#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:26:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179328 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/25/4322556.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_4322556
loop_
_publ_author_name
'Elisa Campazzi'
'Euro Solari'
'Rosario Scopelliti'
'Carlo Floriani'
_publ_contact_author_address
;
Institut de Chimie Minérale et Analytique
BCH # 3307
Université de Lausanne
CH-1015 Lausanne
Switzerland
;
_publ_contact_author_email       carlo.floriani@icma.unil.ch
_publ_contact_author_fax         '+4121 692 3905'
_publ_contact_author_name        'Carlo Floriani'
_publ_contact_author_phone       '+4121 692 3902'
_publ_section_title
;
 Cyclopentadienyl Behavior of Pyrrolyl Anions within the
 meso-Octaethylporphyrinogen-Binding Lanthanides: Carbon-Hydrogen and
 Metal-Carbon Bond Rearrangements
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6240
_journal_page_last               6245
_journal_paper_doi               10.1021/ic990742x
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C92 H140 N8 Na2 Nd2 O10'
_chemical_formula_weight         1852.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 108.11(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.236(2)
_cell_length_b                   13.460(2)
_cell_length_c                   21.626(6)
_cell_measurement_reflns_used    '589 spots from first image'
_cell_measurement_temperature    143(2)
_cell_volume                     4491.9(16)
_computing_cell_refinement       'marresearch, marHKL, release 1.9.1'
_computing_data_collection       'marresearch, mar345, release 1.2.11'
_computing_data_reduction        'marresearch, marHKL'
_computing_molecular_graphics    'Bruker, SHELXTL, release 5.1'
_computing_publication_material  'Bruker, SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_max 0.652
_diffrn_measurement_device_type  'mar345 IPDS'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            9832
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    1.214
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1940
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       0.0078(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         5168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0407
_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)+(0.0913P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1304
_reflns_number_gt                4384
_reflns_number_total             5168
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990742x_4.cif
_cod_data_source_block           14
_cod_original_cell_volume        4491.9(15)
_cod_database_code               4322556
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_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
Nd1 Nd -0.336006(16) -0.106503(15) -0.184427(11) 0.02310(17) Uani 1 1 d . . .
N1 N -0.3489(3) -0.1198(2) -0.0712(2) 0.0258(9) Uani 1 1 d . . .
N2 N -0.2459(3) -0.2672(3) -0.12671(19) 0.0267(9) Uani 1 1 d . . .
N3 N -0.2043(3) -0.0852(3) -0.21656(19) 0.0254(9) Uani 1 1 d . . .
N4 N -0.2691(3) 0.0688(3) -0.13879(19) 0.0257(9) Uani 1 1 d . . .
C1 C -0.3238(3) -0.0440(3) -0.0264(2) 0.0261(10) Uani 1 1 d . . .
C2 C -0.2935(4) -0.0833(4) 0.0364(2) 0.0320(11) Uani 1 1 d . . .
H2 H -0.2707 -0.0470 0.0757 0.038 Uiso 1 1 calc R . .
C3 C -0.3036(4) -0.1878(3) 0.0303(2) 0.0324(11) Uani 1 1 d . . .
H3 H -0.2898 -0.2350 0.0647 0.039 Uiso 1 1 calc R . .
C4 C -0.3376(3) -0.2076(3) -0.0358(2) 0.0296(11) Uani 1 1 d . . .
C5 C -0.3556(3) -0.3062(3) -0.0709(2) 0.0267(10) Uani 1 1 d . . .
C6 C -0.3300(3) -0.2957(3) -0.1325(2) 0.0258(10) Uani 1 1 d . . .
C7 C -0.3748(4) -0.3200(3) -0.1966(2) 0.0317(11) Uani 1 1 d . . .
H7 H -0.4334 -0.3412 -0.2132 0.038 Uiso 1 1 calc R . .
C8 C -0.3154(4) -0.3068(3) -0.2323(2) 0.0316(12) Uani 1 1 d . . .
