#------------------------------------------------------------------------------
#$Date: 2015-07-14 08:43:09 +0200 (mar 14 de jul de 2015) $
#$Revision: 152030 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/15/7221538.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_7221538
loop_
_publ_author_name
'Nayek, Hari Pada'
'Mahato, Mamata'
'Jana, Partha P.'
'Harms, Klaus'
_publ_section_title
;
 Lanthanide (III) Morpholine 4-Dithiocarbamate Complexes: Pr(III)
 Derivative Shows First Example of Polymeric Lanthanide(III)
 Dithiocarbamate
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA09595F
_journal_year                    2015
_chemical_formula_sum            'C29 H36 Cl4 N5 O3 Pr S6'
_chemical_formula_weight         977.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-06-21 deposited with the CCDC.
2015-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 128.037(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8590(4)
_cell_length_b                   10.2274(3)
_cell_length_c                   27.1517(7)
_cell_measurement_reflns_used    8149
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9060
_cell_measurement_theta_min      2.4230
_cell_volume                     3906.0(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            33541
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         2.462
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.880
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.103
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         8482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0604P)²+5.3427P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1305
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6540
_reflns_number_total             8482
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ra09595f2.cif
_cod_data_source_block           1
_cod_original_cell_volume        3906.00(19)
_cod_database_code               7221538
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4461(4) 0.6183(6) 0.7875(3) 0.0478(14) Uani 1 1 d . . . . .
H1 H 0.3999 0.6830 0.7716 0.057 Uiso 1 1 calc R U . . .
C2 C 0.5355(5) 0.6554(7) 0.8072(3) 0.0538(16) Uani 1 1 d . . . . .
H2 H 0.5484 0.7423 0.8050 0.065 Uiso 1 1 calc R U . . .
C3 C 0.6032(4) 0.5632(7) 0.8296(3) 0.0546(17) Uani 1 1 d . . . . .
H3 H 0.6638 0.5865 0.8435 0.066 Uiso 1 1 calc R U . . .
C4 C 0.5821(4) 0.4309(6) 0.8320(3) 0.0453(14) Uani 1 1 d . . . . .
C5 C 0.4898(3) 0.4033(5) 0.8117(2) 0.0332(11) Uani 1 1 d . . . . .
C6 C 0.6495(4) 0.3278(8) 0.8529(3) 0.0609(18) Uani 1 1 d . . . . .
H6 H 0.7101 0.3472 0.8659 0.073 Uiso 1 1 calc R U . . .
C7 C 0.6269(4) 0.2044(7) 0.8541(3) 0.0589(18) Uani 1 1 d . . . . .
H7 H 0.6719 0.1389 0.8675 0.071 Uiso 1 1 calc R U . . .
C8 C 0.5340(4) 0.1704(6) 0.8349(3) 0.0434(13) Uani 1 1 d . . . . .
C9 C 0.4663(4) 0.2702(5) 0.8140(2) 0.0343(11) Uani 1 1 d . . . . .
C10 C 0.5084(5) 0.0422(6) 0.8349(3) 0.0546(16) Uani 1 1 d . . . . .
H10 H 0.5524 -0.0251 0.8491 0.066 Uiso 1 1 calc R U . . .
C11 C 0.4197(5) 0.0163(6) 0.8140(3) 0.0577(17) Uani 1 1 d . . . . .
H11 H 0.4010 -0.0694 0.8124 0.069 Uiso 1 1 calc R U . . .
C12 C 0.3560(4) 0.1188(6) 0.7948(3) 0.0527(15) Uani 1 1 d . . . . .
H12 H 0.2951 0.0987 0.7811 0.063 Uiso 1 1 calc R U . . .
C13 C 0.1146(4) 0.2025(7) 0.7583(3) 0.0608(19) Uani 1 1 d . . . . .
