10A H 0.6862 1.0225 0.6327 0.063 Uiso 1 1 calc R
O11 O 0.8884(4) 1.6854(2) 0.6724(2) 0.1237(16) Uani 1 1 d .
N11 N 1.0411(2) 1.14921(15) 0.93035(15) 0.0455(6) Uani 1 1 d .
H11 H 1.0387 1.1692 0.8918 0.055 Uiso 1 1 calc R
C11 C 0.7171(4) 1.1220(2) 0.5465(2) 0.0657(11) Uani 1 1 d .
H11A H 0.7793 1.1548 0.5340 0.079 Uiso 1 1 calc R
H11B H 0.6514 1.1196 0.5101 0.079 Uiso 1 1 calc R
O12 O 0.9188(5) 1.6689(3) 0.7794(2) 0.1398(19) Uani 1 1 d .
N12 N 1.2095(2) 1.28117(16) 0.94295(17) 0.0527(7) Uani 1 1 d .
H12 H 1.1599 1.2658 0.9011 0.063 Uiso 1 1 calc R
C12 C 0.6254(3) 1.1482(2) 0.6310(2) 0.0636(10) Uani 1 1 d .
O13 O 0.5373(2) 1.1135(2) 0.58809(17) 0.0931(11) Uani 1 1 d .
N13 N 1.2232(2) 1.39591(15) 0.91706(16) 0.0483(7) Uani 1 1 d .
H13 H 1.1662 1.3689 0.8811 0.058 Uiso 1 1 calc R
C13 C 0.5634(3) 1.1758(2) 0.7374(2) 0.0606(10) Uani 1 1 d .
O14 O 0.6637(2) 1.37307(15) 0.86604(17) 0.0682(8) Uani 1 1 d .
N14 N 1.3689(3) 1.7027(2) 0.9074(3) 0.0765(10) Uani 1 1 d .
C14 C 0.4567(3) 1.1280(3) 0.7083(3) 0.0763(13) Uani 1 1 d .
H14 H 0.4329 1.0999 0.6605 0.092 Uiso 1 1 calc R
O15 O 1.0199(3) 1.73705(18) 0.9763(2) 0.1100(13) Uani 1 1 d .
N15 N 0.6726(2) 0.79098(16) 0.73654(15) 0.0514(7) Uani 1 1 d .
C15 C 0.3859(3) 1.1209(3) 0.7478(3) 0.0861(15) Uani 1 1 d .
H15 H 0.3133 1.0885 0.7271 0.103 Uiso 1 1 calc R
O16 O 1.1684(3) 1.71547(17) 0.9891(2) 0.0954(11) Uani 1 1 d .
N16 N 0.8375(2) 0.90313(15) 0.72544(14) 0.0432(6) Uani 1 1 d .
C16 C 0.4195(3) 1.1607(3) 0.8175(3) 0.0885(15) Uani 1 1 d .
H16 H 0.3701 1.1550 0.8448 0.106 Uiso 1 1 calc R
N17 N 1.0581(2) 1.11225(17) 0.71877(16) 0.0533(7) Uani 1 1 d .
H17 H 1.0284 1.1413 0.7365 0.064 Uiso 1 1 calc R
C17 C 0.5267(3) 1.2098(2) 0.8486(3) 0.0719(12) Uani 1 1 d .
H17A H 0.5506 1.2369 0.8967 0.086 Uiso 1 1 calc R
N18 N 1.0219(2) 1.15978(17) 0.61726(16) 0.0542(7) Uani 1 1 d .
H18 H 0.9988 1.1879 0.6428 0.065 Uiso 1 1 calc R
C18 C 0.5970(3) 1.2177(2) 0.8067(2) 0.0564(9) Uani 1 1 d .
N19 N 1.0264(2) 1.29582(16) 0.58095(15) 0.0497(7) Uani 1 1 d .
H19 H 1.0714 1.3003 0.6231 0.060 Uiso 1 1 calc R
C19 C 0.7295(3) 1.3449(2) 0.85828(19) 0.0495(8) Uani 1 1 d .
N20 N 0.9905(3) 1.38743(17) 0.64081(16) 0.0550(8) Uani 1 1 d .
