#------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/10/1101052.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_1101052
loop_
_publ_author_name
'Sawsan Salameh'
'Mohammad Abul-Haj'
'Miguel Quirós'
'Juan M. Salas'
_journal_name_full               'European Journal of Inorganic Chemistry'
_journal_page_first              2779
_journal_page_last               2782
_journal_year                    2005
_chemical_formula_sum            'C40 H72 N40 Ni9 O42'
_chemical_formula_weight         2313.77
_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                65.9660(10)
_cell_angle_beta                 83.2870(10)
_cell_angle_gamma                86.0430(10)
_cell_formula_units_Z            2
_cell_length_a                   11.0481(5)
_cell_length_b                   18.2700(8)
_cell_length_c                   21.3860(9)
_cell_measurement_reflns_used    8147
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.72
_cell_measurement_theta_min      2.22
_cell_volume                     3914.4(3)
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       'phi and omega 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  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0657
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            45862
_diffrn_reflns_theta_max         28.45
_diffrn_reflns_theta_min         1.25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         281
_exptl_absorpt_coefficient_mu    2.237
_exptl_absorpt_correction_T_max  0.8775
_exptl_absorpt_correction_T_min  0.6667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'greenish blue'
_exptl_crystal_density_diffrn    1.963
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregularly shaped block'
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1137
_refine_ls_number_reflns         17819
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1142
_refine_ls_R_factor_gt           0.0808
_refine_ls_shift/su_max          0.269
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1300P)²+20.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2202
_refine_ls_wR_factor_ref         0.2454
_reflns_number_gt                12041
_reflns_number_total             17819
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               1101052
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
Ni1A Ni 0.0000 0.5000 0.5000 0.0190(2) Uani 1 2 d S . .
Ni2A Ni 0.03973(7) 0.68484(5) 0.34406(4) 0.01947(18) Uani 1 1 d . . .
Ni3A Ni 0.09435(9) 0.85454(5) 0.30989(4) 0.0289(2) Uani 1 1 d . . .
Ni4A Ni -0.11395(8) 0.79637(5) 0.23763(4) 0.0287(2) Uani 1 1 d . . .
Ni5A Ni 0.19509(9) 0.74489(5) 0.20671(4) 0.0319(2) Uani 1 1 d . . .
O1 O -0.0549(4) 0.7904(3) 0.3248(2) 0.0255(10) Uani 1 1 d . . .
H1 H -0.1189 0.7915 0.3616 0.031 Uiso 1 1 d R . .
O2 O 0.1828(4) 0.7604(3) 0.2964(2) 0.0265(10) Uani 1 1 d . . .
H2 H 0.2583 0.7428 0.3208 0.032 Uiso 1 1 d R . .
O3 O 0.0213(4) 0.7119(3) 0.2412(2) 0.0285(10) Uani 1 1 d . . .
H3 H -0.0043 0.6662 0.2320 0.034 Uiso 1 1 d R . .
N1M N -0.0021(7) 0.9561(4) 0.3052(4) 0.0483(19) Uani 1 1 d . . .
N2M N 0.2563(8) 0.9147(5) 0.2838(5) 0.071(3) Uani 1 1 d . . .
O1M O -0.1604(6) 0.8119(4) 0.1409(3) 0.0526(16) Uani 1 1 d . . .
O2M O -0.2477(6) 0.8827(3) 0.2342(3) 0.0499(15) Uani 1 1 d . . .
O3M O 0.3666(6) 0.7911(4) 0.1695(4) 0.079(3) Uani 1 1 d . . .
O4M O 0.1890(8) 0.7246(5) 0.1180(3) 0.087(3) Uani 1 1 d . . .
N1A N 0.0645(5) 0.6777(3) 0.4392(3) 0.0215(11) Uani 1 1 d . . .
N2A N 0.0495(5) 0.6091(3) 0.4985(2) 0.0204(10) Uani 1 1 d . . .
C3A C 0.0700(6) 0.6249(4) 0.5502(3) 0.0238(13) Uani 1 1 d . . .
H3A H 0.0671 0.5875 0.5968 0.029 Uiso 1 1 d R . .
N4A N 0.0962(5) 0.7039(3) 0.5265(3) 0.0235(11) Uani 1 1 d . . .
C5A C 0.1200(7) 0.7530(4) 0.5593(4) 0.0304(15) Uani 1 1 d . . .