H8 H -0.3271 -0.3160 -0.2777 0.038 Uiso 1 1 calc R . .
C9 C -0.2369(3) -0.2779(3) -0.1878(2) 0.0282(11) Uani 1 1 d . . .
C10 C -0.1495(3) -0.2617(3) -0.1989(2) 0.0267(10) Uani 1 1 d . . .
C11 C -0.1404(3) -0.1541(3) -0.2155(2) 0.0283(11) Uani 1 1 d . . .
C12 C -0.0732(4) -0.1075(3) -0.2311(3) 0.0369(14) Uani 1 1 d . . .
H12 H -0.0218 -0.1381 -0.2339 0.044 Uiso 1 1 calc R . .
C13 C -0.0955(3) -0.0065(3) -0.2420(2) 0.0322(11) Uani 1 1 d . . .
H13 H -0.0615 0.0440 -0.2529 0.039 Uiso 1 1 calc R . .
C14 C -0.1763(3) 0.0053(3) -0.2339(2) 0.0266(10) Uani 1 1 d . . .
C15 C -0.2304(4) 0.0977(3) -0.2418(2) 0.0273(11) Uani 1 1 d . . .
C16 C -0.2968(3) 0.0861(3) -0.2054(2) 0.0249(10) Uani 1 1 d . . .
C17 C -0.3863(4) 0.0940(3) -0.2291(3) 0.0276(11) Uani 1 1 d . . .
H17 H -0.4207 0.1040 -0.2731 0.033 Uiso 1 1 calc R . .
C18 C -0.4164(4) 0.0839(3) -0.1737(2) 0.0286(11) Uani 1 1 d . . .
H18 H -0.4749 0.0859 -0.1736 0.034 Uiso 1 1 calc R . .
C19 C -0.3434(3) 0.0708(3) -0.1206(2) 0.0262(11) Uani 1 1 d . . .
C20 C -0.3363(3) 0.0639(3) -0.0480(2) 0.0272(11) Uani 1 1 d . . .
C21 C -0.4536(3) -0.3332(3) -0.0902(2) 0.0322(11) Uani 1 1 d . . .
H21A H -0.4875 -0.2770 -0.1151 0.039 Uiso 1 1 calc R . .
H21B H -0.4642 -0.3915 -0.1195 0.039 Uiso 1 1 calc R . .
C22 C -0.4877(4) -0.3568(4) -0.0336(3) 0.0396(13) Uani 1 1 d . . .
H22A H -0.4597 -0.4171 -0.0116 0.059 Uiso 1 1 calc R . .
H22B H -0.5505 -0.3671 -0.0502 0.059 Uiso 1 1 calc R . .
H22C H -0.4749 -0.3012 -0.0028 0.059 Uiso 1 1 calc R . .
C23 C -0.2994(4) -0.3884(3) -0.0283(3) 0.0316(12) Uani 1 1 d . . .
H23A H -0.2380 -0.3679 -0.0169 0.038 Uiso 1 1 calc R . .
H23B H -0.3141 -0.3923 0.0128 0.038 Uiso 1 1 calc R . .
C24 C -0.3079(4) -0.4916(4) -0.0577(3) 0.0447(14) Uani 1 1 d . . .
H24A H -0.3672 -0.5158 -0.0657 0.067 Uiso 1 1 calc R . .
H24B H -0.2673 -0.5367 -0.0275 0.067 Uiso 1 1 calc R . .
H24C H -0.2945 -0.4892 -0.0988 0.067 Uiso 1 1 calc R . .
C25 C -0.0788(4) -0.2931(4) -0.1355(2) 0.0356(12) Uani 1 1 d . . .
H25A H -0.0823 -0.2478 -0.1003 0.043 Uiso 1 1 calc R . .
H25B H -0.0930 -0.3607 -0.1239 0.043 Uiso 1 1 calc R . .
C26 C 0.0149(4) -0.2938(4) -0.1362(3) 0.0419(13) Uani 1 1 d . . .
H26A H 0.0194 -0.3350 -0.1724 0.063 Uiso 1 1 calc R . .
