#------------------------------------------------------------------------------
#$Date: 2016-02-18 10:40:55 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176722 $
#$URL: svn://www.crystallography.net/cod/cif/3/50/00/3500007.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_3500007
loop_
_publ_author_name
'Mohammad Abul Haj'
'Miguel Quirós'
'Juan M. Salas'
_journal_name_full               'Personal communication to COD'
_journal_year                    2011
_chemical_formula_sum            'C30 H54 N14 Ni O3 S'
_chemical_formula_weight         749.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.349(3)
_cell_length_b                   18.253(4)
_cell_length_c                   13.274(3)
_cell_measurement_temperature    253(2)
_cell_volume                     3718.9(14)
_computing_cell_refinement       'DENZO-SMN (Enraf Nonius'
_computing_data_collection       'Collect (Enraf Nonius)'
_computing_data_reduction        'DENZO-SMN (Enraf Nonius'
_computing_molecular_graphics    'SHELXTL v5.1 IRIX'
_computing_publication_material  'SHELXTL v5.1 IRIX'
_computing_structure_refinement  'SHELXTL v5.1 IRIX'
_computing_structure_solution    'SHELXTL v5.1 IRIX'
_diffrn_ambient_temperature      253(2)
_diffrn_measurement_device       'Nonius KappaCCD Diffractometer'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2382
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4708
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.816
_refine_ls_goodness_of_fit_obs   1.110
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         4708
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.815
_refine_ls_restrained_S_obs      1.110
_refine_ls_R_factor_all          0.2234
_refine_ls_R_factor_obs          0.0643
_refine_ls_shift/esd_max         0.055
_refine_ls_shift/esd_mean        0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0340P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_wR_factor_all         0.1057
_refine_ls_wR_factor_obs         0.0801
_reflns_number_observed          1758
_reflns_number_total             4708
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            nidah_baja.cif
_cod_data_source_block           pna21
_cod_original_cell_volume        3718.9(13)
_cod_database_code               3500007
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'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ni Ni 0.24169(4) 0.09834(3) 0.52499(13) 0.0414(2) Uani 1 d . .
N1P N 0.2582(4) 0.1813(4) 0.6385(6) 0.048(2) Uani 1 d . .
H11A H 0.2491 0.2260 0.6124 0.058 Uiso 1 calc . .
H11B H 0.2198 0.1744 0.6889 0.058 Uiso 1 calc . .
N2P N 0.3791(3) 0.0969(3) 0.5375(7) 0.049(2) Uani 1 d . .
H12A H 0.3963 0.0550 0.5671 0.058 Uiso 1 calc . .
H12B H 0.4031 0.0990 0.4757 0.058 Uiso 1 calc . .
C1P C 0.3471(5) 0.1756(5) 0.6766(8) 0.066(3) Uani 1 d . .
H11 H 0.3475 0.1323 0.7164 0.080 Uiso 1 calc . .
C2P C 0.4085(5) 0.1604(5) 0.5983(7) 0.075(3) Uani 1 d . .
H12 H 0.4065 0.2027 0.5529 0.090 Uiso 1 calc . .
C3P C 0.5015(5) 0.1542(5) 0.6322(7) 0.071(3) Uani 1 d . .
H13A H 0.5390 0.1527 0.5735 0.085 Uiso 1 calc . .
H13B H 0.5089 0.1085 0.6685 0.085 Uiso 1 calc . .
C4P C 0.5294(6) 0.2164(7) 0.6988(10) 0.100(4) Uani 1 d . .
H14A H 0.5858 0.2050 0.7277 0.120 Uiso 1 calc . .
H14B H 0.5360 0.2602 0.6581 0.120 Uiso 1 calc . .
C5P C 0.4686(8) 0.2312(6) 0.7792(9) 0.100(4) Uani 1 d . .
H15A H 0.4847 0.2766 0.8122 0.120 Uiso 1 calc . .
H15B H 0.4721 0.1922 0.8288 0.120 Uiso 1 calc . .
C6P C 0.3759(6) 0.2371(5) 0.7414(7) 0.070(3) Uani 1 d . .