H20 H 1.0161 1.3701 0.6784 0.066 Uiso 1 1 calc R
C20 C 0.8899(3) 1.46267(18) 0.89669(17) 0.0423(7) Uani 1 1 d .
N21 N 0.9102(4) 1.6490(3) 0.7163(2) 0.0900(12) Uani 1 1 d .
C21 C 1.0018(3) 1.48982(19) 0.91369(17) 0.0442(8) Uani 1 1 d .
H21 H 1.0373 1.4555 0.9077 0.053 Uiso 1 1 calc R
C22 C 1.0611(3) 1.5651(2) 0.93894(18) 0.0503(8) Uani 1 1 d .
H22 H 1.1370 1.5830 0.9508 0.060 Uiso 1 1 calc R
C23 C 1.0081(3) 1.6140(2) 0.94662(19) 0.0551(9) Uani 1 1 d .
C24 C 0.8977(3) 1.5895(2) 0.9298(2) 0.0560(9) Uani 1 1 d .
H24 H 0.8631 1.6245 0.9351 0.067 Uiso 1 1 calc R
C25 C 0.8383(3) 1.5137(2) 0.90540(19) 0.0519(9) Uani 1 1 d .
H25 H 0.7625 1.4962 0.8945 0.062 Uiso 1 1 calc R
C26 C 0.4606(3) 0.85786(19) 0.65719(17) 0.0467(8) Uani 1 1 d .
C27 C 0.3500(3) 0.8324(2) 0.63968(19) 0.0547(9) Uani 1 1 d .
H27 H 0.3159 0.8559 0.6663 0.066 Uiso 1 1 calc R
C28 C 0.2896(3) 0.7724(2) 0.5832(2) 0.0572(10) Uani 1 1 d .
H28 H 0.2136 0.7537 0.5711 0.069 Uiso 1 1 calc R
C29 C 0.3401(3) 0.7403(2) 0.5450(2) 0.0569(9) Uani 1 1 d .
H29 H 0.2999 0.6996 0.5054 0.068 Uiso 1 1 calc R
C30 C 0.4510(3) 0.7681(2) 0.56465(19) 0.0566(9) Uani 1 1 d .
H30 H 0.4859 0.7459 0.5375 0.068 Uiso 1 1 calc R
C31 C 0.5324(3) 0.92089(19) 0.71644(18) 0.0464(8) Uani 1 1 d .
C32 C 0.4938(3) 0.9647(2) 0.7561(2) 0.0581(9) Uani 1 1 d .
H32 H 0.4193 0.9562 0.7440 0.070 Uiso 1 1 calc R
C33 C 0.5651(3) 1.0207(2) 0.8132(2) 0.0596(10) Uani 1 1 d .
H33 H 0.5395 1.0505 0.8409 0.071 Uiso 1 1 calc R
C34 C 0.6739(3) 1.03380(19) 0.83048(18) 0.0451(8) Uani 1 1 d .
C35 C 0.7064(3) 0.98965(18) 0.78615(17) 0.0417(7) Uani 1 1 d .
H35 H 0.7808 0.9989 0.7958 0.050 Uiso 1 1 calc R
C36 C 0.7530(3) 1.09035(19) 0.89540(18) 0.0484(8) Uani 1 1 d .
H36A H 0.7300 1.1339 0.9023 0.058 Uiso 1 1 calc R
H36B H 0.7526 1.0673 0.9383 0.058 Uiso 1 1 calc R
C37 C 0.9449(3) 1.11221(17) 0.94166(18) 0.0422(7) Uani 1 1 d .
C38 C 1.1431(3) 1.15825(19) 0.97456(18) 0.0449(8) Uani 1 1 d .
C39 C 1.1615(3) 1.1029(2) 1.0104(2) 0.0522(9) Uani 1 1 d .
H39 H 1.1036 1.0579 1.0067 0.063 Uiso 1 1 calc R
C40 C 1.2634(3) 1.1128(2) 1.0513(2) 0.0588(10) Uani 1 1 d .
H40 H 1.2752 1.0749 1.0764 0.071 Uiso 1 1 calc R
C41 C 1.3484(3) 1.1776(2) 1.0561(3) 0.0677(11) Uani 1 1 d .
