#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:53:47 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179545 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/14/4501405.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_4501405
loop_
_publ_author_name
'Qian, Su-Yan'
'Zhou, Hu'
'Yuan, Ai-Hua'
'Song, You'
_publ_section_title
;
 Syntheses, Structures, and Magnetic Properties of Five Novel
 Octacyanometallate-Based Lanthanide Complexes with Helical Chains
;
_journal_issue                   12
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5676
_journal_paper_doi               10.1021/cg201217a
_journal_volume                  11
_journal_year                    2011
_chemical_formula_moiety         'C39 H51 N15 O5 Pr W, C3 H7 N O, 2(H2 O)'
_chemical_formula_sum            'C42 H62 N16 O8 Pr W'
_chemical_formula_weight         1243.84
_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                 126.100(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.0136(13)
_cell_length_b                   19.237(3)
_cell_length_c                   23.1634(15)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.38
_cell_volume                     6125.5(12)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart Aepex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            46243
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    2.716
_exptl_absorpt_correction_T_max  0.6126
_exptl_absorpt_correction_T_min  0.5386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2492
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         12011
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.05P)²+1.66P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                9504
_reflns_number_total             12011
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201217a_si_006.cif
_cod_data_source_block           yah165
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4501405
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
C1 C 0.8569(3) 1.0907(2) 0.6263(2) 0.0316(9) Uani 1 1 d . . .
C2 C 0.8434(4) 1.1907(2) 0.6956(2) 0.0420(11) Uani 1 1 d . . .
C3 C 0.8154(3) 1.2839(2) 0.6054(2) 0.0326(9) Uani 1 1 d . . .
C4 C 0.9920(3) 1.2736(3) 0.7282(2) 0.0412(11) Uani 1 1 d . . .
C5 C 0.9809(3) 1.2708(3) 0.6155(2) 0.0412(11) Uani 1 1 d . . .
C6 C 1.0058(3) 1.1375(2) 0.6288(2) 0.0335(9) Uani 1 1 d . . .
C7 C 0.8233(3) 1.1857(3) 0.5325(2) 0.0387(10) Uani 1 1 d . . .
C8 C 1.0188(3) 1.1445(2) 0.7448(2) 0.0398(10) Uani 1 1 d . . .
C9 C 0.6593(4) 0.9972(2) 0.6273(3) 0.0420(11) Uani 1 1 d . . .
H9 H 0.7134 1.0258 0.6548 0.050 Uiso 1 1 calc R . .
C10 C 0.5773(4) 1.0079(3) 0.6274(3) 0.0478(12) Uani 1 1 d . . .
C11 C 0.4972(3) 0.9670(2) 0.5868(3) 0.0404(11) Uani 1 1 d . . .
C12 C 0.4958(3) 0.9140(3) 0.5447(3) 0.0439(11) Uani 1 1 d . . .
C20 C 0.5792(3) 0.9040(2) 0.5460(2) 0.0384(10) Uani 1 1 d . . .
N9 N 0.6604(3) 0.9453(2) 0.5873(2) 0.0372(8) Uani 1 1 d . . .
C13 C 0.4136(4) 0.8698(3) 0.4995(3) 0.0506(13) Uani 1 1 d . . .
H13 H 0.3574 0.8759 0.4969 0.061 Uiso 1 1 calc R . .
C14 C 0.4173(4) 0.8184(3) 0.4601(3) 0.0535(14) Uani 1 1 d . . .
H14 H 0.3652 0.7878 0.4340 0.064 Uiso 1 1 calc R . .
C15 C 0.4968(4) 0.8109(3) 0.4581(3) 0.0509(13) Uani 1 1 d . . .
C16 C 0.4993(3) 0.7609(3) 0.4142(3) 0.0460(12) Uani 1 1 d . . .
C17 C 0.5782(4) 0.7622(3) 0.4124(3) 0.0552(14) Uani 1 1 d . . .
C18 C 0.6601(3) 0.8040(2) 0.4602(2) 0.0383(10) Uani 1 1 d . . .
H18 H 0.7145 0.8010 0.4600 0.046 Uiso 1 1 calc R . .
C19 C 0.5808(3) 0.8532(2) 0.5041(2) 0.0377(10) Uani 1 1 d . . .
C21 C 0.5891(4) 1.0669(3) 0.6761(4) 0.0582(15) Uani 1 1 d . . .
H21A H 0.5301 1.0934 0.6523 0.087 Uiso 1 1 calc R . .
H21B H 0.6417 1.0965 0.6870 0.087 Uiso 1 1 calc R . .
H21C H 0.6030 1.0478 0.7195 0.087 Uiso 1 1 calc R . .
C22 C 0.4098(3) 0.9783(3) 0.5901(3) 0.0506(13) Uani 1 1 d . . .
H22A H 0.3680 1.0137 0.5565 0.076 Uiso 1 1 calc R . .
H22B H 0.4331 0.9926 0.6374 0.076 Uiso 1 1 calc R . .
H22C H 0.3741 0.9357 0.5784 0.076 Uiso 1 1 calc R . .
C23 C 0.4173(4) 0.7087(4) 0.3687(3) 0.0672(17) Uani 1 1 d . . .
H23A H 0.3730 0.7267 0.3213 0.101 Uiso 1 1 calc R . .