H26B H 0.0524 -0.3211 -0.0951 0.063 Uiso 1 1 calc R . .
H26C H 0.0331 -0.2258 -0.1416 0.063 Uiso 1 1 calc R . .
C27 C -0.1448(4) -0.3275(3) -0.2567(2) 0.0346(12) Uani 1 1 d . . .
H27A H -0.1929 -0.3082 -0.2957 0.042 Uiso 1 1 calc R . .
H27B H -0.0900 -0.3121 -0.2657 0.042 Uiso 1 1 calc R . .
C28 C -0.1491(4) -0.4390(4) -0.2478(3) 0.0467(15) Uani 1 1 d . . .
H28A H -0.1004 -0.4601 -0.2105 0.070 Uiso 1 1 calc R . .
H28B H -0.1460 -0.4729 -0.2871 0.070 Uiso 1 1 calc R . .
H28C H -0.2038 -0.4560 -0.2401 0.070 Uiso 1 1 calc R . .
C29 C -0.1708(4) 0.1874(3) -0.2139(3) 0.0346(12) Uani 1 1 d . . .
H29A H -0.1381 0.1728 -0.1679 0.042 Uiso 1 1 calc R . .
H29B H -0.1281 0.1932 -0.2379 0.042 Uiso 1 1 calc R . .
C30 C -0.2147(4) 0.2870(4) -0.2164(3) 0.0447(14) Uani 1 1 d . . .
H30A H -0.2367 0.3097 -0.2616 0.067 Uiso 1 1 calc R . .
H30B H -0.1729 0.3354 -0.1906 0.067 Uiso 1 1 calc R . .
H30C H -0.2630 0.2805 -0.1985 0.067 Uiso 1 1 calc R . .
C31 C -0.2840(4) 0.1165(3) -0.3156(3) 0.0327(12) Uani 1 1 d . . .
H31A H -0.3237 0.0597 -0.3314 0.039 Uiso 1 1 calc R . .
H31B H -0.3201 0.1766 -0.3183 0.039 Uiso 1 1 calc R . .
C32 C -0.2285(4) 0.1301(5) -0.3612(3) 0.0538(16) Uani 1 1 d . . .
H32A H -0.1915 0.1887 -0.3478 0.081 Uiso 1 1 calc R . .
H32B H -0.2665 0.1390 -0.4060 0.081 Uiso 1 1 calc R . .
H32C H -0.1922 0.0711 -0.3589 0.081 Uiso 1 1 calc R . .
C33 C -0.2595(4) 0.1276(3) -0.0080(2) 0.0309(11) Uani 1 1 d . . .
H33A H -0.2548 0.1213 0.0386 0.037 Uiso 1 1 calc R . .
H33B H -0.2056 0.1004 -0.0136 0.037 Uiso 1 1 calc R . .
C34 C -0.2655(4) 0.2371(3) -0.0256(3) 0.0393(13) Uani 1 1 d . . .
H34A H -0.2691 0.2446 -0.0715 0.059 Uiso 1 1 calc R . .
H34B H -0.2139 0.2716 0.0017 0.059 Uiso 1 1 calc R . .
H34C H -0.3173 0.2657 -0.0186 0.059 Uiso 1 1 calc R . .
C35 C -0.4244(4) 0.1019(3) -0.0420(3) 0.0309(13) Uani 1 1 d . . .
H35A H -0.4363 0.1687 -0.0621 0.037 Uiso 1 1 calc R . .
H35B H -0.4711 0.0570 -0.0671 0.037 Uiso 1 1 calc R . .
C36 C -0.4277(4) 0.1084(3) 0.0286(3) 0.0411(15) Uani 1 1 d . . .
H36A H -0.4114 0.0441 0.0502 0.062 Uiso 1 1 calc R . .
H36B H -0.4866 0.1256 0.0280 0.062 Uiso 1 1 calc R . .
H36C H -0.3872 0.1596 0.0524 0.062 Uiso 1 1 calc R . .