H41 H 1.4185 1.1839 1.0842 0.081 Uiso 1 1 calc R
C42 C 1.3322(3) 1.2329(2) 1.0203(2) 0.0631(11) Uani 1 1 d .
H42 H 1.3913 1.2766 1.0227 0.076 Uiso 1 1 calc R
C43 C 1.2285(3) 1.22477(19) 0.9802(2) 0.0492(8) Uani 1 1 d .
C44 C 1.2615(3) 1.35731(19) 0.9665(2) 0.0470(8) Uani 1 1 d .
C45 C 1.2646(3) 1.47293(18) 0.91765(19) 0.0447(8) Uani 1 1 d .
C46 C 1.3349(3) 1.5269(2) 0.9775(2) 0.0533(9) Uani 1 1 d .
H46 H 1.3590 1.5122 1.0215 0.064 Uiso 1 1 calc R
C47 C 1.3695(3) 1.6018(2) 0.9730(2) 0.0577(9) Uani 1 1 d .
H47 H 1.4180 1.6388 1.0138 0.069 Uiso 1 1 calc R
C48 C 1.3341(3) 1.6228(2) 0.9101(2) 0.0567(9) Uani 1 1 d .
C49 C 1.2652(3) 1.5707(2) 0.8498(2) 0.0627(10) Uani 1 1 d .
H49 H 1.2424 1.5862 0.8060 0.075 Uiso 1 1 calc R
C50 C 1.2297(3) 1.4959(2) 0.8537(2) 0.0554(9) Uani 1 1 d .
H50 H 1.1810 1.4596 0.8127 0.066 Uiso 1 1 calc R
C51 C 0.7686(3) 0.8039(2) 0.78527(18) 0.0486(8) Uani 1 1 d .
C52 C 0.7807(3) 0.7564(2) 0.8325(2) 0.0604(10) Uani 1 1 d .
H52 H 0.8486 0.7661 0.8659 0.072 Uiso 1 1 calc R
C53 C 0.6931(4) 0.6943(2) 0.8309(2) 0.0729(12) Uani 1 1 d .
H53 H 0.7005 0.6604 0.8622 0.088 Uiso 1 1 calc R
C54 C 0.5950(4) 0.6827(2) 0.7830(2) 0.0761(13) Uani 1 1 d .
H54 H 0.5331 0.6417 0.7819 0.091 Uiso 1 1 calc R
C55 C 0.5887(3) 0.7315(2) 0.7367(2) 0.0663(11) Uani 1 1 d .
H55 H 0.5212 0.7226 0.7032 0.080 Uiso 1 1 calc R
C56 C 0.8566(3) 0.87156(19) 0.78387(17) 0.0446(8) Uani 1 1 d .
C57 C 0.9510(3) 0.9037(2) 0.83862(19) 0.0512(8) Uani 1 1 d .
H57 H 0.9627 0.8818 0.8798 0.061 Uiso 1 1 calc R
C58 C 1.0285(3) 0.9679(2) 0.83343(19) 0.0513(9) Uani 1 1 d .
H58 H 1.0930 0.9912 0.8717 0.062 Uiso 1 1 calc R
C59 C 1.0124(3) 0.99847(19) 0.77251(18) 0.0450(8) Uani 1 1 d .
C60 C 0.9146(3) 0.96446(19) 0.72011(18) 0.0445(8) Uani 1 1 d .
H60 H 0.9015 0.9855 0.6785 0.053 Uiso 1 1 calc R
C61 C 1.0986(3) 1.0655(2) 0.7630(2) 0.0519(9) Uani 1 1 d .
H61A H 1.1427 1.0968 0.8109 0.062 Uiso 1 1 calc R
H61B H 1.1459 1.0474 0.7410 0.062 Uiso 1 1 calc R
C62 C 1.0650(3) 1.1123(2) 0.6510(2) 0.0515(9) Uani 1 1 d .
C63 C 1.0117(3) 1.1673(2) 0.54531(19) 0.0517(9) Uani 1 1 d .
C64 C 0.9978(3) 1.1071(2) 0.4916(2) 0.0607(10) Uani 1 1 d .