H23B H 0.3832 0.7008 0.3896 0.101 Uiso 1 1 calc R . .
H23C H 0.4442 0.6656 0.3668 0.101 Uiso 1 1 calc R . .
C24 C 0.5866(4) 0.7180(3) 0.3616(3) 0.0490(12) Uani 1 1 d . . .
H24A H 0.5673 0.6711 0.3618 0.074 Uiso 1 1 calc R . .
H24B H 0.6528 0.7183 0.3770 0.074 Uiso 1 1 calc R . .
H24C H 0.5451 0.7367 0.3142 0.074 Uiso 1 1 calc R . .
C25 C 0.9507(4) 0.9472(3) 0.7937(3) 0.0531(13) Uani 1 1 d . . .
H25 H 1.0044 0.9205 0.8068 0.064 Uiso 1 1 calc R . .
C26 C 1.0432(5) 0.9906(3) 0.9114(4) 0.0754(19) Uani 1 1 d . . .
H26A H 1.0547 0.9476 0.9363 0.113 Uiso 1 1 calc R . .
H26B H 1.0389 1.0278 0.9370 0.113 Uiso 1 1 calc R . .
H26C H 1.0960 0.9995 0.9080 0.113 Uiso 1 1 calc R . .
C27 C 0.8725(6) 1.0314(4) 0.8244(3) 0.082(2) Uani 1 1 d . . .
H27A H 0.8810 1.0770 0.8120 0.124 Uiso 1 1 calc R . .
H27B H 0.8716 1.0345 0.8654 0.124 Uiso 1 1 calc R . .
H27C H 0.8121 1.0121 0.7850 0.124 Uiso 1 1 calc R . .
C28 C 0.8497(3) 0.9811(2) 0.4997(2) 0.0276(8) Uani 1 1 d . . .
H28 H 0.8977 1.0069 0.5390 0.033 Uiso 1 1 calc R . .
C29 C 0.7519(3) 0.9608(3) 0.3721(2) 0.0404(11) Uani 1 1 d . . .
H29A H 0.7422 0.9153 0.3837 0.061 Uiso 1 1 calc R . .
H29B H 0.7695 0.9570 0.3397 0.061 Uiso 1 1 calc R . .
H29C H 0.6929 0.9872 0.3500 0.061 Uiso 1 1 calc R . .
C30 C 0.8872(4) 1.0511(3) 0.4314(3) 0.0466(11) Uani 1 1 d . . .
H30B H 0.9445 1.0307 0.4396 0.070 Uiso 1 1 calc R . .
H30C H 0.9057 1.0864 0.4665 0.070 Uiso 1 1 calc R . .
H30A H 0.8483 1.0714 0.3845 0.070 Uiso 1 1 calc R . .
C31 C 0.9469(3) 0.7605(2) 0.5988(2) 0.0309(9) Uani 1 1 d . . .
H31 H 0.9797 0.7377 0.6425 0.037 Uiso 1 1 calc R . .
C32 C 0.9359(4) 0.7938(3) 0.4944(3) 0.0574(14) Uani 1 1 d . . .
H32A H 0.8828 0.8208 0.4863 0.086 Uiso 1 1 calc R . .
H32B H 0.9118 0.7612 0.4561 0.086 Uiso 1 1 calc R . .
H32C H 0.9823 0.8242 0.4964 0.086 Uiso 1 1 calc R . .
C33 C 1.0686(4) 0.7150(3) 0.5836(3) 0.0565(14) Uani 1 1 d . . .
H33A H 1.1184 0.7224 0.6335 0.085 Uiso 1 1 calc R . .
H33B H 1.0924 0.7286 0.5566 0.085 Uiso 1 1 calc R . .
H33C H 1.0512 0.6666 0.5753 0.085 Uiso 1 1 calc R . .
C34 C 0.7645(4) 0.7641(3) 0.6919(3) 0.0542(14) Uani 1 1 d . . .
H34 H 0.8019 0.7259 0.6974 0.065 Uiso 1 1 calc R . .
C35 C 0.6777(5) 0.8306(4) 0.7298(3) 0.0701(17) Uani 1 1 d . . .
H35A H 0.7260 0.8659 0.7564 0.105 Uiso 1 1 calc R . .
H35B H 0.6460 0.8208 0.7521 0.105 Uiso 1 1 calc R . .
H35C H 0.6305 0.8465 0.6818 0.105 Uiso 1 1 calc R . .
C36 C 0.7401(4) 0.7130(3) 0.7792(3) 0.0632(16) Uani 1 1 d . . .
H36A H 0.7221 0.6681 0.7567 0.095 Uiso 1 1 calc R . .
H36B H 0.7005 0.7240 0.7949 0.095 Uiso 1 1 calc R . .
H36C H 0.8073 0.7123 0.8196 0.095 Uiso 1 1 calc R . .
C37 C 1.0588(3) 0.9603(2) 0.7045(3) 0.0441(11) Uani 1 1 d . . .
H37 H 1.0460 1.0027 0.7168 0.053 Uiso 1 1 calc R . .
C38 C 1.2292(4) 0.9773(3) 0.8026(3) 0.0707(18) Uani 1 1 d . . .