C14A C 0.0361(13) 0.152(2) 0.8092(7) 0.060(6) Uani 0.422(17) 1 d . . P A 1
H14A H 0.0936 0.1038 0.8401 0.072 Uiso 0.422(17) 1 calc R U P A 1
H14B H 0.0403 0.2358 0.8276 0.072 Uiso 0.422(17) 1 calc R U P A 1
C15A C 0.0242(17) 0.599(2) 0.7001(12) 0.053(6) Uani 0.422(17) 1 d . . P A 1
H15A H 0.0582 0.6643 0.6950 0.063 Uiso 0.422(17) 1 calc R U P A 1
H15B H -0.0043 0.5411 0.6644 0.063 Uiso 0.422(17) 1 calc R U P A 1
C16A C -0.0620(9) 0.1547(18) 0.6964(6) 0.047(5) Uani 0.422(17) 1 d . . P A 1
H16A H -0.1014 0.2293 0.6887 0.056 Uiso 0.422(17) 1 calc R U P A 1
H16B H -0.0581 0.1500 0.6623 0.056 Uiso 0.422(17) 1 calc R U P A 1
C17A C 0.105(10) 0.542(13) 0.804(6) 0.090(12) Uani 0.422(17) 1 d . . P A 1
H17A H 0.1717 0.5453 0.8398 0.108 Uiso 0.422(17) 1 calc R U P A 1
H17B H 0.0770 0.4682 0.8093 0.108 Uiso 0.422(17) 1 calc R U P A 1
N4A N 0.0337(11) 0.176(2) 0.7550(7) 0.046(4) Uani 0.422(17) 1 d . . P A 1
C14B C 0.0682(9) 0.062(2) 0.8108(6) 0.071(5) Uani 0.578(17) 1 d . . P A 2
H14C H 0.1116 -0.0119 0.8282 0.085 Uiso 0.578(17) 1 calc R U P A 2
H14D H 0.0986 0.1309 0.8419 0.085 Uiso 0.578(17) 1 calc R U P A 2
C15B C 0.0030(12) 0.528(3) 0.6950(8) 0.077(7) Uani 0.578(17) 1 d . . P A 2
H15C H 0.0060 0.5859 0.6679 0.092 Uiso 0.578(17) 1 calc R U P A 2
H15D H -0.0114 0.4420 0.6763 0.092 Uiso 0.578(17) 1 calc R U P A 2
C16B C -0.0278(8) 0.0512(16) 0.6976(5) 0.060(4) Uani 0.578(17) 1 d . . P A 2
H16C H -0.0376 0.0903 0.6615 0.072 Uiso 0.578(17) 1 calc R U P A 2
H16D H -0.0176 -0.0418 0.6970 0.072 Uiso 0.578(17) 1 calc R U P A 2
C17B C 0.107(7) 0.568(9) 0.807(5) 0.090(12) Uani 0.578(17) 1 d . . P A 2
H17C H 0.1590 0.5228 0.8446 0.108 Uiso 0.578(17) 1 calc R U P A 2
H17D H 0.1223 0.6603 0.8130 0.108 Uiso 0.578(17) 1 calc R U P A 2
N4B N 0.0587(8) 0.1086(17) 0.7551(5) 0.054(3) Uani 0.578(17) 1 d . . P A 2
C18 C 0.1808(4) 0.4874(6) 0.6103(3) 0.0387(12) Uani 1 1 d . . . . .
C19 C 0.1611(7) 0.4098(8) 0.5166(4) 0.084(3) Uani 1 1 d . . . . .
H19A H 0.2083 0.3458 0.5454 0.101 Uiso 1 1 calc R U . . .
H19B H 0.1014 0.3643 0.4872 0.101 Uiso 1 1 calc R U . . .
C20 C 0.1897(8) 0.4698(11) 0.4837(4) 0.107(3) Uani 1 1 d . . . . .
H20A H 0.2545 0.5007 0.5138 0.128 Uiso 1 1 calc R U . . .
H20B H 0.1899 0.4041 0.4580 0.128 Uiso 1 1 calc R U . . .
C21 C 0.1260(7) 0.6683(10) 0.4790(4) 0.090(3) Uani 1 1 d . . . . .
H21A H 0.0833 0.7367 0.4507 0.108 Uiso 1 1 calc R U . . .
H21B H 0.1881 0.7074 0.5091 0.108 Uiso 1 1 calc R U . . .
C22 C 0.0920(6) 0.6194(8) 0.5125(4) 0.076(2) Uani 1 1 d . . . . .
H22A H 0.0258 0.5938 0.4828 0.091 Uiso 1 1 calc R U . . .
H22B H 0.0962 0.6882 0.5388 0.091 Uiso 1 1 calc R U . . .
C23 C 0.3421(4) 0.6667(6) 0.8748(3) 0.0461(14) Uani 1 1 d . . . . .