H64 H 0.9968 1.0603 0.5040 0.073 Uiso 1 1 calc R
C65 C 0.9857(3) 1.1148(3) 0.4222(2) 0.0709(12) Uani 1 1 d .
H65 H 0.9757 1.0733 0.3866 0.085 Uiso 1 1 calc R
C66 C 0.9878(4) 1.1820(3) 0.4036(2) 0.0756(13) Uani 1 1 d .
H66 H 0.9807 1.1873 0.3551 0.091 Uiso 1 1 calc R
C67 C 1.0004(3) 1.2429(3) 0.4550(2) 0.0636(10) Uani 1 1 d .
H67 H 1.0012 1.2893 0.4416 0.076 Uiso 1 1 calc R
C68 C 1.0119(3) 1.2354(2) 0.52621(18) 0.0513(9) Uani 1 1 d .
C69 C 0.9782(3) 1.3470(2) 0.57496(19) 0.0513(9) Uani 1 1 d .
C70 C 0.9677(3) 1.4521(2) 0.6558(2) 0.0582(9) Uani 1 1 d .
C71 C 0.9693(4) 1.4754(3) 0.7254(2) 0.0699(12) Uani 1 1 d .
H71 H 0.9825 1.4458 0.7602 0.084 Uiso 1 1 calc R
C72 C 0.9523(4) 1.5402(3) 0.7451(2) 0.0722(12) Uani 1 1 d .
H72 H 0.9549 1.5559 0.7934 0.087 Uiso 1 1 calc R
C73 C 0.9317(4) 1.5816(3) 0.6955(2) 0.0691(11) Uani 1 1 d .
C74 C 0.9259(5) 1.5590(3) 0.6253(3) 0.0893(16) Uani 1 1 d .
H74 H 0.9087 1.5875 0.5904 0.107 Uiso 1 1 calc R
C75 C 0.9453(5) 1.4946(3) 0.6059(2) 0.0852(15) Uani 1 1 d .
H75 H 0.9432 1.4794 0.5576 0.102 Uiso 1 1 calc R
O1S O 0.5608(5) 1.0017(3) 1.0699(3) 0.1412(18) Uani 1 1 d .
N1S N 1.3648(3) 1.3819(2) 0.79498(19) 0.0746(10) Uani 1 1 d .
C1S C 0.5028(7) 0.9330(4) 1.0166(4) 0.137(3) Uani 1 1 d .
H1S1 H 0.5413 0.8976 1.0247 0.165 Uiso 1 1 calc R
H1S2 H 0.4311 0.9094 1.0228 0.165 Uiso 1 1 calc R
O2S O 1.3656(4) 1.5861(3) 0.6625(3) 0.161(2) Uani 1 1 d .
N2S N 0.2032(5) 0.8606(4) 0.8280(5) 0.143(3) Uani 1 1 d .
C2S C 0.5097(7) 1.0560(4) 1.0534(4) 0.138(3) Uani 1 1 d .
H2S1 H 0.4385 1.0384 1.0615 0.166 Uiso 1 1 calc R
H2S2 H 0.5532 1.1047 1.0868 0.166 Uiso 1 1 calc R
O3S O 1.2679(4) 1.4773(3) 0.5355(3) 0.1391(17) Uani 1 1 d .
C3S C 1.3786(6) 1.4995(5) 0.5735(5) 0.177(4) Uani 1 1 d .
H3S1 H 1.3880 1.4631 0.6046 0.213 Uiso 1 1 calc R
H3S2 H 1.4189 1.4970 0.5384 0.213 Uiso 1 1 calc R
O4S O 1.2191(3) 1.3495(2) 0.69891(19) 0.1009(12) Uani 1 1 d .
C4S C 1.4207(7) 1.5687(5) 0.6141(6) 0.182(4) Uani 1 1 d .
H4S1 H 1.4254 1.6052 0.5817 0.218 Uiso 1 1 calc R
H4S2 H 1.4948 1.5768 0.6424 0.218 Uiso 1 1 calc R
O5S O 0.2369(3) 0.9221(2) 0.7405(2) 0.0972(11) Uani 1 1 d .
C5S C 1.2529(7) 1.5675(5) 0.6244(5) 0.165(4) Uani 1 1 d .