H38A H 1.2481 1.0135 0.7846 0.106 Uiso 1 1 calc R . .
H38B H 1.2842 0.9481 0.8344 0.106 Uiso 1 1 calc R . .
H38C H 1.2063 0.9976 0.8280 0.106 Uiso 1 1 calc R . .
C39 C 1.1775(3) 0.8665(2) 0.7333(3) 0.0453(11) Uani 1 1 d . . .
H39B H 1.2393 0.8681 0.7408 0.068 Uiso 1 1 calc R . .
H39C H 1.1284 0.8511 0.6855 0.068 Uiso 1 1 calc R . .
H39A H 1.1810 0.8348 0.7668 0.068 Uiso 1 1 calc R . .
C40 C 0.5139(8) 0.5985(6) 0.6724(6) 0.064(3) Uani 0.509(5) 1 d P A 1
H40 H 0.5022 0.5988 0.7069 0.077 Uiso 0.509(5) 1 calc PR A 1
C41 C 0.5029(10) 0.6572(7) 0.5714(7) 0.088(5) Uani 0.509(5) 1 d P A 1
H41A H 0.5674 0.6434 0.5884 0.131 Uiso 0.509(5) 1 calc PR A 1
H41B H 0.4901 0.7031 0.5514 0.131 Uiso 0.509(5) 1 calc PR A 1
H41C H 0.4566 0.6253 0.5353 0.131 Uiso 0.509(5) 1 calc PR A 1
C42 C 0.4458(8) 0.7222(6) 0.6237(6) 0.067(3) Uani 0.509(5) 1 d P A 1
H42A H 0.3869 0.7135 0.6192 0.101 Uiso 0.509(5) 1 calc PR A 1
H42B H 0.4307 0.7451 0.5815 0.101 Uiso 0.509(5) 1 calc PR A 1
H42C H 0.4877 0.7514 0.6645 0.101 Uiso 0.509(5) 1 calc PR A 1
C43 C 0.7634(11) 0.6418(8) 0.5303(7) 0.073(4) Uani 0.491(5) 1 d P A 2
H43 H 0.7711 0.6863 0.5486 0.088 Uiso 0.491(5) 1 calc PR A 2
C44 C 0.6478(10) 0.6246(7) 0.5489(8) 0.088(5) Uani 0.491(5) 1 d P A 2
H44A H 0.6877 0.6471 0.5946 0.132 Uiso 0.491(5) 1 calc PR A 2
H44B H 0.6160 0.5852 0.5523 0.132 Uiso 0.491(5) 1 calc PR A 2
H44C H 0.5997 0.6567 0.5142 0.132 Uiso 0.491(5) 1 calc PR A 2
C45 C 0.6581(11) 0.5384(6) 0.4877(7) 0.076(4) Uani 0.491(5) 1 d P A 2
H45A H 0.6251 0.5153 0.5045 0.114 Uiso 0.491(5) 1 calc PR A 2
H45B H 0.7076 0.5084 0.4939 0.114 Uiso 0.491(5) 1 calc PR A 2
H45C H 0.6123 0.5494 0.4380 0.114 Uiso 0.491(5) 1 calc PR A 2
W1 W 0.915596(13) 1.198259(10) 0.646307(9) 0.03610(6) Uani 1 1 d . . .
N1 N 0.8357(3) 1.03433(18) 0.61879(18) 0.0328(8) Uani 1 1 d . . .
N2 N 0.8049(3) 1.1877(2) 0.7248(2) 0.0457(10) Uani 1 1 d . . .
N3 N 0.7614(3) 1.3328(2) 0.5838(2) 0.0444(9) Uani 1 1 d . . .
N4 N 1.0355(3) 1.31672(18) 0.77358(19) 0.0342(8) Uani 1 1 d . . .
N5 N 1.0189(3) 1.3116(2) 0.6012(2) 0.0459(10) Uani 1 1 d . . .
N6 N 1.0530(3) 1.10323(19) 0.61792(19) 0.0375(8) Uani 1 1 d . . .
N7 N 0.7769(3) 1.1767(2) 0.47326(19) 0.0413(9) Uani 1 1 d . . .
N8 N 1.0769(3) 1.1178(2) 0.7977(2) 0.0490(11) Uani 1 1 d . . .
N10 N 0.6617(3) 0.8477(2) 0.50598(19) 0.0372(8) Uani 1 1 d . . .
N11 N 0.9544(4) 0.9859(2) 0.8413(2) 0.0593(12) Uani 1 1 d . . .
N12 N 0.8293(3) 0.9958(2) 0.43687(18) 0.0343(8) Uani 1 1 d . . .
N13 N 0.9822(2) 0.7569(2) 0.56096(18) 0.0359(8) Uani 1 1 d . . .
N14 N 0.7258(3) 0.7652(3) 0.7283(3) 0.0631(14) Uani 1 1 d . . .
N15 N 1.1526(3) 0.93625(19) 0.74384(18) 0.0400(9) Uani 1 1 d . . .
N16 N 0.4944(7) 0.6571(5) 0.6329(6) 0.075(3) Uani 0.509(5) 1 d P A 1
N17 N 0.7034(8) 0.6033(6) 0.5289(6) 0.069(3) Uani 0.491(5) 1 d P A 2
O1 O 0.8759(2) 0.94529(16) 0.73069(16) 0.0411(7) Uani 1 1 d . . .