Na1 Na -0.17466(13) -0.17996(13) -0.02406(9) 0.0324(5) Uani 1 1 d . . .
C37 C -0.5581(4) -0.1052(3) -0.1890(3) 0.0368(14) Uani 1 1 d . . .
H37A H -0.5872 -0.0415 -0.2027 0.055 Uiso 1 1 calc R . .
H37B H -0.5233 -0.1015 -0.1431 0.055 Uiso 1 1 calc R . .
H37C H -0.6016 -0.1578 -0.1948 0.055 Uiso 1 1 calc R . .
O1 O -0.5029(2) -0.1270(2) -0.22771(16) 0.0302(8) Uani 1 1 d . . .
C38 C -0.5482(4) -0.1117(3) -0.2956(3) 0.0363(13) Uani 1 1 d . . .
H38A H -0.5572 -0.0398 -0.3050 0.044 Uiso 1 1 calc R . .
H38B H -0.6056 -0.1447 -0.3077 0.044 Uiso 1 1 calc R . .
C39 C -0.4933(4) -0.1558(4) -0.3336(3) 0.0384(12) Uani 1 1 d . . .
H39A H -0.4905 -0.2289 -0.3283 0.046 Uiso 1 1 calc R . .
H39B H -0.5191 -0.1405 -0.3804 0.046 Uiso 1 1 calc R . .
O2 O -0.4085(3) -0.1149(2) -0.31015(17) 0.0336(9) Uani 1 1 d . . .
C40 C -0.3600(4) -0.1368(4) -0.3542(3) 0.0432(13) Uani 1 1 d . . .
H40A H -0.3669 -0.2072 -0.3662 0.065 Uiso 1 1 calc R . .
H40B H -0.2986 -0.1222 -0.3329 0.065 Uiso 1 1 calc R . .
H40C H -0.3817 -0.0959 -0.3934 0.065 Uiso 1 1 calc R . .
O3 O -0.0673(3) -0.2674(2) 0.05207(18) 0.0415(9) Uani 1 1 d . . .
C41 C 0.0200(4) -0.2788(4) 0.0472(3) 0.0435(13) Uani 1 1 d . . .
H41A H 0.0634 -0.2538 0.0872 0.052 Uiso 1 1 calc R . .
H41B H 0.0257 -0.2404 0.0097 0.052 Uiso 1 1 calc R . .
C42 C 0.0347(5) -0.3863(3) 0.0385(3) 0.0406(15) Uani 1 1 d . . .
H42A H -0.0089 -0.4102 -0.0018 0.049 Uiso 1 1 calc R . .
H42B H 0.0927 -0.3953 0.0333 0.049 Uiso 1 1 calc R . .
O4 O 0.0292(3) -0.4435(3) 0.09116(18) 0.0457(10) Uani 1 1 d . . .
C43 C -0.0550(5) -0.4316(4) 0.0986(3) 0.0499(16) Uani 1 1 d . . .
H43A H -0.0579 -0.4696 0.1371 0.060 Uiso 1 1 calc R . .
H43B H -0.0995 -0.4584 0.0598 0.060 Uiso 1 1 calc R . .
C44 C -0.0734(4) -0.3239(4) 0.1070(3) 0.0483(15) Uani 1 1 d . . .
H44A H -0.1322 -0.3168 0.1109 0.058 Uiso 1 1 calc R . .
H44B H -0.0312 -0.2980 0.1474 0.058 Uiso 1 1 calc R . .
O5 O -0.0745(3) -0.0596(2) -0.01218(16) 0.0366(8) Uani 1 1 d . . .
C45 C -0.0603(4) 0.0004(3) -0.0633(2) 0.0334(11) Uani 1 1 d . . .
H45A H -0.0887 0.0658 -0.0649 0.040 Uiso 1 1 calc R . .
H45B H -0.0858 -0.0327 -0.1059 0.040 Uiso 1 1 calc R . .
C46 C -0.0358(4) -0.0141(4) 0.0501(2) 0.0346(12) Uani 1 1 d . . .