H16A H 0.3372 0.2401 0.7991 0.083 Uiso 1 calc . .
H16B H 0.3701 0.2824 0.7038 0.083 Uiso 1 calc . .
N1Q N 0.2300(4) 0.0150(4) 0.6356(6) 0.051(2) Uani 1 d . .
H21A H 0.2815 0.0081 0.6667 0.062 Uiso 1 calc . .
H21B H 0.1904 0.0280 0.6822 0.062 Uiso 1 calc . .
N2Q N 0.2395(4) 0.0063(4) 0.4284(6) 0.052(2) Uani 1 d . .
H22A H 0.1881 0.0040 0.3957 0.062 Uiso 1 calc . .
H22B H 0.2822 0.0099 0.3823 0.062 Uiso 1 calc . .
C1Q C 0.2026(5) -0.0528(4) 0.5853(7) 0.059(2) Uani 1 d . .
H21 H 0.1415 -0.0458 0.5664 0.070 Uiso 1 calc . .
C2Q C 0.2519(5) -0.0604(4) 0.4899(6) 0.055(3) Uani 1 d . .
H22 H 0.3139 -0.0637 0.5070 0.066 Uiso 1 calc . .
C3Q C 0.2278(6) -0.1284(5) 0.4353(7) 0.084(4) Uani 1 d . .
H23A H 0.2667 -0.1353 0.3785 0.100 Uiso 1 calc . .
H23B H 0.1689 -0.1239 0.4096 0.100 Uiso 1 calc . .
C4Q C 0.2339(9) -0.1971(4) 0.5081(12) 0.117(5) Uani 1 d . .
H24A H 0.2164 -0.2406 0.4714 0.140 Uiso 1 calc . .
H24B H 0.2940 -0.2036 0.5288 0.140 Uiso 1 calc . .
C5Q C 0.1792(9) -0.1899(5) 0.5980(9) 0.117(4) Uani 1 d . .
H25A H 0.1868 -0.2324 0.6411 0.140 Uiso 1 calc . .
H25B H 0.1184 -0.1871 0.5787 0.140 Uiso 1 calc . .
C6Q C 0.2054(7) -0.1212(5) 0.6539(7) 0.078(3) Uani 1 d . .
H26A H 0.2639 -0.1272 0.6803 0.093 Uiso 1 calc . .
H26B H 0.1663 -0.1139 0.7105 0.093 Uiso 1 calc . .
N1R N 0.1047(3) 0.1136(3) 0.5187(7) 0.047(2) Uani 1 d . .
H31A H 0.0788 0.0729 0.4950 0.056 Uiso 1 calc . .
H31B H 0.0837 0.1227 0.5808 0.056 Uiso 1 calc . .
N2R N 0.2379(4) 0.1731(4) 0.4064(6) 0.044(2) Uani 1 d . .
H32A H 0.2546 0.2176 0.4284 0.052 Uiso 1 calc . .
H32B H 0.2749 0.1589 0.3576 0.052 Uiso 1 calc . .
C1R C 0.0864(5) 0.1758(4) 0.4520(7) 0.052(2) Uani 1 d . .
H31 H 0.0971 0.2203 0.4912 0.063 Uiso 1 calc . .
C2R C 0.1483(5) 0.1770(4) 0.3659(6) 0.049(2) Uani 1 d . .
H32 H 0.1387 0.1316 0.3280 0.059 Uiso 1 calc . .
C3R C 0.1340(6) 0.2400(4) 0.2921(7) 0.062(2) Uani 1 d . .
H33A H 0.1723 0.2343 0.2345 0.074 Uiso 1 calc . .
H33B H 0.1477 0.2862 0.3246 0.074 Uiso 1 calc . .
C4R C 0.0388(7) 0.2407(5) 0.2566(8) 0.080(3) Uani 1 d . .
H34A H 0.0293 0.2830 0.2136 0.096 Uiso 1 calc . .
H34B H 0.0274 0.1971 0.2170 0.096 Uiso 1 calc . .