O2 O 0.8070(2) 0.93329(15) 0.50946(15) 0.0318(6) Uani 1 1 d . . .
O3 O 0.8694(2) 0.79407(15) 0.57710(15) 0.0336(6) Uani 1 1 d . . .
O4 O 0.7533(2) 0.81029(15) 0.65244(18) 0.0413(8) Uani 1 1 d . . .
O5 O 0.9910(2) 0.92792(16) 0.65343(14) 0.0357(7) Uani 1 1 d . . .
O6 O 0.5480(6) 0.5424(5) 0.6636(4) 0.070(2) Uani 0.509(5) 1 d P A 1
O7 O 0.8128(7) 0.6269(5) 0.5102(5) 0.077(3) Uani 0.491(5) 1 d P A 2
O1W O 0.6701(7) 0.9676(5) 0.8255(4) 0.058(3) Uani 0.40 1 d P . .
H8A H 0.6502 0.9254 0.8136 0.070 Uiso 0.40 1 d PR . .
H8B H 0.7154 0.9692 0.8692 0.070 Uiso 0.40 1 d PR . .
O2W O 0.8390(8) 0.8881(5) 0.9144(5) 0.069(3) Uani 0.40 1 d P . .
H9A H 0.8416 0.9178 0.9425 0.082 Uiso 0.40 1 d PR . .
H9C H 0.8867 0.8599 0.9370 0.082 Uiso 0.40 1 d PR . .
O3W O 0.6543(6) 0.1602(4) 0.3218(4) 0.047(2) Uani 0.40 1 d P . .
H10A H 0.6474 0.1215 0.3368 0.056 Uiso 0.40 1 d PR . .
H10B H 0.6038 0.1683 0.2807 0.056 Uiso 0.40 1 d PR . .
O4W O 0.7114(7) 0.1083(5) 0.8643(4) 0.056(3) Uani 0.40 1 d P . .
H11A H 0.7060 0.0653 0.8716 0.067 Uiso 0.40 1 d PR . .
H11B H 0.7661 0.1240 0.8984 0.067 Uiso 0.40 1 d PR . .
O5W O 0.6840(6) 0.2149(4) 0.7775(4) 0.048(2) Uani 0.40 1 d P . .
H12D H 0.6929 0.1811 0.8044 0.057 Uiso 0.40 1 d PR . .
H12A H 0.6781 0.2533 0.7935 0.057 Uiso 0.40 1 d PR . .
Pr1 Pr 0.828575(17) 0.895273(12) 0.618785(12) 0.03318(7) 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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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'
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 W1 173.6(4) . .
N2 C2 W1 178.1(4) . .
N3 C3 W1 178.3(4) . .
N4 C4 W1 178.7(4) . .
N5 C5 W1 177.4(4) . .
N6 C6 W1 178.2(4) . .
N7 C7 W1 177.2(4) . .
N8 C8 W1 177.0(5) . .
N9 C9 C10 121.1(4) . .
N9 C9 H9 119.5 . .
C10 C9 H9 119.5 . .
C11 C10 C9 120.2(5) . .
C11 C10 C21 125.6(5) . .
C9 C10 C21 114.2(5) . .
C10 C11 C12 120.1(4) . .
C10 C11 C22 119.0(5) . .
C12 C11 C22 120.9(4) . .
C11 C12 C20 118.6(5) . .
C11 C12 C13 123.3(4) . .
C20 C12 C13 118.1(5) . .
N9 C20 C19 117.9(4) . .
N9 C20 C12 121.3(4) . .
C19 C20 C12 120.8(4) . .
C9 N9 C20 118.8(4) . .
C9 N9 Pr1 121.1(3) . .
C20 N9 Pr1 117.1(3) . .
C14 C13 C12 120.4(5) . .
C14 C13 H13 119.8 . .
C12 C13 H13 119.8 . .
C13 C14 C15 121.6(5) . .
C13 C14 H14 119.2 . .
C15 C14 H14 119.2 . .
C14 C15 C16 122.4(5) . .
C14 C15 C19 118.8(5) . .
C16 C15 C19 118.8(5) . .
C17 C16 C15 117.0(5) . .
C17 C16 C23 120.3(5) . .
C15 C16 C23 122.7(5) . .
C16 C17 C18 121.2(5) . .
C16 C17 C24 123.6(5) . .
C18 C17 C24 115.1(5) . .
N10 C18 C17 121.9(4) . .
N10 C18 H18 119.1 . .
C17 C18 H18 119.1 . .
N10 C19 C20 118.0(4) . .
N10 C19 C15 121.9(4) . .
C20 C19 C15 120.0(4) . .
C10 C21 H21A 109.5 . .
C10 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C10 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C11 C22 H22A 109.5 . .
C11 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C11 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C16 C23 H23A 109.5 . .
C16 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C16 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C17 C24 H24A 109.5 . .
C17 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
C17 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
O1 C25 N11 120.9(5) . .
O1 C25 H25 119.5 . .
N11 C25 H25 119.5 . .
N11 C26 H26A 109.5 . .
N11 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
N11 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
N11 C27 H27A 109.5 . .
N11 C27 H27B 109.5 . .