H5A H 0.1194 0.7330 0.6079 0.037 Uiso 1 1 d R . .
C6A C 0.1432(6) 0.8294(4) 0.5191(4) 0.0300(15) Uani 1 1 d . . .
H6A H 0.1592 0.8645 0.5398 0.036 Uiso 1 1 d R . .
C7A C 0.1448(7) 0.8607(4) 0.4454(4) 0.0312(15) Uani 1 1 d . . .
O7A O 0.1722(6) 0.9324(3) 0.4087(3) 0.0420(13) Uani 1 1 d . . .
N8A N 0.1154(5) 0.8118(3) 0.4147(3) 0.0251(11) Uani 1 1 d . . .
C8AA C 0.0927(6) 0.7353(4) 0.4566(3) 0.0217(12) Uani 1 1 d . . .
N1B N -0.1181(5) 0.6246(3) 0.3767(3) 0.0213(11) Uani 1 1 d . . .
N2B N -0.1364(5) 0.5553(3) 0.4353(3) 0.0213(11) Uani 1 1 d . . .
C3B C -0.2463(6) 0.5328(4) 0.4403(3) 0.0290(14) Uani 1 1 d . . .
H3B H -0.2812 0.4862 0.4760 0.035 Uiso 1 1 d R . .
N4B N -0.3044(5) 0.5861(4) 0.3862(3) 0.0285(12) Uani 1 1 d . . .
C5B C -0.4221(7) 0.5915(5) 0.3675(5) 0.0425(19) Uani 1 1 d . . .
H5B H -0.4822 0.5538 0.3949 0.051 Uiso 1 1 d R . .
C6B C -0.4463(7) 0.6515(5) 0.3099(4) 0.0424(19) Uani 1 1 d . . .
H6B H -0.5267 0.6578 0.2965 0.051 Uiso 1 1 d R . .
C7B C -0.3538(7) 0.7085(5) 0.2657(4) 0.0368(17) Uani 1 1 d . . .
O7B O -0.3772(5) 0.7595(4) 0.2075(3) 0.0497(15) Uani 1 1 d . . .
N8B N -0.2426(5) 0.7056(3) 0.2883(3) 0.0285(12) Uani 1 1 d . . .
C8AB C -0.2214(6) 0.6430(4) 0.3473(3) 0.0234(13) Uani 1 1 d . . .
N1C N 0.1402(5) 0.5841(3) 0.3568(3) 0.0227(11) Uani 1 1 d . . .
N2C N 0.1275(5) 0.5139(3) 0.4158(3) 0.0227(11) Uani 1 1 d . . .
C3C C 0.2097(6) 0.4620(4) 0.4102(3) 0.0255(13) Uani 1 1 d . . .
H3C H 0.2203 0.4089 0.4436 0.031 Uiso 1 1 d R . .
N4C N 0.2789(5) 0.4960(3) 0.3488(3) 0.0220(11) Uani 1 1 d . . .
C5C C 0.3770(6) 0.4676(4) 0.3172(4) 0.0279(14) Uani 1 1 d . . .
H5C H 0.4107 0.4151 0.3388 0.034 Uiso 1 1 d R . .
C6C C 0.4210(6) 0.5177(4) 0.2552(4) 0.0309(15) Uani 1 1 d . . .
H6C H 0.4882 0.5004 0.2322 0.037 Uiso 1 1 d R . .
C7C C 0.3706(6) 0.5984(4) 0.2211(4) 0.0316(15) Uani 1 1 d . . .
O7C O 0.4169(6) 0.6424(4) 0.1632(3) 0.0540(17) Uani 1 1 d . . .
N8C N 0.2755(5) 0.6244(3) 0.2541(3) 0.0241(11) Uani 1 1 d . . .
C8AC C 0.2325(6) 0.5721(4) 0.3168(3) 0.0205(12) Uani 1 1 d . . .
N1D N 0.0219(8) 0.8869(4) 0.1860(4) 0.062(2) Uani 1 1 d . . .
N2D N 0.1278(6) 0.8625(4) 0.1577(3) 0.0401(15) Uani 1 1 d . . .
C3D C 0.1613(8) 0.9202(5) 0.0996(4) 0.0415(19) Uani 1 1 d . . .