H46A H -0.0461 -0.0563 0.0844 0.042 Uiso 1 1 calc R . .
H46B H -0.0633 0.0512 0.0512 0.042 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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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
N3 Nd1 N1 128.51(14) . . ?
N3 Nd1 O1 144.35(12) . . ?
N1 Nd1 O1 87.13(12) . . ?
N3 Nd1 O2 81.99(13) . . ?
N1 Nd1 O2 149.36(14) . . ?
O1 Nd1 O2 62.40(11) . . ?
N3 Nd1 N4 73.17(12) . . ?
N1 Nd1 N4 81.42(11) . . ?
O1 Nd1 N4 119.33(11) . . ?
O2 Nd1 N4 115.18(11) . . ?
N3 Nd1 N2 80.21(12) . . ?
N1 Nd1 N2 71.99(11) . . ?
O1 Nd1 N2 116.00(11) . . ?
O2 Nd1 N2 116.92(10) . . ?
N4 Nd1 N2 116.18(13) . . ?
N3 Nd1 C16 64.92(13) . . ?
N1 Nd1 C16 108.72(12) . . ?
O1 Nd1 C16 108.16(14) . . ?
O2 Nd1 C16 85.46(13) . . ?
N4 Nd1 C16 29.77(13) . . ?
N2 Nd1 C16 135.76(15) . . ?
N3 Nd1 C6 107.29(13) . . ?
N1 Nd1 C6 62.98(11) . . ?
O1 Nd1 C6 87.10(13) . . ?
O2 Nd1 C6 109.28(12) . . ?
N4 Nd1 C6 134.97(14) . . ?
N2 Nd1 C6 29.34(13) . . ?
C16 Nd1 C6 162.77(16) . . ?
N3 Nd1 C19 102.45(13) . . ?
N1 Nd1 C19 63.28(11) . . ?
O1 Nd1 C19 93.97(12) . . ?
O2 Nd1 C19 118.67(12) . . ?
N4 Nd1 C19 29.33(12) . . ?
N2 Nd1 C19 124.16(13) . . ?
C16 Nd1 C19 46.98(12) . . ?
C6 Nd1 C19 126.12(12) . . ?
N3 Nd1 C9 62.37(12) . . ?
N1 Nd1 C9 100.77(12) . . ?
O1 Nd1 C9 116.33(13) . . ?
O2 Nd1 C9 90.78(12) . . ?
N4 Nd1 C9 124.34(14) . . ?
N2 Nd1 C9 28.87(11) . . ?
C16 Nd1 C9 127.16(13) . . ?
C6 Nd1 C9 46.57(12) . . ?
C19 Nd1 C9 145.78(15) . . ?
N3 Nd1 C17 88.67(13) . . ?
N1 Nd1 C17 106.82(12) . . ?
O1 Nd1 C17 79.87(13) . . ?
O2 Nd1 C17 72.74(13) . . ?
N4 Nd1 C17 48.46(15) . . ?
N2 Nd1 C17 163.69(15) . . ?
C16 Nd1 C17 28.31(16) . . ?
C6 Nd1 C17 164.03(13) . . ?
C19 Nd1 C17 46.70(14) . . ?
C9 Nd1 C17 148.78(12) . . ?
N3 Nd1 C18 111.67(13) . . ?
N1 Nd1 C18 79.13(12) . . ?
O1 Nd1 C18 71.28(13) . . ?
O2 Nd1 C18 93.02(12) . . ?
N4 Nd1 C18 48.06(14) . . ?
N2 Nd1 C18 149.47(12) . . ?
C16 Nd1 C18 46.77(13) . . ?
C6 Nd1 C18 137.29(12) . . ?
C19 Nd1 C18 27.93(15) . . ?
C9 Nd1 C18 172.40(15) . . ?
C17 Nd1 C18 28.55(12) . . ?
C1 N1 C4 106.4(4) . . ?
C1 N1 Nd1 122.2(2) . . ?
C4 N1 Nd1 123.9(3) . . ?