H27A C27 H27B 109.5 . .
N11 C27 H27C 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
O2 C28 N12 123.1(4) . .
O2 C28 H28 118.5 . .
N12 C28 H28 118.5 . .
N12 C29 H29A 109.5 . .
N12 C29 H29B 109.5 . .
H29A C29 H29B 109.5 . .
N12 C29 H29C 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
N12 C30 H30B 109.5 . .
N12 C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
N12 C30 H30A 109.5 . .
H30B C30 H30A 109.5 . .
H30C C30 H30A 109.5 . .
O3 C31 N13 122.2(4) . .
O3 C31 H31 118.9 . .
N13 C31 H31 118.9 . .
N13 C32 H32A 109.5 . .
N13 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
N13 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
N13 C33 H33A 109.5 . .
N13 C33 H33B 109.5 . .
H33A C33 H33B 109.5 . .
N13 C33 H33C 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
O4 C34 N14 123.2(5) . .
O4 C34 H34 118.4 . .
N14 C34 H34 118.4 . .
N14 C35 H35A 109.5 . .
N14 C35 H35B 109.5 . .
H35A C35 H35B 109.5 . .
N14 C35 H35C 109.5 . .
H35A C35 H35C 109.5 . .
H35B C35 H35C 109.5 . .
N14 C36 H36A 109.5 . .
N14 C36 H36B 109.5 . .
H36A C36 H36B 109.5 . .
N14 C36 H36C 109.5 . .
H36A C36 H36C 109.5 . .
H36B C36 H36C 109.5 . .
O5 C37 N15 122.2(4) . .
O5 C37 H37 118.9 . .
N15 C37 H37 118.9 . .
N15 C38 H38A 109.5 . .
N15 C38 H38B 109.5 . .
H38A C38 H38B 109.5 . .
N15 C38 H38C 109.5 . .
H38A C38 H38C 109.5 . .
H38B C38 H38C 109.5 . .
N15 C39 H39B 109.5 . .
N15 C39 H39C 109.5 . .
H39B C39 H39C 109.5 . .
N15 C39 H39A 109.5 . .
H39B C39 H39A 109.5 . .
H39C C39 H39A 109.5 . .
O6 C40 N16 122.6(13) . .
O6 C40 H40 118.7 . .
N16 C40 H40 118.7 . .
O7 C43 N17 126.4(16) . .
O7 C43 H43 116.8 . .
N17 C43 H43 116.8 . .
N17 C44 H44A 109.5 . .
N17 C44 H44B 109.5 . .
H44A C44 H44B 109.5 . .
N17 C44 H44C 109.5 . .
H44A C44 H44C 109.5 . .
H44B C44 H44C 109.5 . .
N17 C45 H45A 109.5 . .
N17 C45 H45B 109.5 . .
H45A C45 H45B 109.5 . .
N17 C45 H45C 109.5 . .
H45A C45 H45C 109.5 . .
H45B C45 H45C 109.5 . .
C4 W1 C2 78.98(18) . .
C4 W1 C7 142.85(18) . .
C2 W1 C7 114.73(18) . .
C4 W1 C3 77.26(16) . .
C2 W1 C3 74.28(18) . .
C7 W1 C3 74.20(16) . .
C4 W1 C6 114.29(17) . .
C2 W1 C6 140.32(18) . .
C7 W1 C6 78.10(17) . .
C3 W1 C6 143.43(16) . .
C4 W1 C5 71.87(18) . .
C2 W1 C5 143.18(18) . .
C7 W1 C5 79.16(17) . .
C3 W1 C5 77.71(18) . .
C6 W1 C5 74.00(18) . .
C4 W1 C8 72.10(17) . .
C2 W1 C8 76.46(18) . .
C7 W1 C8 142.93(17) . .
C3 W1 C8 140.88(16) . .
C6 W1 C8 73.20(17) . .
C5 W1 C8 113.88(19) . .
C4 W1 C1 141.84(17) . .
C2 W1 C1 73.52(17) . .
C7 W1 C1 74.10(16) . .
C3 W1 C1 118.63(15) . .
C6 W1 C1 74.80(16) . .
C5 W1 C1 142.27(17) . .
C8 W1 C1 76.07(16) . .
C1 N1 Pr1 167.0(3) . .
C4 N4 Pr1 165.4(4) . 2_756
C18 N10 C19 118.4(4) . .
C18 N10 Pr1 120.6(3) . .
C19 N10 Pr1 118.9(3) . .
C25 N11 C26 119.3(6) . .
C25 N11 C27 122.9(5) . .
C26 N11 C27 117.5(5) . .
C28 N12 C29 122.2(4) . .
C28 N12 C30 119.1(4) . .
C29 N12 C30 118.6(4) . .
C31 N13 C32 120.6(4) . .
C31 N13 C33 122.6(4) . .
C32 N13 C33 116.8(4) . .
C34 N14 C36 126.0(5) . .
C34 N14 C35 120.0(5) . .
C36 N14 C35 113.0(5) . .
C37 N15 C38 119.5(4) . .
C37 N15 C39 122.3(4) . .
C38 N15 C39 117.9(4) . .
C40 N16 C42 135.0(13) . .
C40 N16 C41 120.8(12) . .
