#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/65/7006574.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_7006574
loop_
_publ_author_name
'Christensen, Aase'
'Mayer, Christoph'
'Jensen, Frank'
'Bond, Andrew D.'
'McKenzie, Christine J.'
_publ_section_title
;
 Controlled formation and topologies of thiophenolate-based
 macrocycles: rings, cylinders and bowls.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              108
_journal_page_last               120
_journal_paper_doi               10.1039/b512068c
_journal_year                    2006
_chemical_formula_moiety
;
C30 H38 N4 Ni2 S2 2+, 2(Cl O4 -), 0.5(C3 H7 N O), 0.5(C H4 O)
;
_chemical_formula_sum            'C32 H43.5 Cl2 N4.5 Ni2 O9 S2'
_chemical_formula_weight         887.65
_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
_cell_angle_alpha                102.565(4)
_cell_angle_beta                 100.972(4)
_cell_angle_gamma                117.638(4)
_cell_formula_units_Z            2
_cell_length_a                   12.373(2)
_cell_length_b                   13.331(2)
_cell_length_c                   15.212(3)
_cell_measurement_reflns_used    5140
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.64
_cell_measurement_theta_min      2.72
_cell_volume                     2042.8(6)
_computing_cell_refinement       'SAINT v.7.06a (Bruker, 2003)'
_computing_data_collection       'APEX2 v.1.0-8 (Bruker-Nonius, 2003)'
_computing_data_reduction        'SAINT v.7.06a (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL v.6.10 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL v.6.10 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXTL v.6.10 (Sheldrick, 2000)'
_computing_structure_solution    'SHELXTL v.6.10 (Sheldrick, 2000)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker-Nonius X8APEX-II CCD'
_diffrn_measurement_method       'thin-slice ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17012
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.208
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Sheldrick, 2003)
Ratio of minimum to maximum apparent transmission: 0.551574
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             922
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.100
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         7118
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0760
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1443P)²+4.8208P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2101
_refine_ls_wR_factor_ref         0.2342
_reflns_number_gt                5053
_reflns_number_total             7118
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b512068c.txt
_cod_data_source_block           3
_cod_original_formula_sum        'C32 H43.50 Cl2 N4.50 Ni2 O9 S2'
_cod_database_code               7006574
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.17951(7) 0.22336(7) 0.32763(5) 0.0308(3) Uani 1 1 d . . .
Ni2 Ni 0.32304(7) 0.23571(7) 0.17527(5) 0.0306(3) Uani 1 1 d . . .
S1 S 0.35519(14) 0.35579(14) 0.31152(11) 0.0323(4) Uani 1 1 d . . .
S2 S 0.12605(14) 0.16129(14) 0.17393(11) 0.0312(4) Uani 1 1 d . . .
N1 N 0.2498(5) 0.2993(5) 0.4642(4) 0.0355(12) Uani 1 1 d . . .
N2 N 0.0146(5) 0.0941(5) 0.3222(4) 0.0339(12) Uani 1 1 d . . .
N3 N 0.2703(5) 0.1202(5) 0.0524(3) 0.0310(11) Uani 1 1 d . . .
N4 N 0.5061(5) 0.3187(5) 0.1943(4) 0.0338(12) Uani 1 1 d . . .
C1 C 0.4772(6) 0.3522(6) 0.3912(4) 0.0327(14) Uani 1 1 d . . .
C2 C 0.5827(6) 0.3602(6) 0.3663(4) 0.0345(14) Uani 1 1 d . . .
C3 C 0.6843(6) 0.3687(6) 0.4337(5) 0.0384(15) Uani 1 1 d . . .
H3A H 0.7563 0.3746 0.4164 0.046 Uiso 1 1 calc R . .
C4 C 0.6828(6) 0.3686(6) 0.5255(5) 0.0401(15) Uani 1 1 d . . .
C5 C 0.5762(6) 0.3613(6) 0.5476(5) 0.0368(15) Uani 1 1 d . . .
H5A H 0.5732 0.3622 0.6097 0.044 Uiso 1 1 calc R . .