C24A C 0.4461(18) 0.725(3) 0.9851(9) 0.069(7) Uani 0.455(19) 1 d . . P B 1
H24A H 0.4295 0.6488 0.9980 0.082 Uiso 0.455(19) 1 calc R U P B 1
H24B H 0.5009 0.7012 0.9875 0.082 Uiso 0.455(19) 1 calc R U P B 1
C25A C 0.4710(14) 0.8159(16) 1.0245(7) 0.062(5) Uani 0.455(19) 1 d . . P B 1
H25A H 0.5359 0.8373 1.0418 0.074 Uiso 0.455(19) 1 calc R U P B 1
H25B H 0.4745 0.7755 1.0582 0.074 Uiso 0.455(19) 1 calc R U P B 1
C26A C 0.3803(15) 0.9739(16) 0.9489(8) 0.061(5) Uani 0.455(19) 1 d . . P B 1
H26A H 0.3223 1.0210 0.9330 0.073 Uiso 0.455(19) 1 calc R U P B 1
H26B H 0.4224 1.0360 0.9501 0.073 Uiso 0.455(19) 1 calc R U P B 1
C27A C 0.3595(18) 0.894(2) 0.9093(10) 0.056(5) Uani 0.455(19) 1 d . . P B 1
H27A H 0.3980 0.9139 0.8963 0.067 Uiso 0.455(19) 1 calc R U P B 1
H27B H 0.2941 0.9117 0.8736 0.067 Uiso 0.455(19) 1 calc R U P B 1
O3A O 0.4236(15) 0.942(3) 1.0131(12) 0.068(5) Uani 0.455(19) 1 d . . P B 1
C24B C 0.4033(17) 0.720(2) 0.9864(9) 0.070(5) Uani 0.545(19) 1 d . . P B 2
H24C H 0.3716 0.6393 0.9828 0.084 Uiso 0.545(19) 1 calc R U P B 2
H24D H 0.4698 0.6977 1.0089 0.084 Uiso 0.545(19) 1 calc R U P B 2
C25B C 0.4011(18) 0.7761(18) 1.0153(8) 0.086(7) Uani 0.545(19) 1 d . . P B 2
H25C H 0.4616 0.7653 1.0564 0.103 Uiso 0.545(19) 1 calc R U P B 2
H25D H 0.3532 0.7388 1.0174 0.103 Uiso 0.545(19) 1 calc R U P B 2
C26B C 0.3183(16) 0.9334(18) 0.9409(7) 0.073(6) Uani 0.545(19) 1 d . . P B 2
H26C H 0.2559 0.9328 0.9309 0.088 Uiso 0.545(19) 1 calc R U P B 2
H26D H 0.3295 1.0228 0.9351 0.088 Uiso 0.545(19) 1 calc R U P B 2
C27B C 0.3111(16) 0.8805(18) 0.9061(8) 0.072(6) Uani 0.545(19) 1 d . . P B 2
H27C H 0.3267 0.9392 0.8855 0.086 Uiso 0.545(19) 1 calc R U P B 2
H27D H 0.2440 0.8599 0.8756 0.086 Uiso 0.545(19) 1 calc R U P B 2
O3B O 0.3834(16) 0.910(2) 1.0062(10) 0.087(6) Uani 0.545(19) 1 d . . P B 2
C31 C 0.6366(8) 0.6105(10) 0.9806(5) 0.112(3) Uani 1 1 d . . . . .
H31A H 0.5879 0.5531 0.9477 0.134 Uiso 1 1 calc R U . . .
H31B H 0.6361 0.6006 1.0159 0.134 Uiso 1 1 calc R U . . .
C32 C 0.1104(13) 0.5655(13) 0.1393(12) 0.263(13) Uani 1 1 d . . . . .
H32A H 0.1302 0.5033 0.1723 0.316 Uiso 1 1 calc R U . . .
H32B H 0.1464 0.6459 0.1573 0.316 Uiso 1 1 calc R U . . .
N1 N 0.4219(3) 0.4970(4) 0.7898(2) 0.0342(9) Uani 1 1 d . . . . .
N2 N 0.3765(3) 0.2431(4) 0.7947(2) 0.0375(10) Uani 1 1 d . . . . .
N3 N 0.1491(4) 0.5062(5) 0.5516(2) 0.0542(13) Uani 1 1 d . . . . .
N5 N 0.3659(5) 0.7526(6) 0.9188(2) 0.083(2) Uani 1 1 d . . . . .
O1 O 0.1330(4) 0.5751(7) 0.4452(2) 0.0932(19) Uani 1 1 d . . . . .
O2 O 0.0996(3) 0.5199(5) 0.75250(19) 0.0564(11) Uani 1 1 d . . . . .
Cl4 Cl 0.7455(2) 0.5597(4) 1.00285(17) 0.1421(12) Uani 1 1 d . . . . .
Cl3 Cl 0.6068(2) 0.7685(3) 0.95457(12) 0.1073(8) Uani 1 1 d . . . . .
Cl1 Cl 0.1192(3) 0.4930(6) 0.0766(4) 0.275(4) Uani 1 1 d . . . . .