C42 N16 C41 102.9(9) . .
C43 N17 C44 123.0(14) . .
C43 N17 C45 128.6(14) . .
C44 N17 C45 106.0(12) . .
C25 O1 Pr1 137.0(3) . .
C28 O2 Pr1 130.3(2) . .
C31 O3 Pr1 135.6(3) . .
C34 O4 Pr1 147.8(3) . .
C37 O5 Pr1 132.8(3) . .
H8A O1W H8B 109.2 . .
H9A O2W H9C 110.9 . .
H10A O3W H10B 109.1 . .
H11A O4W H11B 110.2 . .
H12D O5W H12A 111.0 . .
O1 Pr1 O2 138.04(10) . .
O1 Pr1 O3 138.37(10) . .
O2 Pr1 O3 74.58(9) . .
O1 Pr1 O5 87.05(11) . .
O2 Pr1 O5 73.52(9) . .
O3 Pr1 O5 78.87(10) . .
O1 Pr1 O4 80.31(11) . .
O2 Pr1 O4 137.32(11) . .
O3 Pr1 O4 85.32(11) . .
O5 Pr1 O4 139.24(10) . .
O1 Pr1 N10 133.12(12) . .
O2 Pr1 N10 70.21(11) . .
O3 Pr1 N10 73.95(11) . .
O5 Pr1 N10 139.13(11) . .
O4 Pr1 N10 68.16(12) . .
O1 Pr1 N4 70.37(10) . 2_746
O2 Pr1 N4 131.18(11) . 2_746
O3 Pr1 N4 68.00(10) . 2_746
O5 Pr1 N4 69.51(11) . 2_746
O4 Pr1 N4 69.74(11) . 2_746
N10 Pr1 N4 124.41(12) . 2_746
O1 Pr1 N1 67.39(10) . .
O2 Pr1 N1 71.38(10) . .
O3 Pr1 N1 140.47(10) . .
O5 Pr1 N1 72.74(11) . .
O4 Pr1 N1 133.86(11) . .
N10 Pr1 N1 111.60(12) . .
N4 Pr1 N1 123.65(11) 2_746 .
O1 Pr1 N9 77.07(11) . .
O2 Pr1 N9 97.23(10) . .
O3 Pr1 N9 133.09(11) . .
O5 Pr1 N9 144.13(11) . .
O4 Pr1 N9 69.77(11) . .
N10 Pr1 N9 60.17(12) . .
N4 Pr1 N9 131.23(11) 2_746 .
N1 Pr1 N9 71.48(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.123(5) .
C1 W1 2.225(4) .
C2 N2 1.188(7) .
C2 W1 2.118(5) .
C3 N3 1.200(6) .
C3 W1 2.148(4) .
C4 N4 1.193(6) .
C4 W1 2.117(5) .
C5 N5 1.180(6) .
C5 W1 2.152(5) .
C6 N6 1.175(6) .
C6 W1 2.150(5) .
C7 N7 1.122(6) .
C7 W1 2.144(4) .
C8 N8 1.146(6) .
C8 W1 2.154(4) .
C9 N9 1.371(6) .
C9 C10 1.411(7) .
C9 H9 0.9300 .
C10 C11 1.361(7) .
C10 C21 1.526(7) .
C11 C12 1.403(7) .
C11 C22 1.549(7) .
C12 C20 1.415(6) .
C12 C13 1.432(7) .
C20 N9 1.377(6) .
C20 C19 1.388(7) .
N9 Pr1 2.680(4) .
C13 C14 1.372(8) .
C13 H13 0.9300 .
C14 C15 1.388(8) .
C14 H14 0.9300 .
C15 C16 1.418(7) .
C15 C19 1.430(7) .
C16 C17 1.369(8) .
C16 C23 1.528(7) .
C17 C18 1.412(7) .
C17 C24 1.525(7) .
C18 N10 1.341(6) .
C18 H18 0.9300 .
C19 N10 1.357(6) .
C21 H21A 0.9600 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
C22 H22A 0.9600 .
C22 H22B 0.9600 .
C22 H22C 0.9600 .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C24 H24A 0.9600 .
C24 H24B 0.9600 .
C24 H24C 0.9600 .
C25 O1 1.250(6) .
C25 N11 1.301(7) .
C25 H25 0.9300 .
C26 N11 1.427(8) .
C26 H26A 0.9600 .
C26 H26B 0.9600 .
C26 H26C 0.9600 .
C27 N11 1.489(8) .
C27 H27A 0.9600 .
C27 H27B 0.9600 .
C27 H27C 0.9600 .
C28 O2 1.272(5) .
C28 N12 1.313(5) .
C28 H28 0.9300 .
C29 N12 1.452(5) .
C29 H29A 0.9600 .
C29 H29B 0.9600 .
C29 H29C 0.9600 .
C30 N12 1.505(6) .
C30 H30B 0.9600 .
C30 H30C 0.9600 .
C30 H30A 0.9600 .
C31 O3 1.277(5) .
C31 N13 1.323(6) .
C31 H31 0.9300 .
C32 N13 1.439(6) .
C32 H32A 0.9600 .
C32 H32B 0.9600 .
C32 H32C 0.9600 .
C33 N13 1.477(6) .
C33 H33A 0.9600 .