C6 C 0.4733(6) 0.3526(6) 0.4827(4) 0.0365(15) Uani 1 1 d . . .
C7 C 0.3680(6) 0.3461(6) 0.5164(5) 0.0352(14) Uani 1 1 d . . .
H7A H 0.3889 0.3798 0.5835 0.042 Uiso 1 1 calc R . .
C8 C 0.1626(6) 0.3061(6) 0.5161(5) 0.0417(16) Uani 1 1 d . . .
H8A H 0.1332 0.3585 0.4980 0.050 Uiso 1 1 calc R . .
H8B H 0.2105 0.3427 0.5858 0.050 Uiso 1 1 calc R . .
C9 C 0.0456(6) 0.1810(6) 0.4933(5) 0.0402(16) Uani 1 1 d . . .
H9A H 0.0761 0.1270 0.5055 0.048 Uiso 1 1 calc R . .
H9B H -0.0027 0.1869 0.5371 0.048 Uiso 1 1 calc R . .
C10 C -0.0445(6) 0.1254(7) 0.3927(5) 0.0437(17) Uani 1 1 d . . .
H10J H -0.0688 0.1826 0.3780 0.052 Uiso 1 1 calc R . .
H10K H -0.1246 0.0512 0.3860 0.052 Uiso 1 1 calc R . .
C11 C 0.7905(7) 0.3759(8) 0.5992(5) 0.0496(18) Uani 1 1 d . . .
C12 C 0.8435(11) 0.4838(13) 0.6864(7) 0.107(5) Uani 1 1 d . . .
H12A H 0.7731 0.4788 0.7095 0.161 Uiso 1 1 calc R . .
H12B H 0.8837 0.5573 0.6707 0.161 Uiso 1 1 calc R . .
H12C H 0.9087 0.4860 0.7362 0.161 Uiso 1 1 calc R . .
C13 C 0.8987(11) 0.3837(16) 0.5636(7) 0.126(6) Uani 1 1 d . . .
H13A H 0.9348 0.4543 0.5438 0.189 Uiso 1 1 calc R . .
H13B H 0.8651 0.3102 0.5088 0.189 Uiso 1 1 calc R . .
H13C H 0.9668 0.3916 0.6148 0.189 Uiso 1 1 calc R . .
C14 C 0.7339(12) 0.2663(13) 0.6302(11) 0.132(6) Uani 1 1 d . . .
H14A H 0.6634 0.2616 0.6530 0.197 Uiso 1 1 calc R . .
H14B H 0.8017 0.2744 0.6818 0.197 Uiso 1 1 calc R . .
H14C H 0.7003 0.1926 0.5757 0.197 Uiso 1 1 calc R . .
C15 C -0.0520(6) -0.0119(6) 0.2623(5) 0.0359(15) Uani 1 1 d . . .
H15A H -0.1317 -0.0642 0.2693 0.043 Uiso 1 1 calc R . .
C16 C 0.0641(5) 0.0052(6) 0.1407(4) 0.0324(14) Uani 1 1 d . . .
C17 C -0.0211(6) -0.0636(6) 0.1836(4) 0.0324(14) Uani 1 1 d . . .
C18 C -0.0829(6) -0.1887(6) 0.1475(5) 0.0382(15) Uani 1 1 d . . .
H18A H -0.1407 -0.2344 0.1761 0.046 Uiso 1 1 calc R . .
C19 C -0.0640(6) -0.2513(6) 0.0698(5) 0.0364(14) Uani 1 1 d . . .
C20 C 0.0238(6) -0.1792(6) 0.0330(5) 0.0363(15) Uani 1 1 d . . .
H20A H 0.0402 -0.2176 -0.0186 0.044 Uiso 1 1 calc R . .
C21 C 0.0892(6) -0.0537(6) 0.0674(4) 0.0308(13) Uani 1 1 d . . .
C22 C 0.1779(6) 0.0092(6) 0.0192(4) 0.0334(14) Uani 1 1 d . . .
H22A H 0.1653 -0.0374 -0.0429 0.040 Uiso 1 1 calc R . .
C23 C 0.3384(6) 0.1615(6) -0.0154(4) 0.0364(15) Uani 1 1 d . . .