H3D H 0.2298 0.9183 0.0690 0.050 Uiso 1 1 d R . .
N4D N 0.0824(6) 0.9846(4) 0.0892(3) 0.0357(14) Uani 1 1 d . . .
C5D C 0.0721(9) 1.0584(5) 0.0361(4) 0.047(2) Uani 1 1 d . . .
H5D H 0.1299 1.0746 -0.0033 0.057 Uiso 1 1 d R . .
C6D C -0.0205(9) 1.1067(5) 0.0409(4) 0.052(2) Uani 1 1 d . . .
H6D H -0.0257 1.1590 0.0056 0.062 Uiso 1 1 d R . .
C7D C -0.1130(10) 1.0814(5) 0.0990(5) 0.061(3) Uani 1 1 d . . .
O7D O -0.2026(8) 1.1255(4) 0.1033(4) 0.087(3) Uani 1 1 d . . .
N8D N -0.1009(9) 1.0074(5) 0.1508(4) 0.072(3) Uani 1 1 d . . .
C8AD C -0.0027(9) 0.9618(5) 0.1436(4) 0.053(2) Uani 1 1 d . . .
Ni1B Ni 0.5000 0.5000 0.0000 0.0172(2) Uani 1 2 d S . .
Ni2B Ni 0.47250(7) 0.31102(5) 0.15147(4) 0.01922(18) Uani 1 1 d . . .
Ni3B Ni 0.63537(8) 0.20220(5) 0.25321(4) 0.0298(2) Uani 1 1 d . . .
Ni4B Ni 0.43198(9) 0.14026(5) 0.17978(5) 0.0338(2) Uani 1 1 d . . .
Ni5B Ni 0.31123(8) 0.23975(6) 0.28574(4) 0.0327(2) Uani 1 1 d . . .
O4 O 0.5756(4) 0.2092(3) 0.1665(2) 0.0284(10) Uani 1 1 d . . .
H4 H 0.6396 0.2121 0.1285 0.034 Uiso 1 1 d R . .
O5 O 0.4885(4) 0.2755(3) 0.2552(2) 0.0267(10) Uani 1 1 d . . .
H5 H 0.5079 0.3206 0.2672 0.032 Uiso 1 1 d R . .
O6 O 0.3325(4) 0.2324(3) 0.1927(2) 0.0275(10) Uani 1 1 d . . .
H6 H 0.2584 0.2490 0.1670 0.033 Uiso 1 1 d R . .
N3M N 0.7644(6) 0.1153(4) 0.2518(4) 0.0423(16) Uani 1 1 d . . .
N4M N 0.6607(7) 0.1765(4) 0.3532(3) 0.0417(16) Uani 1 1 d . . .
O5M O 0.5525(7) 0.0498(3) 0.1701(3) 0.0616(18) Uani 1 1 d . . .
O6M O 0.2842(6) 0.0673(3) 0.1960(4) 0.0617(19) Uani 1 1 d . . .
O7M O 0.1333(5) 0.1936(3) 0.3074(3) 0.0474(15) Uani 1 1 d . . .
O8M O 0.2976(7) 0.2381(5) 0.3835(3) 0.068(2) Uani 1 1 d . . .
N1E N 0.6248(5) 0.3768(3) 0.1215(3) 0.0224(11) Uani 1 1 d . . .
N2E N 0.6397(5) 0.4460(3) 0.0631(3) 0.0205(10) Uani 1 1 d . . .
C3E C 0.7489(5) 0.4710(4) 0.0568(3) 0.0230(13) Uani 1 1 d . . .
H3E H 0.7815 0.5183 0.0210 0.028 Uiso 1 1 d R . .
N4E N 0.8097(5) 0.4185(3) 0.1099(3) 0.0237(11) Uani 1 1 d . . .
C5E C 0.9278(6) 0.4165(5) 0.1274(4) 0.0315(15) Uani 1 1 d . . .
H5E H 0.9851 0.4562 0.0999 0.038 Uiso 1 1 d R . .
C6E C 0.9554(6) 0.3569(5) 0.1840(4) 0.0328(16) Uani 1 1 d . . .
H6E H 1.0358 0.3531 0.1969 0.039 Uiso 1 1 d R . .
C7E C 0.8679(6) 0.2956(4) 0.2286(4) 0.0309(15) Uani 1 1 d . . .