C33 H33B 0.9600 .
C33 H33C 0.9600 .
C34 O4 1.207(6) .
C34 N14 1.341(8) .
C34 H34 0.9300 .
C35 N14 1.512(8) .
C35 H35A 0.9600 .
C35 H35B 0.9600 .
C35 H35C 0.9600 .
C36 N14 1.456(7) .
C36 H36A 0.9600 .
C36 H36B 0.9600 .
C36 H36C 0.9600 .
C37 O5 1.229(5) .
C37 N15 1.371(6) .
C37 H37 0.9300 .
C38 N15 1.444(6) .
C38 H38A 0.9600 .
C38 H38B 0.9600 .
C38 H38C 0.9600 .
C39 N15 1.470(6) .
C39 H39B 0.9600 .
C39 H39C 0.9600 .
C39 H39A 0.9600 .
C40 O6 1.298(15) .
C40 N16 1.363(14) .
C40 H40 0.9300 .
C41 N16 1.515(19) .
C41 H41A 0.9600 .
C41 H41B 0.9600 .
C41 H41C 0.9600 .
C42 N16 1.445(16) .
C42 H42A 0.9600 .
C42 H42B 0.9600 .
C42 H42C 0.9600 .
C43 O7 1.211(17) .
C43 N17 1.246(18) .
C43 H43 0.9300 .
C44 N17 1.340(19) .
C44 H44A 0.9600 .
C44 H44B 0.9600 .
C44 H44C 0.9600 .
C45 N17 1.482(15) .
C45 H45A 0.9600 .
C45 H45B 0.9600 .
C45 H45C 0.9600 .
N1 Pr1 2.678(4) .
N4 Pr1 2.656(4) 2_756
N10 Pr1 2.642(4) .
O1 Pr1 2.415(3) .
O2 Pr1 2.447(3) .
O3 Pr1 2.448(3) .
O4 Pr1 2.470(3) .
O5 Pr1 2.462(3) .
O1W H8A 0.8607 .
O1W H8B 0.8367 .
O2W H9A 0.8484 .
O2W H9C 0.8533 .
O3W H10A 0.8573 .
O3W H10B 0.8397 .
O4W H11A 0.8614 .
O4W H11B 0.8455 .
O5W H12D 0.8514 .
O5W H12A 0.8570 .
Pr1 N4 2.656(4) 2_746
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_4
N9 C9 C10 C11 -0.7(8) .
N9 C9 C10 C21 178.8(4) .
C9 C10 C11 C12 0.0(7) .
C21 C10 C11 C12 -179.5(5) .
C9 C10 C11 C22 177.8(4) .
C21 C10 C11 C22 -1.7(7) .
C10 C11 C12 C20 0.5(7) .
C22 C11 C12 C20 -177.3(4) .
C10 C11 C12 C13 -178.8(5) .
C22 C11 C12 C13 3.5(7) .
C11 C12 C20 N9 -0.2(7) .
C13 C12 C20 N9 179.1(4) .
C11 C12 C20 C19 -178.7(4) .
C13 C12 C20 C19 0.6(7) .
C10 C9 N9 C20 1.0(7) .
C10 C9 N9 Pr1 -158.7(4) .
C19 C20 N9 C9 178.0(4) .
C12 C20 N9 C9 -0.5(7) .
C19 C20 N9 Pr1 -21.5(5) .
C12 C20 N9 Pr1 159.9(3) .
C11 C12 C13 C14 -179.4(5) .
C20 C12 C13 C14 1.4(8) .
C12 C13 C14 C15 -5.0(8) .
C13 C14 C15 C16 -175.9(5) .
C13 C14 C15 C19 6.6(8) .
C14 C15 C16 C17 174.8(5) .
C19 C15 C16 C17 -7.7(8) .
C14 C15 C16 C23 -3.6(9) .
C19 C15 C16 C23 174.0(5) .
C15 C16 C17 C18 9.5(8) .
C23 C16 C17 C18 -172.1(5) .
C15 C16 C17 C24 -172.7(5) .
C23 C16 C17 C24 5.7(9) .
C16 C17 C18 N10 -4.8(8) .
C24 C17 C18 N10 177.2(4) .
N9 C20 C19 N10 -0.7(6) .
C12 C20 C19 N10 177.9(4) .
N9 C20 C19 C15 -177.5(4) .
C12 C20 C19 C15 1.0(7) .
C14 C15 C19 N10 178.8(5) .
C16 C15 C19 N10 1.2(7) .
C14 C15 C19 C20 -4.5(8) .
C16 C15 C19 C20 177.9(5) .
C17 C18 N10 C19 -2.2(7) .
C17 C18 N10 Pr1 161.3(4) .
C20 C19 N10 C18 -173.0(4) .
C15 C19 N10 C18 3.8(7) .
C20 C19 N10 Pr1 23.3(5) .
C15 C19 N10 Pr1 -159.9(4) .
O1 C25 N11 C26 -175.6(5) .
O1 C25 N11 C27 -1.5(9) .
O2 C28 N12 C29 3.4(6) .
O2 C28 N12 C30 -177.2(4) .
O3 C31 N13 C32 2.7(7) .
O3 C31 N13 C33 -176.5(4) .
O4 C34 N14 C36 -177.0(6) .