H23A H 0.3184 0.2190 -0.0347 0.044 Uiso 1 1 calc R . .
H23B H 0.3059 0.0911 -0.0737 0.044 Uiso 1 1 calc R . .
C24 C 0.4836(6) 0.2222(6) 0.0285(5) 0.0396(16) Uani 1 1 d . . .
H24A H 0.5025 0.1657 0.0508 0.047 Uiso 1 1 calc R . .
H24B H 0.5231 0.2383 -0.0216 0.047 Uiso 1 1 calc R . .
C25 C 0.5457(6) 0.3381(7) 0.1105(5) 0.0429(17) Uani 1 1 d . . .
H25A H 0.6410 0.3781 0.1291 0.051 Uiso 1 1 calc R . .
H25B H 0.5214 0.3927 0.0901 0.051 Uiso 1 1 calc R . .
C26 C -0.1367(7) -0.3878(6) 0.0330(5) 0.0418(16) Uani 1 1 d . . .
C27 C -0.1074(8) -0.4308(8) 0.1137(6) 0.059(2) Uani 1 1 d . . .
H27A H -0.0144 -0.4000 0.1370 0.089 Uiso 1 1 calc R . .
H27B H -0.1563 -0.5194 0.0903 0.089 Uiso 1 1 calc R . .
H27C H -0.1325 -0.4008 0.1660 0.089 Uiso 1 1 calc R . .
C28 C -0.1016(9) -0.4368(7) -0.0508(6) 0.061(2) Uani 1 1 d . . .
H28A H -0.0086 -0.4063 -0.0296 0.091 Uiso 1 1 calc R . .
H28B H -0.1229 -0.4100 -0.1030 0.091 Uiso 1 1 calc R . .
H28C H -0.1507 -0.5254 -0.0732 0.091 Uiso 1 1 calc R . .
C29 C -0.2850(7) -0.4378(7) -0.0033(6) 0.058(2) Uani 1 1 d . . .
H29A H -0.3097 -0.4077 0.0492 0.087 Uiso 1 1 calc R . .
H29B H -0.3333 -0.5264 -0.0264 0.087 Uiso 1 1 calc R . .
H29C H -0.3050 -0.4106 -0.0556 0.087 Uiso 1 1 calc R . .
C30 C 0.5961(6) 0.3609(6) 0.2731(5) 0.0371(15) Uani 1 1 d . . .
H30A H 0.6819 0.3970 0.2712 0.045 Uiso 1 1 calc R . .
Cl1 Cl 0.3894(2) 0.30920(19) 0.75431(14) 0.0616(6) Uani 1 1 d D . .
O1A O 0.3873(6) 0.2802(7) 0.8368(4) 0.087(2) Uani 1 1 d D . .
O1B O 0.3421(13) 0.3866(10) 0.7526(7) 0.195(7) Uani 1 1 d D . .
O1C O 0.5141(6) 0.3646(9) 0.7512(5) 0.166(6) Uani 1 1 d D . .
O1D O 0.3048(6) 0.2072(5) 0.6720(4) 0.085(2) Uani 1 1 d D . .
Cl2 Cl 0.7901(2) 0.2163(2) 0.18813(16) 0.0635(6) Uani 1 1 d D . .
O2A O 0.6654(7) 0.1130(7) 0.1355(8) 0.179(6) Uani 1 1 d D . .
O2B O 0.8089(9) 0.2995(10) 0.1425(10) 0.197(6) Uani 1 1 d D . .
O2C O 0.8798(8) 0.1829(9) 0.1929(5) 0.148(5) Uani 1 1 d D . .
O2D O 0.7955(11) 0.2646(11) 0.2807(6) 0.176(5) Uani 1 1 d D . .
O100 O 0.2524(16) 0.0736(15) 0.3613(12) 0.108(5) Uiso 0.50 1 d PD . .
H100 H 0.2893 0.0565 0.3240 0.162 Uiso 0.50 1 d PR . .
C100 C 0.252(2) 0.030(2) 0.4383(15) 0.105(8) Uiso 0.50 1 d PD . .
