#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:50:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179131 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/93/4309362.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_4309362
loop_
_publ_author_name
'Alexander Jagst'
'Agustin Sánchez'
'Ezequiel M. Vázquez-López'
'Ulrich Abram'
_publ_contact_author
;
      Ulrich Abram
      Free University of Berlin     
      Institute of Chemistry             
      Fabeckstrasse 34-36                     
      D-14195 Berlin         
      Germany                          
;
_publ_contact_author_email       abram@chemie.fu-berlin.de
_publ_contact_author_fax         '0049 (0)30 838 52676'
_publ_contact_author_phone       '0049 (0)30 838 54002'
_publ_section_title
;
Controlled Ligand Deprotonation in Lanthanide Chelates with Asymmetric
Semicarbazone/Benzoylhydrazone or Semicarbazone/Thiosemicarbazone
Coordination Spheres
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5738
_journal_page_last               5744
_journal_paper_doi               10.1021/ic050556t
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         '[Sm(HDFPSCPTSC)2]Cl*H2O'
_chemical_formula_sum            'C42 H36 N15 O6 S2 Sm'
_chemical_formula_weight         1061.33
_chemical_name_common            '[Sm(HDFPSCPTSC)2]Cl*H2O'
_chemical_name_systematic
;
Bis(2,6-diformylpyridine-4-phenylsemicarbazone-4-phenylthiosemicarbazonato)-
samarium(III) nitrate water solvate
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   49.76(5)
_cell_length_b                   49.76(5)
_cell_length_c                   13.85(3)
_cell_measurement_reflns_used    916
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      41.588
_cell_measurement_theta_min      2.250
_cell_volume                     29699(8)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker Smart'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'ccd area detector'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0943
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11364
_diffrn_reflns_theta_full        24.87
_diffrn_reflns_theta_max         24.87
_diffrn_reflns_theta_min         1.42
_diffrn_standards_interval_time  '20sec / frame'
_exptl_absorpt_coefficient_mu    0.997
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             9630
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.285
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         11364
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1261
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1069P)²+49.3899P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1894
_reflns_number_gt                6888
_reflns_number_total             11364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050556tsi20050411_050949_3.cif
_cod_data_source_block           ajl21z
_cod_original_cell_volume        29706(80)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4309362
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Sm Sm 0.319231(10) 0.104456(9) 0.90264(3) 0.03889(15) Uani 1 1 d . . .
N1 N 0.35112(15) 0.07935(15) 0.9794(4) 0.0456(16) Uani 1 1 d . . .
N2 N 0.32509(15) 0.10252(14) 1.0942(4) 0.0396(15) Uani 1 1 d . . .
N3 N 0.31088(15) 0.11516(15) 1.1477(4) 0.0433(16) Uani 1 1 d . . .
H3N H 0.3055 0.1102 1.2084 0.052 Uiso 1 1 calc R . .
N4 N 0.34272(15) 0.07819(15) 0.7830(4) 0.0418(16) Uani 1 1 d . . .
N5 N 0.33987(16) 0.07477(16) 0.6823(4) 0.0453(17) Uani 1 1 d . . .
N6 N 0.29057(16) 0.14755(15) 1.1478(4) 0.0427(16) Uani 1 1 d . . .
H6N H 0.2865 0.1419 1.2087 0.051 Uiso 1 1 calc R . .
N7 N 0.31180(15) 0.07363(15) 0.5478(4) 0.0445(16) Uani 1 1 d . . .
H7 H 0.3007 0.0813 0.5236 0.053 Uiso 1 1 calc R . .
N31 N 0.2852(2) 0.13046(17) 0.8442(4) 0.056(2) Uani 1 1 d . . .
N32 N 0.3470(3) 0.15974(18) 0.8139(5) 0.072(3) Uani 1 1 d . . .
N33 N 0.3792(3) 0.1740(2) 0.8044(7) 0.099(4) Uani 1 1 d . . .
H33N H 0.3900 0.1899 0.7659 0.119 Uiso 1 1 calc R . .
N34 N 0.26055(16) 0.08026(15) 0.9613(5) 0.0494(17) Uani 1 1 d . . .