C5R C -0.0226(6) 0.2435(5) 0.3425(10) 0.085(3) Uani 1 d . .
H35A H -0.0819 0.2418 0.3172 0.102 Uiso 1 calc . .
H35B H -0.0151 0.2894 0.3783 0.102 Uiso 1 calc . .
C6R C -0.0081(5) 0.1795(4) 0.4157(7) 0.068(3) Uani 1 d . .
H36A H -0.0464 0.1852 0.4733 0.081 Uiso 1 calc . .
H36B H -0.0231 0.1339 0.3824 0.081 Uiso 1 calc . .
N1A N 0.4402(6) 0.0434(5) 0.3229(8) 0.091(3) Uani 1 d . .
C2A C 0.5177(12) 0.0173(6) 0.3311(10) 0.110(4) Uani 1 d . .
H42 H 0.5352 -0.0048 0.3908 0.132 Uiso 1 calc . .
N3A N 0.5744(5) 0.0222(5) 0.2521(9) 0.096(3) Uani 1 d . .
N4A N 0.5446(5) 0.0732(5) 0.0905(8) 0.097(3) Uani 1 d . .
C5A C 0.4793(9) 0.1034(6) 0.0425(9) 0.100(3) Uani 1 d . .
H45 H 0.4910 0.1171 -0.0236 0.120 Uiso 1 calc . .
C6A C 0.3985(8) 0.1175(5) 0.0742(9) 0.093(4) Uani 1 d . .
H46 H 0.3595 0.1399 0.0303 0.111 Uiso 1 calc . .
C7A C 0.3705(6) 0.0995(6) 0.1725(10) 0.081(3) Uani 1 d . .
O7A O 0.3029(4) 0.1059(4) 0.2185(6) 0.109(3) Uani 1 d . .
N8A N 0.4417(5) 0.0667(4) 0.2258(7) 0.066(2) Uani 1 d . .
C3AA C 0.5241(7) 0.0543(5) 0.1855(9) 0.070(3) Uani 1 d . .
N1B N 0.0634(5) 0.0754(4) -0.2450(8) 0.086(3) Uani 1 d . .
C2B C -0.0065(7) 0.0328(6) -0.2415(10) 0.087(4) Uani 1 d . .
H52 H -0.0339 0.0163 -0.2997 0.105 Uiso 1 calc . .
N3B N -0.0360(5) 0.0145(4) -0.1485(8) 0.085(3) Uani 1 d . .
N4B N 0.0165(5) 0.0450(4) 0.0155(10) 0.104(3) Uani 1 d . .
C5B C 0.0762(8) 0.0853(6) 0.0464(11) 0.122(5) Uani 1 d . .
H55 H 0.0769 0.0892 0.1162 0.146 Uiso 1 calc . .
C6B C 0.1405(6) 0.1250(5) 0.0023(8) 0.082(3) Uani 1 d . .
H56 H 0.1800 0.1499 0.0428 0.099 Uiso 1 calc . .
C7B C 0.1490(6) 0.1295(6) -0.1044(10) 0.090(4) Uani 1 d . .
O7B O 0.1996(6) 0.1533(5) -0.1566(7) 0.157(4) Uani 1 d . .
N8B N 0.0784(5) 0.0868(4) -0.1444(7) 0.061(2) Uani 1 d . .
C3AB C 0.0210(6) 0.0489(5) -0.0929(9) 0.062(3) Uani 1 d . .
S1D S 0.7892(5) 0.0999(3) 0.5269(9) 0.080(3) Uani 0.451(9) d P .
S1D' S 0.7174(4) 0.0997(2) 0.5259(7) 0.080(2) Uani 0.549(9) d P .
O1D O 0.7534(4) 0.1777(2) 0.5180(9) 0.102(2) Uani 1 d . .
C1D C 0.7659(8) 0.0621(6) 0.6399(11) 0.131(5) Uani 1 d . .
C2D C 0.7514(9) 0.0518(8) 0.4316(10) 0.146(6) Uani 1 d . .
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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2R Ni N2Q 93.5(3) . . ?