H10A H 0.3326 0.0323 0.4638 0.157 Uiso 0.50 1 d PR . .
H10B H 0.1785 -0.0537 0.4156 0.157 Uiso 0.50 1 d PR . .
H10C H 0.2415 0.0806 0.4889 0.157 Uiso 0.50 1 d PR . .
O101 O 0.3593(12) 0.0697(11) 0.2467(9) 0.073(3) Uiso 0.50 1 d PD . .
N101 N 0.4462(14) -0.0473(13) 0.2389(10) 0.065(4) Uiso 0.50 1 d PD . .
C101 C 0.440(2) 0.043(2) 0.2708(19) 0.112(8) Uiso 0.50 1 d PD . .
H101 H 0.5131 0.1037 0.3253 0.134 Uiso 0.50 1 calc PR . .
C102 C 0.338(2) -0.146(2) 0.1595(15) 0.106(8) Uiso 0.50 1 d PD . .
H10D H 0.3568 -0.2091 0.1379 0.159 Uiso 0.50 1 calc PR . .
H10E H 0.3216 -0.1176 0.1072 0.159 Uiso 0.50 1 calc PR . .
H10F H 0.2612 -0.1792 0.1791 0.159 Uiso 0.50 1 calc PR . .
C103 C 0.562(3) -0.040(3) 0.288(2) 0.132(10) Uiso 0.50 1 d P . .
H10G H 0.5603 -0.1133 0.2553 0.198 Uiso 0.50 1 calc PR . .
H10H H 0.5667 -0.0340 0.3539 0.198 Uiso 0.50 1 calc PR . .
H10I H 0.6375 0.0310 0.2873 0.198 Uiso 0.50 1 calc PR . .
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'
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'
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'
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 Ni1 N2 96.5(2) . . ?
N1 Ni1 S2 171.32(16) . . ?
N2 Ni1 S2 92.09(16) . . ?
N1 Ni1 S1 91.73(16) . . ?
N2 Ni1 S1 171.73(17) . . ?
S2 Ni1 S1 79.68(6) . . ?
N3 Ni2 N4 95.9(2) . . ?
N3 Ni2 S2 92.29(16) . . ?
N4 Ni2 S2 171.76(16) . . ?
N3 Ni2 S1 172.26(16) . . ?
N4 Ni2 S1 91.78(16) . . ?
S2 Ni2 S1 79.98(6) . . ?
C1 S1 Ni2 102.6(2) . . ?
C1 S1 Ni1 102.2(2) . . ?
Ni2 S1 Ni1 93.74(7) . . ?
C16 S2 Ni1 104.1(2) . . ?
C16 S2 Ni2 103.4(2) . . ?
Ni1 S2 Ni2 94.37(6) . . ?
C7 N1 C8 115.7(5) . . ?
C7 N1 Ni1 126.0(4) . . ?
C8 N1 Ni1 118.4(4) . . ?
C15 N2 C10 116.2(5) . . ?
C15 N2 Ni1 126.9(4) . . ?
C10 N2 Ni1 116.8(4) . . ?
C22 N3 C23 114.9(5) . . ?
C22 N3 Ni2 126.8(4) . . ?
C23 N3 Ni2 118.3(4) . . ?
C30 N4 C25 116.9(5) . . ?
C30 N4 Ni2 125.6(4) . . ?
C25 N4 Ni2 117.4(4) . . ?
C2 C1 C6 119.9(6) . . ?
C2 C1 S1 120.1(5) . . ?
C6 C1 S1 119.7(5) . . ?
C1 C2 C3 119.4(6) . . ?
C1 C2 C30 124.1(6) . . ?
C3 C2 C30 116.6(6) . . ?
C4 C3 C2 122.1(6) . . ?
C4 C3 H3A 119.0 . . ?
C2 C3 H3A 119.0 . . ?
C5 C4 C3 116.8(6) . . ?
C5 C4 C11 120.1(6) . . ?
C3 C4 C11 123.1(6) . . ?
C4 C5 C6 122.8(6) . . ?
C4 C5 H5A 118.6 . . ?
C6 C5 H5A 118.6 . . ?