N35 N 0.24725(17) 0.05713(17) 1.0322(5) 0.0575(19) Uani 1 1 d . . .
N36 N 0.4249(3) 0.1774(3) 0.8585(10) 0.127(5) Uani 1 1 d . . .
H36N H 0.4335 0.1945 0.8237 0.153 Uiso 1 1 calc R . .
N37 N 0.25046(17) 0.01631(15) 1.1032(5) 0.0577(19) Uani 1 1 d . . .
H37N H 0.2544 0.0012 1.0907 0.069 Uiso 1 1 calc R . .
O18 O 0.31548(13) 0.14284(12) 1.0123(3) 0.0470(14) Uani 1 1 d . . .
O48 O 0.37766(17) 0.13803(17) 0.9074(5) 0.076(2) Uani 1 1 d . . .
S28 S 0.29425(5) 0.09004(5) 0.70735(13) 0.0444(5) Uani 1 1 d . . .
S58 S 0.28212(6) 0.03713(5) 0.94152(15) 0.0570(6) Uani 1 1 d . . .
C2 C 0.3657(2) 0.0689(2) 0.9214(6) 0.051(2) Uani 1 1 d . . .
C3 C 0.3845(2) 0.0576(2) 0.9579(6) 0.066(3) Uani 1 1 d . . .
H3A H 0.3950 0.0509 0.9151 0.079 Uiso 1 1 calc R . .
C4 C 0.3877(2) 0.0561(2) 1.0577(7) 0.073(3) Uani 1 1 d . . .
H4 H 0.4004 0.0486 1.0838 0.087 Uiso 1 1 calc R . .
C5 C 0.3719(2) 0.0659(2) 1.1179(6) 0.054(2) Uani 1 1 d . . .
H5 H 0.3731 0.0647 1.1860 0.065 Uiso 1 1 calc R . .
C6 C 0.35422(19) 0.07764(18) 1.0769(5) 0.0440(19) Uani 1 1 d . . .
C7 C 0.3382(2) 0.08900(18) 1.1376(5) 0.046(2) Uani 1 1 d . . .
H7A H 0.3374 0.0866 1.2058 0.055 Uiso 1 1 calc R . .
C9 C 0.3607(2) 0.0692(2) 0.8183(5) 0.051(2) Uani 1 1 d . . .
H9 H 0.3711 0.0625 0.7755 0.062 Uiso 1 1 calc R . .
C11 C 0.2804(2) 0.16765(19) 1.1121(5) 0.048(2) Uani 1 1 d . . .
C12 C 0.2585(2) 0.1705(2) 1.1695(7) 0.066(3) Uani 1 1 d . . .
H12 H 0.2515 0.1594 1.2285 0.079 Uiso 1 1 calc R . .
C13 C 0.2474(3) 0.1893(3) 1.1394(8) 0.085(3) Uani 1 1 d . . .
H13 H 0.2330 0.1915 1.1789 0.102 Uiso 1 1 calc R . .
C14 C 0.2565(3) 0.2053(3) 1.0536(8) 0.086(4) Uani 1 1 d . . .
H14 H 0.2477 0.2174 1.0327 0.103 Uiso 1 1 calc R . .
C15 C 0.2784(3) 0.2034(2) 0.9986(7) 0.066(3) Uani 1 1 d . . .
H15 H 0.2856 0.2151 0.9407 0.079 Uiso 1 1 calc R . .
C16 C 0.2905(2) 0.18426(19) 1.0272(5) 0.053(2) Uani 1 1 d . . .
H16 H 0.3054 0.1828 0.9882 0.063 Uiso 1 1 calc R . .
C17 C 0.30581(19) 0.13625(17) 1.0981(5) 0.0421(19) Uani 1 1 d . . .
C21 C 0.32055(19) 0.05804(17) 0.4811(5) 0.0400(18) Uani 1 1 d . . .
C22 C 0.30344(19) 0.04816(18) 0.3941(5) 0.0439(19) Uani 1 1 d . . .
H22 H 0.2875 0.0530 0.3820 0.053 Uiso 1 1 calc R . .