Cl2 Cl -0.0178(4) 0.5942(5) 0.0883(3) 0.247(3) Uani 1 1 d . . . . .
Pr1 Pr 0.25171(2) 0.43589(3) 0.75968(2) 0.03214(10) Uani 1 1 d . . . . .
S1 S 0.10151(11) 0.23973(18) 0.69205(7) 0.0567(4) Uani 1 1 d . . . . .
S2 S 0.21584(10) 0.25289(17) 0.82928(7) 0.0506(4) Uani 1 1 d . . . . .
S3 S 0.24725(11) 0.35387(15) 0.65264(7) 0.0480(4) Uani 1 1 d . . . . .
S4 S 0.15648(12) 0.59944(16) 0.64600(7) 0.0514(4) Uani 1 1 d . . . . .
S5 S 0.37914(10) 0.50663(15) 0.89367(7) 0.0447(3) Uani 1 1 d . . . . .
S6 S 0.27350(11) 0.71406(14) 0.79787(7) 0.0459(4) Uani 1 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'
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'
Pr Pr -0.2180 2.8214 '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'
H H 0.0000 0.0000 '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
N1 C1 C2 124.6(6) . .
N1 C1 H1 117.7 . .
C2 C1 H1 117.7 . .
C3 C2 C1 118.9(6) . .
C3 C2 H2 120.5 . .
C1 C2 H2 120.5 . .
C2 C3 C4 119.8(5) . .
C2 C3 H3 120.1 . .
C4 C3 H3 120.1 . .
C5 C4 C3 117.0(5) . .
C5 C4 C6 120.3(6) . .
C3 C4 C6 122.7(6) . .
N1 C5 C4 122.9(5) . .
N1 C5 C9 118.7(4) . .
C4 C5 C9 118.4(5) . .
C7 C6 C4 121.0(6) . .
C7 C6 H6 119.5 . .
C4 C6 H6 119.5 . .
C6 C7 C8 121.2(6) . .
C6 C7 H7 119.4 . .
C8 C7 H7 119.4 . .
C10 C8 C9 119.0(5) . .
C10 C8 C7 122.2(6) . .
C9 C8 C7 118.8(6) . .
N2 C9 C8 121.2(5) . .
N2 C9 C5 118.6(4) . .
C8 C9 C5 120.2(5) . .
C11 C10 C8 119.3(6) . .
C11 C10 H10 120.3 . .
C8 C10 H10 120.3 . .
C10 C11 C12 119.4(6) . .
C10 C11 H11 120.3 . .
C12 C11 H11 120.3 . .
N2 C12 C11 124.1(6) . .
N2 C12 H12 118.0 . .
C11 C12 H12 118.0 . .
N4B C13 S1 118.4(7) . .
N4A C13 S1 120.2(7) . .
N4B C13 S2 120.7(6) . .
N4A C13 S2 117.1(8) . .
S1 C13 S2 118.8(3) . .
C15A C14A N4A 115.9(19) 2_546 .
C15A C14A H14A 108.3 2_546 .
N4A C14A H14A 108.3 . .
C15A C14A H14B 108.3 2_546 .
N4A C14A H14B 108.3 . .
H14A C14A H14B 107.4 . .
C14A C15A O2 134(2) 2_556 .
C14A C15A H15A 103.8 2_556 .
O2 C15A H15A 103.8 . .
C14A C15A H15B 103.8 2_556 .
O2 C15A H15B 103.8 . .
H15A C15A H15B 105.4 . .
C17A C16A N4A 114(6) 2_546 .
C17A C16A H16A 108.9 2_546 .
N4A C16A H16A 108.9 . .
C17A C16A H16B 108.8 2_546 .
N4A C16A H16B 108.9 . .
H16A C16A H16B 107.7 . .
O2 C17A C16A 117(10) . 2_556
O2 C17A H17A 108.0 . .
C16A C17A H17A 108.1 2_556 .
O2 C17A H17B 108.0 . .
C16A C17A H17B 108.1 2_556 .
H17A C17A H17B 107.3 . .
C13 N4A C16A 123.9(12) . .
C13 N4A C14A 124.7(12) . .
C16A N4A C14A 111.1(12) . .
C15B C14B N4B 119.8(13) 2_546 .
C15B C14B H14C 107.4 2_546 .
N4B C14B H14C 107.4 . .
C15B C14B H14D 107.4 2_546 .
N4B C14B H14D 107.4 . .
H14C C14B H14D 106.9 . .
C14B C15B O2 127.3(14) 2_556 .
C14B C15B H15C 105.5 2_556 .