C1 N1 Na1 85.0(3) . . ?
C4 N1 Na1 67.0(3) . . ?
Nd1 N1 Na1 89.69(12) . . ?
C9 N2 C6 106.2(4) . . ?
C9 N2 Na1 138.8(3) . . ?
C6 N2 Na1 112.8(3) . . ?
C9 N2 Nd1 81.0(3) . . ?
C6 N2 Nd1 78.5(3) . . ?
Na1 N2 Nd1 94.01(12) . . ?
C11 N3 C14 106.5(4) . . ?
C11 N3 Nd1 129.0(3) . . ?
C14 N3 Nd1 124.3(3) . . ?
C19 N4 C16 105.2(4) . . ?
C19 N4 Nd1 80.2(3) . . ?
C16 N4 Nd1 78.4(3) . . ?
N1 C1 C2 109.9(4) . . ?
N1 C1 C20 120.6(4) . . ?
C2 C1 C20 129.3(4) . . ?
N1 C1 Na1 68.0(3) . . ?
C2 C1 Na1 73.6(3) . . ?
C20 C1 Na1 127.8(3) . . ?
C1 C2 C3 106.9(4) . . ?
C1 C2 Na1 79.4(2) . . ?
C3 C2 Na1 66.0(2) . . ?
C4 C3 C2 106.5(4) . . ?
C4 C3 Na1 70.9(3) . . ?
C2 C3 Na1 85.4(3) . . ?
N1 C4 C3 110.2(4) . . ?
N1 C4 C5 119.9(4) . . ?
C3 C4 C5 129.7(4) . . ?
N1 C4 Na1 83.6(3) . . ?
C3 C4 Na1 78.8(3) . . ?
C5 C4 Na1 102.0(3) . . ?
C4 C5 C6 107.1(3) . . ?
C4 C5 C23 110.1(4) . . ?
C6 C5 C23 108.6(4) . . ?
C4 C5 C21 111.2(4) . . ?
C6 C5 C21 108.8(4) . . ?
C23 C5 C21 111.0(4) . . ?
N2 C6 C7 110.6(4) . . ?
N2 C6 C5 118.4(4) . . ?
C7 C6 C5 130.6(4) . . ?
N2 C6 Nd1 72.1(2) . . ?
C7 C6 Nd1 82.6(3) . . ?
C5 C6 Nd1 117.1(3) . . ?
C6 C7 C8 106.2(5) . . ?
C6 C7 Nd1 69.4(3) . . ?
C8 C7 Nd1 76.3(3) . . ?
C9 C8 C7 106.9(4) . . ?
C9 C8 Nd1 71.4(2) . . ?
C7 C8 Nd1 75.7(2) . . ?
N2 C9 C8 110.0(4) . . ?
N2 C9 C10 121.0(5) . . ?
C8 C9 C10 128.9(4) . . ?
N2 C9 Nd1 70.1(2) . . ?
C8 C9 Nd1 80.8(3) . . ?
C10 C9 Nd1 116.9(3) . . ?
C11 C10 C9 109.8(4) . . ?
C11 C10 C25 111.8(4) . . ?
C9 C10 C25 107.0(3) . . ?
C11 C10 C27 108.8(3) . . ?
C9 C10 C27 109.0(4) . . ?
C25 C10 C27 110.4(4) . . ?
C12 C11 N3 109.6(4) . . ?
C12 C11 C10 129.3(4) . . ?
N3 C11 C10 121.1(4) . . ?
C11 C12 C13 107.3(4) . . ?
C14 C13 C12 107.0(4) . . ?
C13 C14 N3 109.6(4) . . ?
C13 C14 C15 128.6(4) . . ?
N3 C14 C15 121.8(4) . . ?
C14 C15 C16 109.7(3) . . ?
C14 C15 C29 109.2(5) . . ?
C16 C15 C29 109.6(4) . . ?
C14 C15 C31 111.5(4) . . ?
C16 C15 C31 106.3(4) . . ?
C29 C15 C31 110.4(4) . . ?