H5S1 H 1.2124 1.5709 0.6592 0.198 Uiso 1 1 calc R
H5S2 H 1.2452 1.6034 0.5924 0.198 Uiso 1 1 calc R
C6S C 1.2115(6) 1.4923(5) 0.5827(4) 0.136(3) Uani 1 1 d .
H6S1 H 1.2101 1.4569 0.6162 0.163 Uiso 1 1 calc R
H6S2 H 1.1365 1.4814 0.5542 0.163 Uiso 1 1 calc R
C7S C 1.2691(5) 1.3386(4) 0.7526(3) 0.108(2) Uani 1 1 d .
H7S H 1.2361 1.2931 0.7668 0.130 Uiso 1 1 calc R
C8S C 1.4143(5) 1.3594(5) 0.8569(4) 0.143(3) Uani 1 1 d .
H8S1 H 1.4844 1.3983 0.8819 0.214 Uiso 1 1 calc R
H8S2 H 1.4235 1.3119 0.8425 0.214 Uiso 1 1 calc R
H8S3 H 1.3690 1.3525 0.8891 0.214 Uiso 1 1 calc R
C9S C 1.4218(7) 1.4551(5) 0.7881(6) 0.183(4) Uani 1 1 d .
H9S1 H 1.4906 1.4758 0.8259 0.274 Uiso 1 1 calc R
H9S2 H 1.3799 1.4873 0.7926 0.274 Uiso 1 1 calc R
H9S3 H 1.4344 1.4532 0.7410 0.274 Uiso 1 1 calc R
C10S C 0.2278(5) 0.9127(5) 0.7980(4) 0.117(2) Uani 1 1 d .
H10S H 0.2447 0.9592 0.8290 0.140 Uiso 1 1 calc R
C11S C 0.1656(10) 0.7847(6) 0.7766(7) 0.276(10) Uani 1 1 d .
H11C H 0.1379 0.7904 0.7273 0.413 Uiso 1 1 calc R
H11D H 0.1089 0.7476 0.7897 0.413 Uiso 1 1 calc R
H11E H 0.2260 0.7675 0.7801 0.413 Uiso 1 1 calc R
C12S C 0.1941(8) 0.8532(7) 0.8974(5) 0.193(5) Uani 1 1 d .
H12A H 0.2475 0.8972 0.9327 0.289 Uiso 1 1 calc R
H12B H 0.2063 0.8075 0.9090 0.289 Uiso 1 1 calc R
H12C H 0.1221 0.8497 0.8987 0.289 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 0.0033 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'
S S 0.1246 0.1234 '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
N2 Ni1 N8 92.63(11) .
N2 Ni1 N1 78.47(12) .
N8 Ni1 N1 95.70(11) .
N2 Ni1 N16 95.39(11) .
N8 Ni1 N16 168.62(11) .
N1 Ni1 N16 93.81(11) .
N2 Ni1 N15 171.44(12) .
N8 Ni1 N15 94.03(11) .
N1 Ni1 N15 95.52(12) .
N16 Ni1 N15 78.82(11) .
N2 Ni1 N9 96.97(11) .
N8 Ni1 N9 78.38(11) .
N1 Ni1 N9 172.44(11) .
N16 Ni1 N9 92.61(10) .
N15 Ni1 N9 89.64(11) .
O4 S1 O3 111.70(18) .
O4 S1 O2 109.9(2) .
O3 S1 O2 108.06(17) .
O4 S1 O1 109.62(15) .
O3 S1 O1 109.37(14) .
O2 S1 O1 108.06(15) .
C5 N1 C1 118.2(3) .
C5 N1 Ni1 126.2(3) .
C1 N1 Ni1 115.6(2) .
N1 C1 C2 123.0(4) .
N1 C1 C6 115.3(3) .
C2 C1 C6 121.7(4) .
C10 N2 C6 118.0(3) .
C10 N2 Ni1 126.7(2) .
C6 N2 Ni1 115.3(2) .
C3 C2 C1 117.7(4) .
C12 N3 C11 120.6(3) .
C4 C3 C2 120.0(4) .
C12 N4 C13 129.0(3) .
C3 C4 C5 118.4(4) .
C19 N5 C18 123.2(3) .