O4 C34 N14 C35 -9.2(9) .
O5 C37 N15 C38 179.2(5) .
O5 C37 N15 C39 -7.2(8) .
O6 C40 N16 C42 170.3(12) .
O6 C40 N16 C41 5.9(17) .
O7 C43 N17 C44 -176.6(13) .
O7 C43 N17 C45 -17(2) .
N11 C25 O1 Pr1 173.0(4) .
N12 C28 O2 Pr1 -179.5(3) .
N13 C31 O3 Pr1 -116.7(4) .
N14 C34 O4 Pr1 126.1(6) .
N15 C37 O5 Pr1 131.6(4) .
C25 O1 Pr1 O2 -100.7(5) .
C25 O1 Pr1 O3 30.0(6) .
C25 O1 Pr1 O5 -39.6(5) .
C25 O1 Pr1 O4 101.5(5) .
C25 O1 Pr1 N10 148.9(5) .
C25 O1 Pr1 N4 29.7(5) 2_746
C25 O1 Pr1 N1 -112.1(5) .
C25 O1 Pr1 N9 172.8(5) .
C28 O2 Pr1 O1 29.9(4) .
C28 O2 Pr1 O3 -118.6(3) .
C28 O2 Pr1 O5 -36.0(3) .
C28 O2 Pr1 O4 176.4(3) .
C28 O2 Pr1 N10 163.2(3) .
C28 O2 Pr1 N4 -77.9(3) 2_746
C28 O2 Pr1 N1 40.9(3) .
C28 O2 Pr1 N9 108.6(3) .
C31 O3 Pr1 O1 -37.6(4) .
C31 O3 Pr1 O2 110.7(4) .
C31 O3 Pr1 O5 34.9(4) .
C31 O3 Pr1 O4 -107.3(4) .
C31 O3 Pr1 N10 -175.9(4) .
C31 O3 Pr1 N4 -37.3(4) 2_746
C31 O3 Pr1 N1 79.4(4) .
C31 O3 Pr1 N9 -163.8(4) .
C37 O5 Pr1 O1 -4.6(4) .
C37 O5 Pr1 O2 137.7(4) .
C37 O5 Pr1 O3 -145.2(4) .
C37 O5 Pr1 O4 -76.1(4) .
C37 O5 Pr1 N10 165.9(4) .
C37 O5 Pr1 N4 -74.7(4) 2_746
C37 O5 Pr1 N1 62.6(4) .
C37 O5 Pr1 N9 58.4(4) .
C34 O4 Pr1 O1 -69.8(7) .
C34 O4 Pr1 O2 132.2(7) .
C34 O4 Pr1 O3 71.0(7) .
C34 O4 Pr1 O5 4.1(8) .
C34 O4 Pr1 N10 145.6(8) .
C34 O4 Pr1 N4 2.7(7) 2_746
C34 O4 Pr1 N1 -114.9(7) .
C34 O4 Pr1 N9 -149.5(8) .
C18 N10 Pr1 O1 -159.7(3) .
C19 N10 Pr1 O1 3.7(4) .
C18 N10 Pr1 O2 62.1(3) .
C19 N10 Pr1 O2 -134.5(4) .
C18 N10 Pr1 O3 -16.9(3) .
C19 N10 Pr1 O3 146.5(4) .
C18 N10 Pr1 O5 33.3(4) .
C19 N10 Pr1 O5 -163.3(3) .
C18 N10 Pr1 O4 -108.3(4) .
C19 N10 Pr1 O4 55.1(3) .
C18 N10 Pr1 N4 -64.9(4) 2_746
C19 N10 Pr1 N4 98.5(3) 2_746
C18 N10 Pr1 N1 121.6(3) .
C19 N10 Pr1 N1 -75.0(3) .
C18 N10 Pr1 N9 173.2(4) .
C19 N10 Pr1 N9 -23.4(3) .
C1 N1 Pr1 O1 76.0(15) .
C1 N1 Pr1 O2 -96.0(15) .
C1 N1 Pr1 O3 -64.1(15) .
C1 N1 Pr1 O5 -18.0(15) .
C1 N1 Pr1 O4 125.2(15) .
C1 N1 Pr1 N10 -154.8(15) .
C1 N1 Pr1 N4 31.6(15) 2_746
C1 N1 Pr1 N9 159.4(15) .
C9 N9 Pr1 O1 22.4(3) .
C20 N9 Pr1 O1 -137.6(3) .
C9 N9 Pr1 O2 -115.4(3) .
C20 N9 Pr1 O2 84.7(3) .
C9 N9 Pr1 O3 169.0(3) .
C20 N9 Pr1 O3 9.0(4) .
C9 N9 Pr1 O5 -43.6(4) .
C20 N9 Pr1 O5 156.4(3) .
C9 N9 Pr1 O4 106.7(3) .
C20 N9 Pr1 O4 -53.3(3) .
C9 N9 Pr1 N10 -177.6(4) .
C20 N9 Pr1 N10 22.5(3) .
C9 N9 Pr1 N4 71.1(4) 2_746
C20 N9 Pr1 N4 -88.9(3) 2_746
C9 N9 Pr1 N1 -47.8(3) .
C20 N9 Pr1 N1 152.2(3) .