C5 C6 C1 119.1(6) . . ?
C5 C6 C7 116.7(6) . . ?
C1 C6 C7 124.3(6) . . ?
N1 C7 C6 126.4(6) . . ?
N1 C7 H7A 116.8 . . ?
C6 C7 H7A 116.8 . . ?
N1 C8 C9 111.0(5) . . ?
N1 C8 H8A 109.4 . . ?
C9 C8 H8A 109.4 . . ?
N1 C8 H8B 109.4 . . ?
C9 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
C10 C9 C8 113.8(6) . . ?
C10 C9 H9A 108.8 . . ?
C8 C9 H9A 108.8 . . ?
C10 C9 H9B 108.8 . . ?
C8 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 N2 112.2(5) . . ?
C9 C10 H10J 109.2 . . ?
N2 C10 H10J 109.2 . . ?
C9 C10 H10K 109.2 . . ?
N2 C10 H10K 109.2 . . ?
H10J C10 H10K 107.9 . . ?
C12 C11 C13 109.4(9) . . ?
C12 C11 C4 108.7(7) . . ?
C13 C11 C4 113.2(6) . . ?
C12 C11 C14 106.1(10) . . ?
C13 C11 C14 109.9(10) . . ?
C4 C11 C14 109.3(7) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C15 C17 127.4(6) . . ?
N2 C15 H15A 116.3 . . ?
C17 C15 H15A 116.3 . . ?
C21 C16 C17 119.1(6) . . ?
C21 C16 S2 121.0(5) . . ?
C17 C16 S2 119.7(5) . . ?
C18 C17 C16 118.9(6) . . ?
C18 C17 C15 117.0(5) . . ?
C16 C17 C15 124.1(6) . . ?
C17 C18 C19 123.0(6) . . ?
C17 C18 H18A 118.5 . . ?
C19 C18 H18A 118.5 . . ?
C20 C19 C18 115.5(6) . . ?
C20 C19 C26 124.4(6) . . ?
C18 C19 C26 120.1(6) . . ?
C19 C20 C21 123.6(6) . . ?
C19 C20 H20A 118.2 . . ?
C21 C20 H20A 118.2 . . ?
C20 C21 C16 119.7(5) . . ?
C20 C21 C22 116.6(5) . . ?
C16 C21 C22 123.6(6) . . ?
N3 C22 C21 126.8(6) . . ?
N3 C22 H22A 116.6 . . ?
C21 C22 H22A 116.6 . . ?
N3 C23 C24 111.9(5) . . ?
N3 C23 H23A 109.2 . . ?
C24 C23 H23A 109.2 . . ?
N3 C23 H23B 109.2 . . ?
C24 C23 H23B 109.2 . . ?
H23A C23 H23B 107.9 . . ?
C25 C24 C23 114.0(6) . . ?
C25 C24 H24A 108.7 . . ?
C23 C24 H24A 108.7 . . ?
C25 C24 H24B 108.7 . . ?
C23 C24 H24B 108.7 . . ?
H24A C24 H24B 107.6 . . ?
N4 C25 C24 112.0(5) . . ?
N4 C25 H25A 109.2 . . ?
C24 C25 H25A 109.2 . . ?
N4 C25 H25B 109.2 . . ?
C24 C25 H25B 109.2 . . ?
H25A C25 H25B 107.9 . . ?
C19 C26 C27 109.5(6) . . ?
C19 C26 C28 111.5(6) . . ?
C27 C26 C28 110.3(6) . . ?
C19 C26 C29 108.7(6) . . ?
C27 C26 C29 108.8(6) . . ?
C28 C26 C29 108.1(6) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N4 C30 C2 127.3(6) . . ?
N4 C30 H30A 116.3 . . ?
C2 C30 H30A 116.3 . . ?
O1C Cl1 O1A 110.4(4) . . ?
O1C Cl1 O1D 110.7(4) . . ?
O1A Cl1 O1D 111.5(4) . . ?
O1C Cl1 O1B 109.9(6) . . ?
O1A Cl1 O1B 109.5(5) . . ?
O1D Cl1 O1B 104.7(6) . . ?