N1 C5 C4 122.7(4) .
C19 N6 C20 127.4(3) .
N2 C6 C7 121.1(3) .
N2 C6 C1 115.2(3) .
C7 C6 C1 123.7(3) .
O16 N7 O15 124.4(4) .
O16 N7 C23 118.4(4) .
O15 N7 C23 117.3(4) .
C8 C7 C6 120.0(3) .
C30 N8 C26 118.0(3) .
C30 N8 Ni1 126.3(3) .
C26 N8 Ni1 115.4(2) .
C7 C8 C9 119.3(3) .
C31 N9 C35 118.8(3) .
C31 N9 Ni1 114.6(2) .
C35 N9 Ni1 126.5(2) .
C10 C9 C8 117.8(4) .
C10 C9 C11 122.9(3) .
C8 C9 C11 119.3(3) .
C37 N10 C36 121.6(3) .
N2 C10 C9 123.8(3) .
C37 N11 C38 126.2(3) .
N3 C11 C9 114.8(3) .
C44 N12 C43 125.8(3) .
O13 C12 N3 123.4(4) .
O13 C12 N4 123.1(4) .
N3 C12 N4 113.4(3) .
C44 N13 C45 127.5(3) .
C18 C13 C14 119.2(4) .
C18 C13 N4 118.2(3) .
C14 C13 N4 122.5(4) .
O8 N14 O7 122.6(4) .
O8 N14 C48 119.8(4) .
O7 N14 C48 117.6(4) .
C15 C14 C13 120.7(5) .
C55 N15 C51 117.9(3) .
C55 N15 Ni1 127.2(3) .
C51 N15 Ni1 114.7(2) .
C14 C15 C16 120.4(4) .
C60 N16 C56 118.8(3) .
C60 N16 Ni1 125.6(2) .
C56 N16 Ni1 114.3(2) .
C15 C16 C17 120.4(4) .
C62 N17 C61 121.8(3) .
C18 C17 C16 118.3(4) .
C62 N18 C63 125.7(3) .
C13 C18 C17 120.9(4) .
C13 C18 N5 119.9(3) .
C17 C18 N5 119.2(4) .
C69 N19 C68 126.6(3) .
O14 C19 N5 123.6(3) .
O14 C19 N6 124.1(3) .
N5 C19 N6 112.3(3) .
C69 N20 C70 128.4(3) .
N6 C20 C25 124.1(3) .
N6 C20 C21 117.0(3) .
C25 C20 C21 118.9(3) .
O11 N21 O12 121.3(4) .
O11 N21 C73 120.3(4) .
O12 N21 C73 118.4(4) .
C22 C21 C20 121.2(3) .
C21 C22 C23 118.5(3) .
C22 C23 C24 122.0(3) .
C22 C23 N7 119.1(4) .
C24 C23 N7 118.9(4) .
C23 C24 C25 119.4(3) .
C24 C25 C20 119.9(3) .
N8 C26 C27 121.5(3) .
N8 C26 C31 114.6(3) .
C27 C26 C31 123.9(3) .
C28 C27 C26 119.4(4) .
C29 C28 C27 119.3(3) .
C28 C29 C30 118.9(4) .
N8 C30 C29 122.8(4) .
N9 C31 C32 121.2(3) .
N9 C31 C26 116.6(3) .
C32 C31 C26 122.1(3) .
C33 C32 C31 119.1(3) .
C32 C33 C34 120.6(3) .
C33 C34 C35 116.7(3) .
C33 C34 C36 122.0(3) .
C35 C34 C36 121.2(3) .
N9 C35 C34 123.4(3) .
N10 C36 C34 113.2(3) .
O5 C37 N11 125.2(3) .
O5 C37 N10 123.4(3) .
N11 C37 N10 111.4(3) .
C39 C38 C43 119.8(3) .
C39 C38 N11 122.0(3) .
C43 C38 N11 118.1(3) .
C40 C39 C38 120.3(3) .
C39 C40 C41 120.3(3) .
C42 C41 C40 120.4(4) .
C41 C42 C43 120.1(3) .
C38 C43 C42 119.1(3) .
C38 C43 N12 119.6(3) .
C42 C43 N12 121.2(3) .