O2 C15B H15C 105.5 . .
C14B C15B H15D 105.5 2_556 .
O2 C15B H15D 105.5 . .
H15C C15B H15D 106.1 . .
C17B C16B N4B 114(4) 2_546 .
C17B C16B H16C 108.8 2_546 .
N4B C16B H16C 108.8 . .
C17B C16B H16D 108.7 2_546 .
N4B C16B H16D 108.8 . .
H16C C16B H16D 107.7 . .
C16B C17B O2 115(6) 2_556 .
C16B C17B H17C 108.7 2_556 .
O2 C17B H17C 108.7 . .
C16B C17B H17D 108.5 2_556 .
O2 C17B H17D 108.6 . .
H17C C17B H17D 107.6 . .
C13 N4B C16B 126.9(10) . .
C13 N4B C14B 123.1(11) . .
C16B N4B C14B 109.5(10) . .
N3 C18 S3 121.7(4) . .
N3 C18 S4 120.5(4) . .
S3 C18 S4 117.7(3) . .
C20 C19 N3 111.7(8) . .
C20 C19 H19A 109.3 . .
N3 C19 H19A 109.3 . .
C20 C19 H19B 109.3 . .
N3 C19 H19B 109.3 . .
H19A C19 H19B 107.9 . .
O1 C20 C19 115.3(8) . .
O1 C20 H20A 108.4 . .
C19 C20 H20A 108.4 . .
O1 C20 H20B 108.4 . .
C19 C20 H20B 108.4 . .
H20A C20 H20B 107.5 . .
O1 C21 C22 115.0(8) . .
O1 C21 H21A 108.5 . .
C22 C21 H21A 108.5 . .
O1 C21 H21B 108.5 . .
C22 C21 H21B 108.5 . .
H21A C21 H21B 107.5 . .
C21 C22 N3 110.3(7) . .
C21 C22 H22A 109.6 . .
N3 C22 H22A 109.6 . .
C21 C22 H22B 109.6 . .
N3 C22 H22B 109.6 . .
H22A C22 H22B 108.1 . .
N5 C23 S6 120.2(5) . .
N5 C23 S5 120.8(5) . .
S6 C23 S5 119.0(3) . .
C25A C24A N5 117.0(18) . .
C25A C24A H24A 108.0 . .
N5 C24A H24A 108.0 . .
C25A C24A H24B 108.0 . .
N5 C24A H24B 108.0 . .
H24A C24A H24B 107.3 . .
C24A C25A O3A 127.4(17) . .
C24A C25A H25A 105.4 . .
O3A C25A H25A 105.4 . .
C24A C25A H25B 105.4 . .
O3A C25A H25B 105.4 . .
H25A C25A H25B 106.0 . .
C27A C26A O3A 124.1(19) . .
C27A C26A H26A 106.3 . .
O3A C26A H26A 106.3 . .
C27A C26A H26B 106.3 . .
O3A C26A H26B 106.3 . .
H26A C26A H26B 106.4 . .
C26A C27A N5 124.3(18) . .
C26A C27A H27A 106.3 . .
N5 C27A H27A 106.3 . .
C26A C27A H27B 106.3 . .
N5 C27A H27B 106.3 . .
H27A C27A H27B 106.4 . .
C26A O3A C25A 105.4(19) . .
C25B C24B N5 128(2) . .
C25B C24B H24C 105.4 . .
N5 C24B H24C 105.4 . .
C25B C24B H24D 105.4 . .
N5 C24B H24D 105.4 . .
H24C C24B H24D 106.0 . .
C24B C25B O3B 123(2) . .
C24B C25B H25C 106.6 . .
O3B C25B H25C 106.6 . .
C24B C25B H25D 106.6 . .
O3B C25B H25D 106.6 . .
H25C C25B H25D 106.6 . .
C27B C26B O3B 127.1(17) . .
C27B C26B H26C 105.5 . .
O3B C26B H26C 105.5 . .
C27B C26B H26D 105.5 . .
O3B C26B H26D 105.5 . .
H26C C26B H26D 106.1 . .
C26B C27B N5 122.6(17) . .
C26B C27B H27C 106.7 . .
N5 C27B H27C 106.7 . .
C26B C27B H27D 106.7 . .
N5 C27B H27D 106.7 . .
H27C C27B H27D 106.6 . .
C25B O3B C26B 108.0(16) . .
Cl3 C31 Cl4 115.2(6) . .
Cl3 C31 H31A 108.5 . .
Cl4 C31 H31A 108.5 . .
Cl3 C31 H31B 108.5 . .
Cl4 C31 H31B 108.5 . .