O2C Cl2 O2B 113.2(6) . . ?
O2C Cl2 O2D 108.4(5) . . ?
O2B Cl2 O2D 109.6(8) . . ?
O2C Cl2 O2A 109.1(5) . . ?
O2B Cl2 O2A 107.0(6) . . ?
O2D Cl2 O2A 109.5(6) . . ?
C100 O100 H100 115.9 . . ?
O100 C100 H10A 111.9 . . ?
O100 C100 H10B 108.6 . . ?
H10A C100 H10B 109.5 . . ?
O100 C100 H10C 107.9 . . ?
H10A C100 H10C 109.5 . . ?
H10B C100 H10C 109.5 . . ?
C101 N101 C102 117(2) . . ?
C101 N101 C103 115(2) . . ?
C102 N101 C103 128(2) . . ?
N101 C101 O101 133(2) . . ?
N101 C101 H101 113.4 . . ?
O101 C101 H101 113.4 . . ?
N101 C102 H10D 109.5 . . ?
N101 C102 H10E 109.5 . . ?
H10D C102 H10E 109.5 . . ?
N101 C102 H10F 109.5 . . ?
H10D C102 H10F 109.5 . . ?
H10E C102 H10F 109.5 . . ?
N101 C103 H10G 109.5 . . ?
N101 C103 H10H 109.5 . . ?
H10G C103 H10H 109.5 . . ?
N101 C103 H10I 109.5 . . ?
H10G C103 H10I 109.5 . . ?
H10H C103 H10I 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 N1 1.917(5) . ?
Ni1 N2 1.937(5) . ?
Ni1 S2 2.1565(18) . ?
Ni1 S1 2.1754(17) . ?
Ni2 N3 1.908(5) . ?
Ni2 N4 1.930(5) . ?
Ni2 S2 2.1574(17) . ?
Ni2 S1 2.1607(18) . ?
S1 C1 1.774(6) . ?
S2 C16 1.757(7) . ?
N1 C7 1.286(8) . ?
N1 C8 1.476(8) . ?
N2 C15 1.256(8) . ?
N2 C10 1.499(8) . ?
N3 C22 1.280(8) . ?
N3 C23 1.491(7) . ?
N4 C30 1.270(8) . ?
N4 C25 1.482(8) . ?
C1 C2 1.390(8) . ?
C1 C6 1.401(9) . ?
C2 C3 1.404(9) . ?
C2 C30 1.460(9) . ?
C3 C4 1.401(9) . ?
C3 H3A 0.9500 . ?
C4 C5 1.388(9) . ?
C4 C11 1.518(9) . ?
C5 C6 1.395(9) . ?
C5 H5A 0.9500 . ?
C6 C7 1.462(9) . ?
C7 H7A 0.9500 . ?
C8 C9 1.521(9) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.492(9) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10J 0.9900 . ?
C10 H10K 0.9900 . ?
C11 C12 1.491(13) . ?
C11 C13 1.506(11) . ?
C11 C14 1.524(14) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C17 1.454(9) . ?
C15 H15A 0.9500 . ?
C16 C21 1.391(9) . ?
C16 C17 1.417(8) . ?
C17 C18 1.387(9) . ?
C18 C19 1.417(9) . ?
C18 H18A 0.9500 . ?
C19 C20 1.383(9) . ?
C19 C26 1.511(9) . ?
C20 C21 1.388(9) . ?
C20 H20A 0.9500 . ?
C21 C22 1.471(8) . ?
C22 H22A 0.9500 . ?
C23 C24 1.513(9) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.493(10) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.515(10) . ?
C26 C28 1.533(10) . ?
C26 C29 1.561(10) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9500 . ?
Cl1 O1C 1.383(6) . ?
Cl1 O1A 1.392(5) . ?
Cl1 O1D 1.397(5) . ?
Cl1 O1B 1.405(7) . ?
Cl2 O2C 1.370(5) . ?
Cl2 O2B 1.387(7) . ?
Cl2 O2D 1.389(7) . ?
Cl2 O2A 1.413(6) . ?
O100 C100 1.419(10) . ?