O6 C44 N12 125.4(3) .
O6 C44 N13 123.9(3) .
N12 C44 N13 110.7(3) .
C46 C45 C50 119.0(3) .
C46 C45 N13 124.3(3) .
C50 C45 N13 116.6(3) .
C47 C46 C45 119.9(3) .
C48 C47 C46 119.9(4) .
C47 C48 C49 121.5(3) .
C47 C48 N14 118.8(4) .
C49 C48 N14 119.6(4) .
C50 C49 C48 119.1(4) .
C49 C50 C45 120.5(4) .
N15 C51 C52 121.4(3) .
N15 C51 C56 115.2(3) .
C52 C51 C56 123.3(3) .
C51 C52 C53 119.6(4) .
C54 C53 C52 118.8(4) .
C55 C54 C53 118.7(4) .
N15 C55 C54 123.5(4) .
N16 C56 C57 121.0(3) .
N16 C56 C51 115.5(3) .
C57 C56 C51 123.4(3) .
C56 C57 C58 119.6(3) .
C57 C58 C59 120.0(3) .
C60 C59 C58 117.4(3) .
C60 C59 C61 121.2(3) .
C58 C59 C61 121.3(3) .
N16 C60 C59 123.0(3) .
N17 C61 C59 114.1(3) .
O9 C62 N17 122.9(3) .
O9 C62 N18 123.5(3) .
N17 C62 N18 113.6(3) .
C68 C63 C64 118.8(3) .
C68 C63 N18 119.2(3) .
C64 C63 N18 121.9(3) .
C65 C64 C63 121.2(4) .
C64 C65 C66 120.1(4) .
C65 C66 C67 120.6(4) .
C68 C67 C66 119.7(4) .
C67 C68 C63 119.5(4) .
C67 C68 N19 122.1(4) .
C63 C68 N19 118.4(3) .
O10 C69 N19 124.8(4) .
O10 C69 N20 123.2(4) .
N19 C69 N20 112.1(3) .
C75 C70 C71 118.3(4) .
C75 C70 N20 124.0(4) .
C71 C70 N20 117.7(3) .
C72 C71 C70 121.2(4) .
C73 C72 C71 119.5(4) .
C72 C73 C74 120.9(4) .
C72 C73 N21 119.3(4) .
C74 C73 N21 119.8(4) .
C73 C74 C75 119.4(4) .
C70 C75 C74 120.6(4) .
C1S O1S C2S 108.5(6) .
C7S N1S C9S 124.8(6) .
C7S N1S C8S 120.7(6) .
C9S N1S C8S 114.3(6) .
C2S C1S O1S 113.4(6) 2_677
C4S O2S C5S 110.1(7) .
C10S N2S C12S 135.2(10) .
C10S N2S C11S 111.7(9) .
C12S N2S C11S 113.0(8) .
C1S C2S O1S 113.3(6) 2_677
C6S O3S C3S 109.8(6) .
C4S C3S O3S 113.9(8) .
C3S C4S O2S 117.1(9) .
C6S C5S O2S 108.7(8) .
O3S C6S C5S 116.1(7) .
O4S C7S N1S 128.1(7) .
O5S C10S N2S 137.9(9) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N2 2.079(3) .
Ni1 N8 2.083(3) .
Ni1 N1 2.084(3) .
Ni1 N16 2.088(3) .
Ni1 N15 2.090(3) .
Ni1 N9 2.093(3) .
S1 O4 1.447(3) .
S1 O3 1.450(2) .
S1 O2 1.474(3) .
S1 O1 1.487(2) .
N1 C5 1.331(5) .
N1 C1 1.343(5) .
C1 C2 1.389(5) .
C1 C6 1.480(5) .
N2 C10 1.342(5) .
N2 C6 1.355(4) .
C2 C3 1.383(6) .
N3 C12 1.337(5) .
N3 C11 1.445(5) .
C3 C4 1.378(7) .
N4 C12 1.377(5) .
N4 C13 1.401(5) .
C4 C5 1.389(6) .
O5 C37 1.214(4) .
N5 C19 1.360(5) .
N5 C18 1.429(4) .
O6 C44 1.212(4) .
N6 C19 1.374(4) .