C23 C 0.3098(2) 0.03146(19) 0.3260(5) 0.049(2) Uani 1 1 d . . .
H23 H 0.2982 0.0251 0.2676 0.059 Uiso 1 1 calc R . .
C24 C 0.3325(2) 0.0241(2) 0.3424(6) 0.056(2) Uani 1 1 d . . .
H24 H 0.3369 0.0128 0.2956 0.067 Uiso 1 1 calc R . .
C25 C 0.3490(2) 0.0333(2) 0.4286(5) 0.056(2) Uani 1 1 d . . .
H25 H 0.3646 0.0280 0.4405 0.068 Uiso 1 1 calc R . .
C26 C 0.34354(19) 0.0498(2) 0.4964(5) 0.050(2) Uani 1 1 d . . .
H26 H 0.3553 0.0559 0.5544 0.060 Uiso 1 1 calc R . .
C27 C 0.31803(19) 0.07880(16) 0.6462(5) 0.0393(18) Uani 1 1 d . . .
C32 C 0.2557(3) 0.1180(2) 0.8676(6) 0.060(3) Uani 1 1 d . . .
C33 C 0.2367(3) 0.1301(3) 0.8375(8) 0.092(4) Uani 1 1 d . . .
H33A H 0.2153 0.1208 0.8541 0.110 Uiso 1 1 calc R . .
C34 C 0.2523(5) 0.1577(4) 0.7797(9) 0.119(6) Uani 1 1 d . . .
H34 H 0.2411 0.1670 0.7546 0.143 Uiso 1 1 calc R . .
C35 C 0.2842(4) 0.1710(3) 0.7603(9) 0.100(5) Uani 1 1 d . . .
H35 H 0.2949 0.1897 0.7241 0.119 Uiso 1 1 calc R . .
C36 C 0.2988(3) 0.1572(2) 0.7932(5) 0.067(3) Uani 1 1 d . . .
C37 C 0.3326(4) 0.1721(2) 0.7792(6) 0.083(4) Uani 1 1 d . . .
H37A H 0.3434 0.1910 0.7442 0.099 Uiso 1 1 calc R . .
C39 C 0.24372(15) 0.09160(17) 0.9339(4) 0.061(2) Uani 1 1 d . . .
H39 H 0.2230 0.0827 0.9570 0.073 Uiso 1 1 calc R . .
C41 C 0.44391(15) 0.16920(17) 0.9043(4) 0.159(7) Uani 1 1 d RU . .
C42 C 0.43697(15) 0.14005(17) 0.9373(4) 0.144(6) Uani 1 1 d RU . .
H42 H 0.4170 0.1226 0.9262 0.172 Uiso 1 1 calc R . .
C43 C 0.45927(15) 0.13641(17) 0.9867(4) 0.195(8) Uani 1 1 d RU . .
H43 H 0.4545 0.1165 1.0093 0.234 Uiso 1 1 calc R . .
C44 C 0.48850(15) 0.16192(17) 1.0030(4) 0.288(15) Uani 1 1 d RU . .
H44 H 0.5037 0.1594 1.0367 0.346 Uiso 1 1 calc R . .
C45 C 0.49544(15) 0.19107(17) 0.9699(4) 0.37(3) Uani 1 1 d RU . .
H45 H 0.5154 0.2085 0.9811 0.446 Uiso 1 1 calc R . .
C46 C 0.47314(15) 0.19471(17) 0.9206(4) 0.294(15) Uani 1 1 d RU . .
H46 H 0.4779 0.2146 0.8980 0.353 Uiso 1 1 calc R . .
C47 C 0.3928(3) 0.1602(4) 0.8638(10) 0.095(4) Uani 1 1 d . . .
C51 C 0.2364(2) 0.0141(2) 1.1939(6) 0.053(2) Uani 1 1 d . . .
C52 C 0.2270(2) -0.0134(2) 1.2453(7) 0.065(3) Uani 1 1 d . . .
H52 H 0.2290 -0.0298 1.2176 0.078 Uiso 1 1 calc R . .
C53 C 0.2147(2) -0.0163(2) 1.3390(8) 0.076(3) Uani 1 1 d . . .