C17 C16 N4 111.2(4) . . ?
C17 C16 C15 128.9(4) . . ?
N4 C16 C15 119.9(5) . . ?
C17 C16 Nd1 82.1(3) . . ?
N4 C16 Nd1 71.8(3) . . ?
C15 C16 Nd1 114.8(3) . . ?
C16 C17 C18 105.9(5) . . ?
C16 C17 Nd1 69.6(3) . . ?
C18 C17 Nd1 76.6(3) . . ?
C19 C18 C17 106.2(4) . . ?
C19 C18 Nd1 70.4(3) . . ?
C17 C18 Nd1 74.9(2) . . ?
N4 C19 C18 111.5(4) . . ?
N4 C19 C20 119.5(5) . . ?
C18 C19 C20 128.9(4) . . ?
N4 C19 Nd1 70.5(2) . . ?
C18 C19 Nd1 81.7(3) . . ?
C20 C19 Nd1 116.9(3) . . ?
C1 C20 C33 110.6(4) . . ?
C1 C20 C19 109.4(3) . . ?
C33 C20 C19 109.3(3) . . ?
C1 C20 C35 109.0(3) . . ?
C33 C20 C35 111.9(4) . . ?
C19 C20 C35 106.5(4) . . ?
C22 C21 C5 115.4(4) . . ?
C24 C23 C5 116.5(5) . . ?
C26 C25 C10 117.4(4) . . ?
C28 C27 C10 116.5(4) . . ?
C30 C29 C15 116.6(5) . . ?
C32 C31 C15 114.6(5) . . ?
C34 C33 C20 115.0(5) . . ?
C36 C35 C20 114.4(5) . . ?
O5 Na1 O3 85.83(15) . . ?
O5 Na1 N2 124.52(13) . . ?
O3 Na1 N2 115.98(14) . . ?
O5 Na1 C4 142.12(16) . . ?
O3 Na1 C4 120.97(15) . . ?
N2 Na1 C4 70.43(14) . . ?
O5 Na1 C3 127.41(14) . . ?
O3 Na1 C3 100.64(15) . . ?
N2 Na1 C3 99.42(16) . . ?
C4 Na1 C3 30.30(16) . . ?
O5 Na1 N1 116.34(14) . . ?
O3 Na1 N1 148.80(13) . . ?
N2 Na1 N1 70.87(13) . . ?
C4 Na1 N1 29.40(13) . . ?
C3 Na1 N1 48.79(14) . . ?
O5 Na1 C2 100.43(14) . . ?
O3 Na1 C2 111.18(14) . . ?
N2 Na1 C2 114.96(16) . . ?
C4 Na1 C2 47.28(15) . . ?
C3 Na1 C2 28.61(13) . . ?
N1 Na1 C2 46.40(14) . . ?
O5 Na1 C1 96.46(14) . . ?
O3 Na1 C1 137.96(13) . . ?
N2 Na1 C1 97.15(15) . . ?
C4 Na1 C1 45.66(13) . . ?
C3 Na1 C1 46.09(13) . . ?
N1 Na1 C1 27.03(12) . . ?
C2 Na1 C1 27.03(13) . . ?
O5 Na1 Nd1 100.77(11) . . ?
O3 Na1 Nd1 160.45(10) . . ?
N2 Na1 Nd1 45.40(10) . . ?
C4 Na1 Nd1 63.48(11) . . ?
C3 Na1 Nd1 89.99(13) . . ?
N1 Na1 Nd1 42.09(8) . . ?
C2 Na1 Nd1 85.92(12) . . ?
C1 Na1 Nd1 60.12(9) . . ?
C37 O1 C38 110.6(4) . . ?
C37 O1 Nd1 122.7(3) . . ?
C38 O1 Nd1 120.0(3) . . ?
O1 C38 C39 107.3(4) . . ?
O2 C39 C38 108.9(4) . . ?
C39 O2 C40 110.6(4) . . ?
C39 O2 Nd1 117.5(3) . . ?