H31A C31 H31B 107.5 . .
Cl2 C32 Cl1 97.8(12) . .
Cl2 C32 H32A 112.2 . .
Cl1 C32 H32A 112.2 . .
Cl2 C32 H32B 112.2 . .
Cl1 C32 H32B 112.2 . .
H32A C32 H32B 109.8 . .
C1 N1 C5 116.8(5) . .
C1 N1 Pr1 122.8(4) . .
C5 N1 Pr1 120.3(3) . .
C12 N2 C9 117.0(5) . .
C12 N2 Pr1 122.5(4) . .
C9 N2 Pr1 120.5(3) . .
C18 N3 C19 123.4(6) . .
C18 N3 C22 124.6(6) . .
C19 N3 C22 111.9(6) . .
C23 N5 C27A 123.4(9) . .
C23 N5 C24A 120.0(10) . .
C27A N5 C24A 108.5(16) . .
C23 N5 C27B 123.7(8) . .
C23 N5 C24B 126.0(9) . .
C27B N5 C24B 101.5(13) . .
C21 O1 C20 110.6(6) . .
C17A O2 C15A 110(6) . .
C15B O2 C17B 112(4) . .
C17A O2 Pr1 123(6) . .
C15B O2 Pr1 124.4(7) . .
C15A O2 Pr1 121.5(9) . .
C17B O2 Pr1 124(4) . .
N2 Pr1 N1 61.65(13) . .
N2 Pr1 O2 146.05(14) . .
N1 Pr1 O2 146.51(14) . .
N2 Pr1 S1 87.62(10) . .
N1 Pr1 S1 141.19(10) . .
O2 Pr1 S1 71.59(11) . .
N2 Pr1 S5 84.36(10) . .
N1 Pr1 S5 72.55(9) . .
O2 Pr1 S5 89.34(9) . .
S1 Pr1 S5 130.90(4) . .
N2 Pr1 S4 127.28(10) . .
N1 Pr1 S4 90.06(10) . .
O2 Pr1 S4 80.85(10) . .
S1 Pr1 S4 91.00(5) . .
S5 Pr1 S4 131.12(4) . .
N2 Pr1 S6 132.92(10) . .
N1 Pr1 S6 77.92(10) . .
O2 Pr1 S6 68.61(11) . .
S1 Pr1 S6 138.57(5) . .
S5 Pr1 S6 60.00(4) . .
S4 Pr1 S6 71.94(4) . .
N2 Pr1 S3 69.80(10) . .
N1 Pr1 S3 73.02(9) . .
O2 Pr1 S3 126.14(9) . .
S1 Pr1 S3 74.39(5) . .
S5 Pr1 S3 143.84(4) . .
S4 Pr1 S3 59.24(4) . .
S6 Pr1 S3 121.96(4) . .
N2 Pr1 S2 76.72(10) . .
N1 Pr1 S2 126.46(10) . .
O2 Pr1 S2 69.68(11) . .
S1 Pr1 S2 59.79(4) . .
S5 Pr1 S2 71.23(4) . .
S4 Pr1 S2 143.38(5) . .
S6 Pr1 S2 114.27(5) . .
S3 Pr1 S2 123.50(5) . .
C13 S1 Pr1 90.8(2) . .
C13 S2 Pr1 88.1(2) . .
C18 S3 Pr1 91.23(19) . .
C18 S4 Pr1 91.7(2) . .
C23 S5 Pr1 90.2(2) . .
C23 S6 Pr1 89.8(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.327(7) .
C1 C2 1.387(8) .
C1 H1 0.9300 .
C2 C3 1.347(9) .
C2 H2 0.9300 .
C3 C4 1.417(8) .
C3 H3 0.9300 .
C4 C5 1.407(7) .
C4 C6 1.429(9) .
C5 N1 1.362(6) .
C5 C9 1.437(7) .
C6 C7 1.331(10) .
C6 H6 0.9300 .
C7 C8 1.443(8) .
C7 H7 0.9300 .
C8 C10 1.389(9) .
C8 C9 1.407(7) .
C9 N2 1.374(6) .
C10 C11 1.339(9) .
C10 H10 0.9300 .
C11 C12 1.391(9) .
C11 H11 0.9300 .
C12 N2 1.323(7) .
C12 H12 0.9300 .
C13 N4B 1.349(14) .
C13 N4A 1.418(15) .
C13 S1 1.708(6) .
C13 S2 1.718(6) .
C14A C15A 1.09(3) 2_546
C14A N4A 1.47(2) .
C14A H14A 0.9700 .
C14A H14B 0.9700 .