H53 H 0.2086 -0.0349 1.3742 0.091 Uiso 1 1 calc R . .
C54 C 0.2115(3) 0.0066(3) 1.3800(7) 0.090(4) Uani 1 1 d . . .
H54 H 0.2037 0.0045 1.4439 0.108 Uiso 1 1 calc R . .
C55 C 0.2197(3) 0.0332(3) 1.3269(8) 0.083(3) Uani 1 1 d . . .
H55 H 0.2162 0.0488 1.3534 0.099 Uiso 1 1 calc R . .
C56 C 0.2328(2) 0.0375(2) 1.2360(7) 0.067(3) Uani 1 1 d . . .
H56 H 0.2394 0.0564 1.2024 0.081 Uiso 1 1 calc R . .
C57 C 0.2592(2) 0.03855(18) 1.0304(6) 0.050(2) Uani 1 1 d . . .
N61 N 0.27779(19) 0.10684(16) 0.3808(5) 0.0496(18) Uani 1 1 d . . .
O62 O 0.26868(15) 0.09511(15) 0.4637(4) 0.0606(16) Uani 1 1 d . . .
O63 O 0.30284(15) 0.11038(15) 0.3495(4) 0.0601(16) Uani 1 1 d . . .
O64 O 0.26229(16) 0.11505(16) 0.3311(4) 0.0656(18) Uani 1 1 d . . .
O71 O 0.1808(14) 0.0872(11) 0.115(6) 0.51(6) Uani 0.50 1 d P . .
O72 O 0.2199(5) 0.1011(5) 0.5899(17) 0.204(14) Uani 0.50 1 d P . .
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'
Sm Sm -0.1638 3.4418 '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
O18 Sm O48 88.8(2) . . ?
O18 Sm N34 71.3(2) . . ?
O48 Sm N34 158.1(2) . . ?
O18 Sm N2 58.67(19) . . ?
O48 Sm N2 83.6(2) . . ?
N34 Sm N2 78.2(2) . . ?
O18 Sm N32 72.2(2) . . ?
O48 Sm N32 60.1(3) . . ?
N34 Sm N32 119.3(3) . . ?
N2 Sm N32 118.8(2) . . ?
O18 Sm N1 113.5(2) . . ?
O48 Sm N1 62.9(2) . . ?
N34 Sm N1 116.0(2) . . ?
N2 Sm N1 59.31(19) . . ?
N32 Sm N1 122.5(3) . . ?
O18 Sm N4 161.33(19) . . ?
O48 Sm N4 72.8(2) . . ?
N34 Sm N4 127.4(2) . . ?
N2 Sm N4 120.5(2) . . ?
N32 Sm N4 95.1(2) . . ?
N1 Sm N4 61.3(2) . . ?
O18 Sm N31 61.2(2) . . ?
O48 Sm N31 118.5(3) . . ?
N34 Sm N31 60.3(2) . . ?
N2 Sm N31 114.67(19) . . ?
N32 Sm N31 60.0(3) . . ?
N1 Sm N31 173.94(19) . . ?
N4 Sm N31 124.7(2) . . ?
O18 Sm S28 124.23(15) . . ?
O48 Sm S28 113.28(17) . . ?
N34 Sm S28 86.33(18) . . ?
N2 Sm S28 162.28(15) . . ?
N32 Sm S28 76.4(2) . . ?
N1 Sm S28 122.18(14) . . ?
N4 Sm S28 63.09(17) . . ?
N31 Sm S28 63.25(14) . . ?
O18 Sm S58 120.55(14) . . ?
O48 Sm S58 127.19(19) . . ?
N34 Sm S58 60.70(15) . . ?
N2 Sm S58 78.23(14) . . ?
N32 Sm S58 162.95(17) . . ?
N1 Sm S58 65.13(15) . . ?
N4 Sm S58 74.96(15) . . ?
N31 Sm S58 114.13(19) . . ?
S28 Sm S58 86.69(8) . . ?
C2 N1 C6 117.7(7) . . ?
C2 N1 Sm 120.1(5) . . ?
C6 N1 Sm 122.2(5) . . ?
C7 N2 N3 119.7(6) . . ?