O100 H100 0.8500 . ?
C100 H10A 0.9800 . ?
C100 H10B 0.9800 . ?
C100 H10C 0.9799 . ?
O101 C101 1.233(16) . ?
N101 C101 1.233(16) . ?
N101 C102 1.428(13) . ?
N101 C103 1.43(3) . ?
C101 H101 0.9500 . ?
C102 H10D 0.9800 . ?
C102 H10E 0.9800 . ?
C102 H10F 0.9800 . ?
C103 H10G 0.9800 . ?
C103 H10H 0.9800 . ?
C103 H10I 0.9800 . ?
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
N4 Ni2 S1 C1 -50.5(3) . . . . ?
S2 Ni2 S1 C1 129.4(2) . . . . ?
N4 Ni2 S1 Ni1 -153.91(17) . . . . ?
S2 Ni2 S1 Ni1 26.00(6) . . . . ?
N1 Ni1 S1 C1 51.5(3) . . . . ?
S2 Ni1 S1 C1 -129.8(2) . . . . ?
N1 Ni1 S1 Ni2 155.20(17) . . . . ?
S2 Ni1 S1 Ni2 -26.04(6) . . . . ?
N2 Ni1 S2 C16 -48.1(3) . . . . ?
S1 Ni1 S2 C16 131.2(2) . . . . ?
N2 Ni1 S2 Ni2 -153.13(17) . . . . ?
S1 Ni1 S2 Ni2 26.10(7) . . . . ?
N3 Ni2 S2 C16 48.7(3) . . . . ?
S1 Ni2 S2 C16 -131.9(2) . . . . ?
N3 Ni2 S2 Ni1 154.33(16) . . . . ?
S1 Ni2 S2 Ni1 -26.27(7) . . . . ?
N2 Ni1 N1 C7 141.1(6) . . . . ?
S1 Ni1 N1 C7 -38.3(6) . . . . ?
N2 Ni1 N1 C8 -38.9(5) . . . . ?
S1 Ni1 N1 C8 141.7(5) . . . . ?
N1 Ni1 N2 C15 -146.9(6) . . . . ?
S2 Ni1 N2 C15 34.3(6) . . . . ?
N1 Ni1 N2 C10 37.5(5) . . . . ?
S2 Ni1 N2 C10 -141.4(5) . . . . ?
N4 Ni2 N3 C22 143.6(5) . . . . ?
S2 Ni2 N3 C22 -36.4(5) . . . . ?
N4 Ni2 N3 C23 -38.9(5) . . . . ?
S2 Ni2 N3 C23 141.1(4) . . . . ?
N3 Ni2 N4 C30 -142.2(6) . . . . ?
S1 Ni2 N4 C30 38.4(6) . . . . ?
N3 Ni2 N4 C25 39.7(5) . . . . ?
S1 Ni2 N4 C25 -139.8(5) . . . . ?
Ni2 S1 C1 C2 44.4(5) . . . . ?
Ni1 S1 C1 C2 141.1(5) . . . . ?
Ni2 S1 C1 C6 -141.6(5) . . . . ?
Ni1 S1 C1 C6 -44.9(5) . . . . ?
C6 C1 C2 C3 0.0(10) . . . . ?
S1 C1 C2 C3 174.1(5) . . . . ?
C6 C1 C2 C30 -179.8(6) . . . . ?
S1 C1 C2 C30 -5.7(9) . . . . ?
C1 C2 C3 C4 0.4(10) . . . . ?
C30 C2 C3 C4 -179.8(6) . . . . ?
C2 C3 C4 C5 -0.8(10) . . . . ?
C2 C3 C4 C11 179.1(7) . . . . ?
C3 C4 C5 C6 0.8(10) . . . . ?
C11 C4 C5 C6 -179.0(7) . . . . ?
C4 C5 C6 C1 -0.5(10) . . . . ?
C4 C5 C6 C7 -179.7(6) . . . . ?
C2 C1 C6 C5 0.0(10) . . . . ?
S1 C1 C6 C5 -174.0(5) . . . . ?
C2 C1 C6 C7 179.2(6) . . . . ?