N2R Ni N2P 95.5(3) . . ?
N2Q Ni N2P 93.1(3) . . ?
N2R Ni N1R 81.8(3) . . ?
N2Q Ni N1R 93.7(2) . . ?
N2P Ni N1R 172.8(2) . . ?
N2R Ni N1Q 171.8(3) . . ?
N2Q Ni N1Q 81.3(2) . . ?
N2P Ni N1Q 91.2(3) . . ?
N1R Ni N1Q 92.2(3) . . ?
N2R Ni N1P 94.1(2) . . ?
N2Q Ni N1P 170.5(3) . . ?
N2P Ni N1P 80.6(3) . . ?
N1R Ni N1P 93.0(3) . . ?
N1Q Ni N1P 91.7(3) . . ?
C1P N1P Ni 107.6(5) . . ?
C2P N2P Ni 109.7(4) . . ?
C2P C1P N1P 112.3(8) . . ?
C2P C1P C6P 111.9(7) . . ?
N1P C1P C6P 115.3(8) . . ?
C1P C2P N2P 110.3(7) . . ?
C1P C2P C3P 115.0(8) . . ?
N2P C2P C3P 113.3(7) . . ?
C2P C3P C4P 113.1(8) . . ?
C5P C4P C3P 113.1(8) . . ?
C4P C5P C6P 112.1(10) . . ?
C1P C6P C5P 114.8(8) . . ?
C1Q N1Q Ni 108.3(6) . . ?
C2Q N2Q Ni 108.5(6) . . ?
N1Q C1Q C2Q 108.8(7) . . ?
N1Q C1Q C6Q 113.9(8) . . ?
C2Q C1Q C6Q 114.4(8) . . ?
C1Q C2Q N2Q 109.2(7) . . ?
C1Q C2Q C3Q 111.6(8) . . ?
N2Q C2Q C3Q 112.7(6) . . ?
C2Q C3Q C4Q 110.5(7) . . ?
C5Q C4Q C3Q 113.1(9) . . ?
C4Q C5Q C6Q 108.8(10) . . ?
C5Q C6Q C1Q 112.0(8) . . ?
C1R N1R Ni 108.3(4) . . ?
C2R N2R Ni 109.4(5) . . ?
N1R C1R C2R 110.7(6) . . ?
N1R C1R C6R 113.9(6) . . ?
C2R C1R C6R 111.3(7) . . ?
C1R C2R N2R 108.3(7) . . ?
C1R C2R C3R 114.3(7) . . ?
N2R C2R C3R 113.8(7) . . ?
C2R C3R C4R 109.9(7) . . ?
C5R C4R C3R 111.7(9) . . ?
C4R C5R C6R 111.7(7) . . ?
C1R C6R C5R 111.7(7) . . ?
C2A N1A N8A 100.4(9) . . ?
N1A C2A N3A 120.1(12) . . ?
C3AA N3A C2A 99.9(10) . . ?
C5A N4A C3AA 112.7(9) . . ?
N4A C5A C6A 129.8(11) . . ?
C5A C6A C7A 121.9(10) . . ?
O7A C7A C6A 134.8(12) . . ?
O7A C7A N8A 116.5(12) . . ?
C6A C7A N8A 108.8(9) . . ?
N1A N8A C3AA 109.2(9) . . ?
N1A N8A C7A 125.9(10) . . ?
C3AA N8A C7A 124.8(10) . . ?
N3A C3AA N4A 127.6(10) . . ?
N3A C3AA N8A 110.4(10) . . ?
N4A C3AA N8A 122.0(11) . . ?
C2B N1B N8B 101.0(9) . . ?
N1B C2B N3B 116.5(11) . . ?
N1B C2B C3AB 77.3(7) . . ?
N3B C2B C3AB 39.1(5) . . ?
C3AB N3B C2B 99.9(8) . . ?
C5B N4B C3AB 105.3(12) . . ?
N4B C5B C6B 135.2(16) . . ?
C5B C6B C7B 121.8(11) . . ?
O7B C7B C6B 134.1(12) . . ?