N6 C20 1.398(4) .
C6 C7 1.389(5) .
O7 N14 1.231(5) .
N7 O16 1.227(5) .
N7 O15 1.234(5) .
N7 C23 1.466(5) .
C7 C8 1.371(6) .
O8 N14 1.216(5) .
N8 C30 1.341(4) .
N8 C26 1.354(5) .
C8 C9 1.389(5) .
O9 C62 1.227(4) .
N9 C31 1.342(4) .
N9 C35 1.345(4) .
C9 C10 1.377(5) .
C9 C11 1.505(6) .
O10 C69 1.222(4) .
N10 C37 1.376(4) .
N10 C36 1.439(4) .
O11 N21 1.204(5) .
N11 C37 1.373(4) .
N11 C38 1.406(4) .
O12 N21 1.220(5) .
N12 C44 1.370(4) .
N12 C43 1.421(4) .
C12 O13 1.221(5) .
N13 C44 1.382(4) .
N13 C45 1.397(4) .
C13 C18 1.388(6) .
C13 C14 1.395(5) .
O14 C19 1.225(4) .
N14 C48 1.459(5) .
C14 C15 1.369(7) .
N15 C55 1.339(5) .
N15 C51 1.360(4) .
C15 C16 1.381(7) .
N16 C60 1.341(4) .
N16 C56 1.358(4) .
C16 C17 1.411(6) .
N17 C62 1.353(5) .
N17 C61 1.451(5) .
C17 C18 1.398(6) .
N18 C62 1.376(5) .
N18 C63 1.409(5) .
N19 C69 1.348(5) .
N19 C68 1.419(5) .
N20 C69 1.375(5) .
N20 C70 1.390(5) .
C20 C25 1.399(5) .
C20 C21 1.399(5) .
N21 C73 1.452(6) .
C21 C22 1.374(5) .
C22 C23 1.376(5) .
C23 C24 1.382(5) .
C24 C25 1.381(5) .
C26 C27 1.385(5) .
C26 C31 1.471(5) .
C27 C28 1.381(5) .
C28 C29 1.362(6) .
C29 C30 1.386(5) .
C31 C32 1.395(5) .
C32 C33 1.378(5) .
C33 C34 1.386(5) .
C34 C35 1.396(5) .
C34 C36 1.502(5) .
C38 C39 1.385(5) .
C38 C43 1.402(5) .
C39 C40 1.379(5) .
C40 C41 1.383(6) .
C41 C42 1.376(5) .
C42 C43 1.404(5) .
C45 C46 1.390(5) .
C45 C50 1.396(5) .
C46 C47 1.377(5) .
C47 C48 1.362(5) .
C48 C49 1.375(6) .
C49 C50 1.372(5) .
C51 C52 1.381(5) .
C51 C56 1.472(5) .
C52 C53 1.388(6) .
C53 C54 1.379(6) .
C54 C55 1.375(6) .
C56 C57 1.375(5) .
C57 C58 1.378(5) .
C58 C59 1.384(5) .
C59 C60 1.385(5) .
C59 C61 1.509(5) .
C63 C68 1.393(5) .
C63 C64 1.406(5) .
C64 C65 1.356(6) .
C65 C66 1.368(7) .
C66 C67 1.393(6) .
C67 C68 1.392(5) .
C70 C75 1.376(5) .
C70 C71 1.382(6) .
C71 C72 1.369(6) .
C72 C73 1.350(6) .
C73 C74 1.374(6) .
C74 C75 1.376(7) .
O1S C1S 1.447(8) .
O1S C2S 1.451(7) .
N1S C7S 1.318(7) .
N1S C9S 1.409(8) .
N1S C8S 1.420(7) .
C1S C2S 1.386(9) 2_677
O2S C4S 1.426(10) .
O2S C5S 1.457(9) .
N2S C10S 1.207(8) .
N2S C12S 1.413(10) .
N2S C11S 1.533(13) .
C2S C1S 1.386(9) 2_677
O3S C6S 1.407(8) .
O3S C3S 1.425(9) .
C3S C4S 1.336(10) .
O4S C7S 1.187(6) .
O5S C10S 1.188(7) .
C5S C6S 1.437(10) .