C15A C14A 1.09(3) 2_556
C15A O2 1.46(3) .
C15A H15A 0.9700 .
C15A H15B 0.9700 .
C16A C17A 1.38(15) 2_546
C16A N4A 1.465(19) .
C16A H16A 0.9700 .
C16A H16B 0.9700 .
C17A O2 1.35(15) .
C17A C16A 1.38(15) 2_556
C17A H17A 0.9700 .
C17A H17B 0.9700 .
C14B C15B 1.23(2) 2_546
C14B N4B 1.493(17) .
C14B H14C 0.9700 .
C14B H14D 0.9700 .
C15B C14B 1.23(2) 2_556
C15B O2 1.449(16) .
C15B H15C 0.9700 .
C15B H15D 0.9700 .
C16B C17B 1.34(10) 2_546
C16B N4B 1.482(16) .
C16B H16C 0.9700 .
C16B H16D 0.9700 .
C17B C16B 1.34(10) 2_556
C17B O2 1.50(10) .
C17B H17C 0.9700 .
C17B H17D 0.9700 .
C18 N3 1.337(7) .
C18 S3 1.707(6) .
C18 S4 1.721(6) .
C19 C20 1.413(12) .
C19 N3 1.473(9) .
C19 H19A 0.9700 .
C19 H19B 0.9700 .
C20 O1 1.405(10) .
C20 H20A 0.9700 .
C20 H20B 0.9700 .
C21 O1 1.382(10) .
C21 C22 1.458(11) .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C22 N3 1.474(9) .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
C23 N5 1.324(8) .
C23 S6 1.716(6) .
C23 S5 1.722(6) .
C24A C25A 1.27(3) .
C24A N5 1.48(2) .
C24A H24A 0.9700 .
C24A H24B 0.9700 .
C25A O3A 1.47(3) .
C25A H25A 0.9700 .
C25A H25B 0.9700 .
C26A C27A 1.21(2) .
C26A O3A 1.44(3) .
C26A H26A 0.9700 .
C26A H26B 0.9700 .
C27A N5 1.46(2) .
C27A H27A 0.9700 .
C27A H27B 0.9700 .
C24B C25B 0.99(2) .
C24B N5 1.55(2) .
C24B H24C 0.9700 .
C24B H24D 0.9700 .
C25B O3B 1.39(3) .
C25B H25C 0.9700 .
C25B H25D 0.9700 .
C26B C27B 1.03(2) .
C26B O3B 1.42(3) .
C26B H26C 0.9700 .
C26B H26D 0.9700 .
C27B N5 1.539(18) .
C27B H27C 0.9700 .
C27B H27D 0.9700 .
C31 Cl3 1.712(11) .
C31 Cl4 1.723(11) .
C31 H31A 0.9700 .
C31 H31B 0.9700 .
C32 Cl2 1.827(18) .
C32 Cl1 1.95(2) .
C32 H32A 0.9700 .
C32 H32B 0.9700 .
N1 Pr1 2.690(4) .
N2 Pr1 2.674(4) .
O2 Pr1 2.739(4) .
Pr1 S1 2.9192(16) .
Pr1 S5 2.9554(15) .
Pr1 S4 2.9578(16) .
Pr1 S6 2.9704(15) .
Pr1 S3 2.9785(15) .
Pr1 S2 2.9960(15) .
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
N1 C1 C2 C3 1.0(10) .
C1 C2 C3 C4 0.7(9) .
C2 C3 C4 C5 -1.5(9) .
C2 C3 C4 C6 177.5(6) .
C3 C4 C5 N1 0.8(8) .
C6 C4 C5 N1 -178.3(5) .
C3 C4 C5 C9 -179.5(5) .
C6 C4 C5 C9 1.4(8) .
C5 C4 C6 C7 -0.5(10) .
C3 C4 C6 C7 -179.5(6) .
C4 C6 C7 C8 -0.6(11) .
C6 C7 C8 C10 179.0(7) .
C6 C7 C8 C9 0.8(9) .
C10 C8 C9 N2 1.3(8) .
C7 C8 C9 N2 179.5(5) .
C10 C8 C9 C5 -178.1(5) .
C7 C8 C9 C5 0.1(8) .
N1 C5 C9 N2 -0.9(7) .
C4 C5 C9 N2 179.4(5) .
N1 C5 C9 C8 178.5(5) .
C4 C5 C9 C8 -1.2(7) .
C9 C8 C10 C11 1.0(9) .
C7 C8 C10 C11 -177.2(6) .
C8 C10 C11 C12 -2.1(10) .