C40 O2 Nd1 122.4(3) . . ?
C44 O3 C41 108.7(4) . . ?
C44 O3 Na1 128.8(3) . . ?
C41 O3 Na1 122.4(3) . . ?
O3 C41 C42 108.0(5) . . ?
O4 C42 C41 112.2(4) . . ?
C42 O4 C43 109.5(5) . . ?
O4 C43 C44 110.7(5) . . ?
O3 C44 C43 110.0(4) . . ?
C46 O5 C45 110.6(3) . . ?
C46 O5 Na1 120.3(2) . . ?
C45 O5 Na1 126.6(3) . . ?
O5 C45 C46 109.0(4) . 3 ?
O5 C46 C45 110.9(4) . 3 ?
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
Nd1 N3 2.461(4) . ?
Nd1 N1 2.527(4) . ?
Nd1 O1 2.592(4) . ?
Nd1 O2 2.608(4) . ?
Nd1 N4 2.657(4) . ?
Nd1 N2 2.691(4) . ?
Nd1 C16 2.740(5) . ?
Nd1 C6 2.772(4) . ?
Nd1 C19 2.778(4) . ?
Nd1 C9 2.827(4) . ?
Nd1 C17 2.897(5) . ?
Nd1 C18 2.919(5) . ?
N1 C1 1.379(6) . ?
N1 C4 1.389(6) . ?
N1 Na1 2.812(5) . ?
N2 C9 1.382(5) . ?
N2 C6 1.386(6) . ?
N2 Na1 2.460(4) . ?
N3 C11 1.387(6) . ?
N3 C14 1.391(6) . ?
N4 C19 1.381(6) . ?
N4 C16 1.389(6) . ?
C1 C2 1.397(7) . ?
C1 C20 1.520(6) . ?
C1 Na1 3.022(5) . ?
C2 C3 1.417(6) . ?
C2 Na1 2.949(5) . ?
C3 C4 1.390(7) . ?
C3 Na1 2.703(4) . ?
C4 C5 1.511(6) . ?
C4 Na1 2.604(5) . ?
C5 C6 1.521(5) . ?
C5 C23 1.543(7) . ?
C5 C21 1.558(7) . ?
C6 C7 1.389(7) . ?
C7 C8 1.421(6) . ?
C8 C9 1.393(8) . ?
C9 C10 1.525(6) . ?
C10 C11 1.511(6) . ?
C10 C25 1.548(7) . ?
C10 C27 1.553(6) . ?
C11 C12 1.387(7) . ?
C12 C13 1.408(6) . ?
C13 C14 1.387(7) . ?
C14 C15 1.501(6) . ?
C15 C16 1.527(6) . ?
C15 C29 1.548(7) . ?
C15 C31 1.584(7) . ?
C16 C17 1.387(8) . ?
C17 C18 1.434(6) . ?
C18 C19 1.382(8) . ?
C19 C20 1.541(6) . ?
C20 C33 1.539(7) . ?
C20 C35 1.562(7) . ?
C21 C22 1.524(5) . ?
C23 C24 1.517(6) . ?
C25 C26 1.525(7) . ?
C27 C28 1.517(7) . ?
C29 C30 1.511(7) . ?
C31 C32 1.539(6) . ?
C33 C34 1.518(6) . ?
C35 C36 1.548(7) . ?
Na1 O5 2.252(4) . ?
Na1 O3 2.313(4) . ?
C37 O1 1.435(5) . ?
O1 C38 1.438(7) . ?
C38 C39 1.510(7) . ?
C39 O2 1.422(7) . ?
O2 C40 1.442(5) . ?
O3 C44 1.439(6) . ?
O3 C41 1.461(7) . ?
C41 C42 1.488(7) . ?
C42 O4 1.400(6) . ?
O4 C43 1.434(7) . ?
C43 C44 1.503(8) . ?
O5 C46 1.434(6) . ?
O5 C45 1.445(5) . ?
C45 C46 1.509(7) 3 ?
C46 C45 1.509(7) 3 ?