O7E O 0.8959(5) 0.2433(3) 0.2848(3) 0.0419(13) Uani 1 1 d . . .
N8E N 0.7550(5) 0.2974(3) 0.2073(3) 0.0273(12) Uani 1 1 d . . .
C8AE C 0.7282(6) 0.3605(4) 0.1492(3) 0.0234(13) Uani 1 1 d . . .
N1F N 0.4528(5) 0.3215(3) 0.0549(3) 0.0211(11) Uani 1 1 d . . .
N2F N 0.4565(5) 0.3926(3) -0.0022(2) 0.0196(10) Uani 1 1 d . . .
C3F C 0.4294(6) 0.3810(4) -0.0542(3) 0.0240(13) Uani 1 1 d . . .
H3F H 0.4258 0.4209 -0.0995 0.029 Uiso 1 1 d R . .
N4F N 0.4061(5) 0.3014(3) -0.0333(3) 0.0239(11) Uani 1 1 d . . .
C5F C 0.3775(7) 0.2574(4) -0.0686(4) 0.0326(15) Uani 1 1 d . . .
H5F H 0.3688 0.2812 -0.1165 0.039 Uiso 1 1 d R . .
C6F C 0.3622(8) 0.1799(5) -0.0318(5) 0.044(2) Uani 1 1 d . . .
H6F H 0.3465 0.1468 -0.0544 0.053 Uiso 1 1 d R . .
C7F C 0.3694(8) 0.1433(5) 0.0420(5) 0.046(2) Uani 1 1 d . . .
O7F O 0.3413(8) 0.0710(3) 0.0761(4) 0.068(2) Uani 1 1 d . . .
N8F N 0.4036(6) 0.1887(3) 0.0745(3) 0.0328(13) Uani 1 1 d . . .
C8AF C 0.4206(5) 0.2666(4) 0.0352(3) 0.0232(13) Uani 1 1 d . . .
N1G N 0.3650(4) 0.4077(3) 0.1432(2) 0.0195(10) Uani 1 1 d . . .
N2G N 0.3730(5) 0.4802(3) 0.0865(2) 0.0193(10) Uani 1 1 d . . .
C3G C 0.2901(6) 0.5297(4) 0.0953(3) 0.0242(13) Uani 1 1 d . . .
H3G H 0.2765 0.5832 0.0636 0.029 Uiso 1 1 d R . .
N4G N 0.2259(5) 0.4925(3) 0.1578(3) 0.0233(11) Uani 1 1 d . . .
C5G C 0.1311(6) 0.5178(4) 0.1932(4) 0.0307(15) Uani 1 1 d . . .
H5G H 0.0960 0.5702 0.1738 0.037 Uiso 1 1 d R . .
C6G C 0.0917(6) 0.4657(4) 0.2551(4) 0.0313(15) Uani 1 1 d . . .
H6G H 0.0261 0.4814 0.2802 0.038 Uiso 1 1 d R . .
C7G C 0.1447(6) 0.3852(5) 0.2862(4) 0.0314(15) Uani 1 1 d . . .
O7G O 0.1070(5) 0.3401(4) 0.3455(3) 0.0472(15) Uani 1 1 d . . .
N8G N 0.2357(5) 0.3608(3) 0.2491(3) 0.0258(12) Uani 1 1 d . . .
C8AG C 0.2746(5) 0.4160(4) 0.1865(3) 0.0221(12) Uani 1 1 d . . .
N1H N 0.4521(8) 0.0927(5) 0.2875(4) 0.069(3) Uani 1 1 d . . .
N2H N 0.3791(6) 0.1233(4) 0.3287(3) 0.0482(19) Uani 1 1 d . . .
C3H C 0.3675(10) 0.0710(6) 0.3917(5) 0.067(3) Uani 1 1 d . . .
H3H H 0.3217 0.0777 0.4295 0.080 Uiso 1 1 d R . .
N4H N 0.4319(8) 0.0060(5) 0.3942(4) 0.073(3) Uani 1 1 d . . .
C5H C 0.4430(11) -0.0688(7) 0.4548(8) 0.095(5) Uani 1 1 d . . .
H5H H 0.4064 -0.0793 0.4999 0.113 Uiso 1 1 d R . .
C6H C 0.5093(11) -0.1155(8) 0.4362(5) 0.079(4) Uani 1 1 d . . .