C7 N2 Sm 124.8(5) . . ?
N3 N2 Sm 115.3(4) . . ?
N2 N3 C17 114.3(6) . . ?
C9 N4 N5 112.6(6) . . ?
C9 N4 Sm 118.7(5) . . ?
N5 N4 Sm 128.6(5) . . ?
C27 N5 N4 113.9(6) . . ?
C17 N6 C11 126.5(6) . . ?
C27 N7 C21 130.0(7) . . ?
C32 N31 C36 119.0(9) . . ?
C32 N31 Sm 121.0(6) . . ?
C36 N31 Sm 119.9(8) . . ?
C37 N32 N33 120.5(10) . . ?
C37 N32 Sm 123.5(8) . . ?
N33 N32 Sm 116.0(8) . . ?
N32 N33 C47 113.5(9) . . ?
C39 N34 N35 115.2(7) . . ?
C39 N34 Sm 121.4(5) . . ?
N35 N34 Sm 123.0(5) . . ?
C57 N35 N34 111.6(7) . . ?
C41 N36 C47 123.3(13) . . ?
C57 N37 C51 130.3(8) . . ?
C17 O18 Sm 122.3(5) . . ?
C47 O48 Sm 127.3(10) . . ?
C27 S28 Sm 104.7(3) . . ?
C57 S58 Sm 97.8(3) . . ?
N1 C2 C3 122.3(7) . . ?
N1 C2 C9 116.9(7) . . ?
C3 C2 C9 120.8(7) . . ?
C4 C3 C2 119.5(8) . . ?
C5 C4 C3 118.4(8) . . ?
C4 C5 C6 119.2(8) . . ?
N1 C6 C5 122.9(7) . . ?
N1 C6 C7 116.5(7) . . ?
C5 C6 C7 120.6(7) . . ?
N2 C7 C6 116.7(6) . . ?
N4 C9 C2 122.4(7) . . ?
C16 C11 C12 119.2(8) . . ?
C16 C11 N6 124.7(7) . . ?
C12 C11 N6 116.1(7) . . ?
C13 C12 C11 119.5(9) . . ?
C12 C13 C14 121.9(10) . . ?
C15 C14 C13 119.1(10) . . ?
C14 C15 C16 120.6(9) . . ?
C11 C16 C15 119.6(8) . . ?
O18 C17 N6 126.7(7) . . ?
O18 C17 N3 118.4(7) . . ?
N6 C17 N3 114.9(6) . . ?
N7 C21 C26 125.5(7) . . ?
N7 C21 C22 116.9(7) . . ?
C26 C21 C22 117.5(7) . . ?
C23 C22 C21 120.6(8) . . ?
C24 C23 C22 120.7(7) . . ?
C23 C24 C25 118.8(8) . . ?
C26 C25 C24 121.9(8) . . ?
C25 C26 C21 120.5(7) . . ?
N5 C27 N7 118.3(7) . . ?
N5 C27 S28 127.7(5) . . ?
N7 C27 S28 114.0(6) . . ?
N31 C32 C33 123.5(10) . . ?
N31 C32 C39 115.8(8) . . ?
C33 C32 C39 120.5(11) . . ?
C32 C33 C34 114.5(13) . . ?
C35 C34 C33 120.0(12) . . ?
C36 C35 C34 118.6(13) . . ?
C35 C36 N31 124.2(14) . . ?
C35 C36 C37 119.0(12) . . ?
N31 C36 C37 116.7(9) . . ?
N32 C37 C36 119.5(9) . . ?
N34 C39 C32 121.3(7) . . ?
N36 C41 C46 111.6(6) . . ?
N36 C41 C42 128.4(6) . . ?
C46 C41 C42 120.0 . . ?
C43 C42 C41 120.0 . . ?
C44 C43 C42 120.0 . . ?
C45 C44 C43 120.0 . . ?
C44 C45 C46 120.0 . . ?
C45 C46 C41 120.0 . . ?
O48 C47 N36 128.3(18) . . ?
O48 C47 N33 121.2(13) . . ?
N36 C47 N33 110.4(14) . . ?
C56 C51 C52 119.1(9) . . ?