S1 C1 C6 C7 5.1(9) . . . . ?
C8 N1 C7 C6 -179.1(6) . . . . ?
Ni1 N1 C7 C6 0.9(10) . . . . ?
C5 C6 C7 N1 -155.3(7) . . . . ?
C1 C6 C7 N1 25.5(11) . . . . ?
C7 N1 C8 C9 -124.4(6) . . . . ?
Ni1 N1 C8 C9 55.6(7) . . . . ?
N1 C8 C9 C10 -68.0(8) . . . . ?
C8 C9 C10 N2 68.1(8) . . . . ?
C15 N2 C10 C9 129.1(6) . . . . ?
Ni1 N2 C10 C9 -54.7(7) . . . . ?
C5 C4 C11 C12 -58.0(10) . . . . ?
C3 C4 C11 C12 122.1(9) . . . . ?
C5 C4 C11 C13 -179.8(9) . . . . ?
C3 C4 C11 C13 0.3(12) . . . . ?
C5 C4 C11 C14 57.4(11) . . . . ?
C3 C4 C11 C14 -122.5(10) . . . . ?
C10 N2 C15 C17 176.5(6) . . . . ?
Ni1 N2 C15 C17 0.8(10) . . . . ?
Ni1 S2 C16 C21 -141.5(5) . . . . ?
Ni2 S2 C16 C21 -43.4(5) . . . . ?
Ni1 S2 C16 C17 43.6(5) . . . . ?
Ni2 S2 C16 C17 141.8(4) . . . . ?
C21 C16 C17 C18 -3.7(9) . . . . ?
S2 C16 C17 C18 171.2(5) . . . . ?
C21 C16 C17 C15 178.3(6) . . . . ?
S2 C16 C17 C15 -6.7(9) . . . . ?
N2 C15 C17 C18 158.7(6) . . . . ?
N2 C15 C17 C16 -23.4(11) . . . . ?
C16 C17 C18 C19 0.7(9) . . . . ?
C15 C17 C18 C19 178.7(6) . . . . ?
C17 C18 C19 C20 1.6(9) . . . . ?
C17 C18 C19 C26 -178.8(6) . . . . ?
C18 C19 C20 C21 -0.8(9) . . . . ?
C26 C19 C20 C21 179.6(6) . . . . ?
C19 C20 C21 C16 -2.2(9) . . . . ?
C19 C20 C21 C22 -179.2(6) . . . . ?
C17 C16 C21 C20 4.5(9) . . . . ?
S2 C16 C21 C20 -170.4(5) . . . . ?
C17 C16 C21 C22 -178.8(5) . . . . ?
S2 C16 C21 C22 6.3(8) . . . . ?
C23 N3 C22 C21 -175.8(6) . . . . ?
Ni2 N3 C22 C21 1.7(9) . . . . ?
C20 C21 C22 N3 -160.7(6) . . . . ?
C16 C21 C22 N3 22.4(10) . . . . ?
C22 N3 C23 C24 -127.9(6) . . . . ?
Ni2 N3 C23 C24 54.3(7) . . . . ?
N3 C23 C24 C25 -65.7(8) . . . . ?
C30 N4 C25 C24 125.3(6) . . . . ?
Ni2 N4 C25 C24 -56.4(7) . . . . ?
C23 C24 C25 N4 67.1(8) . . . . ?
C20 C19 C26 C27 122.0(7) . . . . ?
C18 C19 C26 C27 -57.5(8) . . . . ?
C20 C19 C26 C28 -0.3(10) . . . . ?
C18 C19 C26 C28 -179.8(6) . . . . ?
C20 C19 C26 C29 -119.3(7) . . . . ?
C18 C19 C26 C29 61.2(8) . . . . ?
C25 N4 C30 C2 175.9(6) . . . . ?
Ni2 N4 C30 C2 -2.3(10) . . . . ?
C1 C2 C30 N4 -23.6(11) . . . . ?
C3 C2 C30 N4 156.6(7) . . . . ?
C102 N101 C101 O101 -3(4) . . . . ?
C103 N101 C101 O101 178(3) . . . . ?