H6H H 0.5190 -0.1675 0.4715 0.095 Uiso 1 1 d R . .
C7H C 0.5713(15) -0.1029(7) 0.3702(7) 0.102(5) Uani 1 1 d . . .
O7H O 0.6409(14) -0.1567(6) 0.3572(5) 0.157(6) Uani 1 1 d . . .
N8H N 0.5524(13) -0.0285(6) 0.3164(5) 0.105(4) Uani 1 1 d . . .
C8AH C 0.4841(10) 0.0210(6) 0.3313(6) 0.067(3) Uani 1 1 d . . .
N1N N 0.0995(8) 0.3326(5) 0.0455(4) 0.0512(18) Uani 1 1 d . . .
O1N O 0.1764(5) 0.3479(4) 0.0752(3) 0.0562(17) Uani 1 1 d . . .
O2N O 0.0538(7) 0.3865(4) -0.0028(3) 0.067(2) Uani 1 1 d . . .
O3N O 0.0576(13) 0.2636(5) 0.0672(6) 0.144(5) Uani 1 1 d . . .
N2N N 0.7821(12) 0.5181(10) 0.2408(9) 0.117(5) Uani 1 1 d . . .
O4N O 0.7275(8) 0.5163(7) 0.1997(5) 0.102(4) Uani 1 1 d . . .
O5N O 0.7869(9) 0.4666(9) 0.3015(6) 0.121(4) Uani 1 1 d . . .
O6N O 0.8573(10) 0.5786(7) 0.2281(6) 0.120(4) Uani 1 1 d . . .
N3N N 0.212(2) 0.0330(12) 0.5713(9) 0.293(14) Uiso 1 1 d D . .
O7N O 0.1538(9) 0.0943(6) 0.5326(5) 0.104(3) Uiso 1 1 d D . .
O8N O 0.2754(13) -0.0151(8) 0.5510(8) 0.183(6) Uiso 1 1 d D . .
O9N O 0.241(2) 0.0377(12) 0.6255(8) 0.288(11) Uiso 1 1 d D . .
N4N N 0.3933(12) 0.6489(8) 0.4796(7) 0.128(5) Uiso 1 1 d D . .
O10N O 0.3369(11) 0.6339(8) 0.4384(6) 0.144(5) Uiso 1 1 d D . .
O11N O 0.4705(12) 0.6000(8) 0.5152(7) 0.159(5) Uiso 1 1 d D . .
O12N O 0.431(3) 0.7213(9) 0.4536(16) 0.49(2) Uiso 1 1 d D . .
O1W O 0.0710(6) 0.0661(4) 0.4221(3) 0.0558(16) Uani 1 1 d . . .
O2W O 0.0720(7) 0.1457(5) 0.2008(4) 0.077(2) Uani 1 1 d . . .
O3W O 0.803(3) 0.281(2) 0.0051(18) 0.078(9) Uiso 0.25 1 d P . .
O3W' O 0.8110(10) 0.3028(7) 0.0274(6) 0.077(3) Uiso 0.75 1 d P . .
O4W O 0.9252(17) 0.6693(12) 0.1186(10) 0.086(5) Uiso 0.50 1 d P . .
O4W' O 0.9498(11) 0.7027(8) 0.0929(7) 0.044(3) Uiso 0.50 1 d P . .
O5W O 0.6108(12) 0.3426(8) 0.3390(7) 0.104(4) Uiso 0.75 1 d P . .
O5W' O 0.546(3) 0.294(2) 0.3976(17) 0.080(9) Uiso 0.25 1 d P . .
O6W O 0.7881(11) 0.7623(7) 0.4521(6) 0.050(3) Uiso 0.50 1 d P . .
O7W O 0.3310(13) 0.8133(8) 0.0087(7) 0.063(4) Uiso 0.50 1 d P . .
O8W O 0.5951(17) 0.0290(11) 0.0067(9) 0.095(5) Uiso 0.50 1 d P . .
O9W O 0.5114(18) -0.0808(12) 0.1418(10) 0.105(6) Uiso 0.50 1 d P . .
O10W O 0.373(2) 0.3083(14) 0.4625(12) 0.130(8) Uiso 0.50 1 d P . .
O11W O 0.420(3) 0.7945(16) 0.3309(14) 0.154(10) Uiso 0.50 1 d P . .