O7B C7B N8B 120.1(12) . . ?
C6B C7B N8B 105.5(8) . . ?
C3AB N8B N1B 108.4(8) . . ?
C3AB N8B C7B 126.8(10) . . ?
N1B N8B C7B 124.7(9) . . ?
N8B C3AB N3B 114.1(11) . . ?
N8B C3AB N4B 125.4(10) . . ?
N3B C3AB N4B 120.5(10) . . ?
N8B C3AB C2B 73.2(7) . . ?
N3B C3AB C2B 41.0(6) . . ?
N4B C3AB C2B 161.4(9) . . ?
S1D' S1D O1D 69.0(5) . . ?
S1D' S1D C2D 68.7(7) . . ?
O1D S1D C2D 108.1(9) . . ?
S1D' S1D C1D 78.4(7) . . ?
O1D S1D C1D 111.9(9) . . ?
C2D S1D C1D 112.9(6) . . ?
S1D S1D' O1D 68.7(5) . . ?
S1D S1D' C2D 71.8(7) . . ?
O1D S1D' C2D 109.6(8) . . ?
S1D S1D' C1D 65.3(7) . . ?
O1D S1D' C1D 105.1(7) . . ?
C2D S1D' C1D 107.9(5) . . ?
S1D O1D S1D' 42.2(2) . . ?
S1D C1D S1D' 36.4(3) . . ?
S1D' C2D S1D 39.5(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni N2R 2.084(7) . ?
Ni N2Q 2.114(8) . ?
Ni N2P 2.115(5) . ?
Ni N1R 2.123(4) . ?
Ni N1Q 2.122(8) . ?
Ni N1P 2.152(8) . ?
N1P C1P 1.458(9) . ?
N2P C2P 1.483(9) . ?
C1P C2P 1.431(12) . ?
C1P C6P 1.482(11) . ?
C2P C3P 1.501(10) . ?
C3P C4P 1.502(13) . ?
C4P C5P 1.443(14) . ?
C5P C6P 1.513(12) . ?
N1Q C1Q 1.467(10) . ?
N2Q C2Q 1.478(10) . ?
C1Q C2Q 1.482(10) . ?
C1Q C6Q 1.546(11) . ?
C2Q C3Q 1.484(11) . ?
C3Q C4Q 1.587(13) . ?
C4Q C5Q 1.46(2) . ?
C5Q C6Q 1.513(12) . ?
N1R C1R 1.466(9) . ?
N2R C2R 1.478(9) . ?
C1R C2R 1.486(10) . ?
C1R C6R 1.531(10) . ?
C2R C3R 1.528(11) . ?
C3R C4R 1.535(11) . ?
C4R C5R 1.481(14) . ?
C5R C6R 1.535(12) . ?
N1A C2A 1.286(14) . ?
N1A N8A 1.357(11) . ?
C2A N3A 1.365(14) . ?
N3A C3AA 1.312(12) . ?
N4A C5A 1.308(12) . ?
N4A C3AA 1.345(12) . ?
C5A C6A 1.336(12) . ?
C6A C7A 1.412(13) . ?
C7A O7A 1.209(10) . ?
C7A N8A 1.433(11) . ?
N8A C3AA 1.392(10) . ?
N1B C2B 1.326(12) . ?
N1B N8B 1.370(10) . ?
C2B N3B 1.357(14) . ?
C2B C3AB 2.04(2) . ?
N3B C3AB 1.305(11) . ?
N4B C5B 1.245(13) . ?
N4B C3AB 1.443(14) . ?
C5B C6B 1.357(13) . ?
C6B C7B 1.424(14) . ?
C7B O7B 1.128(10) . ?
C7B N8B 1.438(11) . ?
N8B C3AB 1.311(10) . ?
S1D S1D' 1.102(4) . ?
S1D O1D 1.528(7) . ?
S1D C2D 1.65(2) . ?
S1D C1D 1.689(15) . ?
S1D' O1D 1.531(6) . ?
S1D' C2D 1.61(2) . ?
S1D' C1D 1.821(14) . ?