C10 C11 C12 N2 1.0(10) .
S1 C13 N4A C16A 11(2) .
S2 C13 N4A C16A 168.8(14) .
S1 C13 N4A C14A -175.4(15) .
S2 C13 N4A C14A -18(2) .
C17A C16A N4A C13 129(6) 2_546
C17A C16A N4A C14A -45(7) 2_546
C15A C14A N4A C13 -158(2) 2_546
C15A C14A N4A C16A 16(3) 2_546
S1 C13 N4B C16B -13.8(18) .
S2 C13 N4B C16B -177.1(11) .
S1 C13 N4B C14B 175.9(11) .
S2 C13 N4B C14B 12.6(18) .
C17B C16B N4B C13 -120(5) 2_546
C17B C16B N4B C14B 52(5) 2_546
C15B C14B N4B C13 146(2) 2_546
C15B C14B N4B C16B -26(3) 2_546
N3 C19 C20 O1 -52.2(12) .
O1 C21 C22 N3 52.6(10) .
N5 C24A C25A O3A 7(4) .
O3A C26A C27A N5 7(4) .
C27A C26A O3A C25A 24(3) .
C24A C25A O3A C26A -31(3) .
N5 C24B C25B O3B -16(5) .
O3B C26B C27B N5 6(5) .
C24B C25B O3B C26B 35(4) .
C27B C26B O3B C25B -30(4) .
C2 C1 N1 C5 -1.7(8) .
C2 C1 N1 Pr1 174.7(5) .
C4 C5 N1 C1 0.8(7) .
C9 C5 N1 C1 -178.9(5) .
C4 C5 N1 Pr1 -175.8(4) .
C9 C5 N1 Pr1 4.5(6) .
C11 C12 N2 C9 1.2(9) .
C11 C12 N2 Pr1 -178.5(5) .
C8 C9 N2 C12 -2.3(8) .
C5 C9 N2 C12 177.1(5) .
C8 C9 N2 Pr1 177.4(4) .
C5 C9 N2 Pr1 -3.2(6) .
S3 C18 N3 C19 5.5(9) .
S4 C18 N3 C19 -175.2(6) .
S3 C18 N3 C22 -179.7(6) .
S4 C18 N3 C22 -0.4(9) .
C20 C19 N3 C18 -136.3(8) .
C20 C19 N3 C22 48.3(10) .
C21 C22 N3 C18 136.8(7) .
C21 C22 N3 C19 -47.8(10) .
S6 C23 N5 C27A -17.0(15) .
S5 C23 N5 C27A 163.1(13) .
S6 C23 N5 C24A -162.0(15) .
S5 C23 N5 C24A 18.0(17) .
S6 C23 N5 C27B 21.4(17) .
S5 C23 N5 C27B -158.6(14) .
S6 C23 N5 C24B 162.7(13) .
S5 C23 N5 C24B -17.2(16) .
C26A C27A N5 C23 179.5(19) .
C26A C27A N5 C24A -32(3) .
C25A C24A N5 C23 173.9(18) .
C25A C24A N5 C27A 24(3) .
C26B C27B N5 C23 163(2) .
C26B C27B N5 C24B 14(3) .
C25B C24B N5 C23 -157(3) .
C25B C24B N5 C27B -9(4) .
C22 C21 O1 C20 -54.8(11) .
C19 C20 O1 C21 54.8(12) .
C16A C17A O2 C15A -18(11) 2_556
C16A C17A O2 Pr1 136(7) 2_556
C14B C15B O2 C17B -4(5) 2_556
C14B C15B O2 Pr1 178(2) 2_556
C14A C15A O2 C17A -16(7) 2_556
C14A C15A O2 Pr1 -171(3) 2_556
C16B C17B O2 C15B 30(8) 2_556
C16B C17B O2 Pr1 -152(5) 2_556
N4B C13 S1 Pr1 -179.7(10) .
N4A C13 S1 Pr1 140.9(12) .
S2 C13 S1 Pr1 -16.1(5) .
N4B C13 S2 Pr1 178.9(10) .
N4A C13 S2 Pr1 -142.0(11) .
S1 C13 S2 Pr1 15.7(5) .
N3 C18 S3 Pr1 -177.0(5) .
S4 C18 S3 Pr1 3.7(3) .
N3 C18 S4 Pr1 177.0(4) .
S3 C18 S4 Pr1 -3.7(3) .
N5 C23 S5 Pr1 170.3(6) .
S6 C23 S5 Pr1 -9.7(4) .
N5 C23 S6 Pr1 -170.3(6) .
S5 C23 S6 Pr1 9.7(4) .