C56 C51 N37 125.0(8) . . ?
C52 C51 N37 115.8(8) . . ?
C51 C52 C53 118.9(9) . . ?
C54 C53 C52 121.8(10) . . ?
C53 C54 C55 118.7(10) . . ?
C56 C55 C54 121.4(11) . . ?
C55 C56 C51 120.0(9) . . ?
N35 C57 N37 118.0(8) . . ?
N35 C57 S58 125.8(6) . . ?
N37 C57 S58 115.9(7) . . ?
O64 N61 O63 120.1(7) . . ?
O64 N61 O62 121.0(7) . . ?
O63 N61 O62 118.9(7) . . ?
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
Sm O18 2.519(6) . ?
Sm O48 2.528(8) . ?
Sm N34 2.669(7) . ?
Sm N2 2.677(8) . ?
Sm N32 2.681(8) . ?
Sm N1 2.682(7) . ?
Sm N4 2.711(7) . ?
Sm N31 2.720(8) . ?
Sm S28 2.913(6) . ?
Sm S58 2.956(4) . ?
N1 C2 1.349(10) . ?
N1 C6 1.366(10) . ?
N2 C7 1.296(9) . ?
N2 N3 1.374(8) . ?
N3 C17 1.379(9) . ?
N4 C9 1.277(10) . ?
N4 N5 1.404(8) . ?
N5 C27 1.300(10) . ?
N6 C17 1.338(9) . ?
N6 C11 1.417(10) . ?
N7 C27 1.393(9) . ?
N7 C21 1.409(9) . ?
N31 C32 1.315(12) . ?
N31 C36 1.351(12) . ?
N32 C37 1.253(15) . ?
N32 N33 1.393(14) . ?
N33 C47 1.440(18) . ?
N34 C39 1.279(9) . ?
N34 N35 1.401(9) . ?
N35 C57 1.325(11) . ?
N36 C41 1.359(16) . ?
N36 C47 1.387(16) . ?
N37 C57 1.397(10) . ?
N37 C51 1.416(11) . ?
O18 C17 1.263(9) . ?
O48 C47 1.150(15) . ?
S28 C27 1.758(8) . ?
S58 C57 1.705(9) . ?
C2 C3 1.407(12) . ?
C2 C9 1.452(11) . ?
C3 C4 1.397(12) . ?
C4 C5 1.392(12) . ?
C5 C6 1.396(11) . ?
C6 C7 1.455(11) . ?
C11 C16 1.380(11) . ?
C11 C12 1.412(12) . ?
C12 C13 1.370(13) . ?
C13 C14 1.373(15) . ?
C14 C15 1.372(15) . ?
C15 C16 1.413(12) . ?
C21 C26 1.409(11) . ?
C21 C22 1.415(10) . ?
C22 C23 1.393(11) . ?
C23 C24 1.374(12) . ?
C24 C25 1.392(11) . ?
C25 C26 1.362(11) . ?
C32 C33 1.416(14) . ?
C32 C39 1.464(12) . ?
C33 C34 1.44(2) . ?
C34 C35 1.41(2) . ?
C35 C36 1.308(16) . ?
C36 C37 1.473(16) . ?
C41 C46 1.3900 . ?
C41 C42 1.3900 . ?
C42 C43 1.3900 . ?
C43 C44 1.3900 . ?
C44 C45 1.3900 . ?
C45 C46 1.3900 . ?
C51 C56 1.391(13) . ?
C51 C52 1.402(12) . ?
C52 C53 1.410(14) . ?
C53 C54 1.356(15) . ?
C54 C55 1.385(15) . ?
C55 C56 1.386(14) . ?
N61 O64 1.246(8) . ?
N61 O63 1.246(9) . ?
N61 O62 1.265(8) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3N O63 0.88 1.96 2.818(10) 164.6 1_556
N6 H6N O64 0.88 2.12 2.961(10) 159.2 1_556
N7 H7 O62 0.88 2.19 3.066(9) 173.7 .
N33 H33N O72 0.88 2.56 3.27(2) 138.0 13_556
N36 H36N O72 0.88 1.99 2.86(3) 171.9 13_556
