#------------------------------------------------------------------------------
#$Date: 2015-05-08 18:26:18 +0300 (Fri, 08 May 2015) $
#$Revision: 135743 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/01/7220171.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_7220171
loop_
_publ_author_name
'Wang, Haoze'
'Wei, Peifa'
'Yan, Xuzhou'
_publ_section_title
;
 [n]Pseudorotaxanes constructed by a bis(p-phenylene)-34-crown-10-based
 cryptand: different binding behaviors induced by minor structural changes
 of guests
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA06927K
_journal_year                    2015
_chemical_formula_moiety         'F6 P, C37 H45 N O14, C7 H9 N, C2 H3 N, H2 O'
_chemical_formula_sum            'C46 H59 F6 N3 O15 P'
_chemical_formula_weight         1038.93
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-05-08
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2015-01-29 deposited with the CCDC.
2015-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                101.306(4)
_cell_angle_beta                 99.715(4)
_cell_angle_gamma                94.513(4)
_cell_formula_units_Z            2
_cell_length_a                   10.9381(5)
_cell_length_b                   11.7474(7)
_cell_length_c                   19.8477(9)
_cell_measurement_reflns_used    3398
_cell_measurement_temperature    170.1
_cell_measurement_theta_max      29.5932
_cell_measurement_theta_min      2.9889
_cell_volume                     2448.4(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      170.1
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0249641000
_diffrn_orient_matrix_UB_12      0.0502574000
_diffrn_orient_matrix_UB_13      0.0157963000
_diffrn_orient_matrix_UB_21      -0.0343277000
_diffrn_orient_matrix_UB_22      -0.0347147000
_diffrn_orient_matrix_UB_23      0.0174854000
_diffrn_orient_matrix_UB_31      0.0508470000
_diffrn_orient_matrix_UB_32      0.0105758000
_diffrn_orient_matrix_UB_33      0.0286671000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.0731
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15160
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.99
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.150
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1090
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         8937
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1816
_refine_ls_wR_factor_ref         0.2234
_reflns_number_gt                5447
_reflns_number_total             8937
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra06927k2.cif
_cod_data_source_block           140507_ljy_046_b_g4
_cod_database_code               7220171
_chemical_oxdiff_formula         'c10 h10 n2 o8 p1 f6'
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C44-C40
 1.51 with sigma of 0.02
 C40-C44A
 1.51 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C44) = Uanis(C44A)
4. Others
 Sof(H33C)=Sof(H33D)=Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(C34A)=Sof(H34C)=
 Sof(H34D)=Sof(O12A)=1-FVAR(1)
 Sof(O12)=Sof(H33A)=Sof(H33B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C34)=Sof(H34A)=
 Sof(H34B)=FVAR(1)
 Sof(C44A)=Sof(H44C)=Sof(H44D)=1-FVAR(2)
 Sof(C44)=Sof(H44A)=Sof(H44B)=FVAR(2)
5.a Free rotating group:
 O15(H15C,H15D)
5.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C14(H14A,H14B), C28(H28A,H28B), C21(H21A,H21B), C19(H19A,
 H19B), C20(H20A,H20B), C18(H18A,H18B), C16(H16A,H16B), C15(H15A,H15B),
 C31(H31A,H31B), C7(H7A,H7B), C17(H17A,H17B), C37(H37A,H37B), C36(H36A,H36B),
 C33(H33A,H33B), C33(H33C,H33D), C32(H32A,H32B), C35(H35A,H35B), C34(H34A,H34B),
  C44(H44A,H44B), C35A(H35C,H35D), C34A(H34C,H34D), C44A(H44C,H44D)
5.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C11(H11), C9(H9), C23(H23), C26(H26), C12(H12), C2(H2), C3(H3),
 C4(H4), C42(H42), C38(H38), C41(H41), C39(H39)
5.d Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C46(H46A,H46B,H46C)
;
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
P1 P 1.64047(10) 1.62909(10) 1.22787(5) 0.0539(3) Uani 1 d . . .
O3 O 1.3333(2) 1.0540(2) 0.93323(10) 0.0426(6) Uani 1 d . . .
O7 O 0.7252(2) 1.1956(2) 0.94354(10) 0.0403(6) Uani 1 d . . .
O10 O 0.5215(2) 0.8418(2) 0.71456(10) 0.0408(6) Uani 1 d . . .
O6 O 0.9069(2) 1.3670(2) 1.03508(10) 0.0384(6) Uani 1 d . . .
O8 O 0.68371(19) 1.0082(2) 0.65046(9) 0.0362(5) Uani 1 d . . .
O14 O 1.1367(2) 0.7003(2) 0.70344(11) 0.0465(6) Uani 1 d A . .
O2 O 1.0962(2) 0.9154(2) 0.64136(10) 0.0406(6) Uani 1 d . . .
O4 O 1.3394(2) 1.2685(2) 1.03032(11) 0.0433(6) Uani 1 d . . .
O11 O 0.5018(2) 0.6177(2) 0.60796(12) 0.0506(7) Uani 1 d . . .
O5 O 1.1722(2) 1.4096(2) 1.09260(10) 0.0420(6) Uani 1 d . . .
C27 C 0.6429(3) 1.0002(3) 0.89639(15) 0.0355(8) Uani 1 d . . .
H27 H 0.6540 0.9878 0.9428 0.043 Uiso 1 calc . . R
C24 C 0.6119(3) 1.0353(3) 0.76062(14) 0.0307(7) Uani 1 d . . .
C25 C 0.5749(3) 0.9253(3) 0.77309(15) 0.0335(7) Uani 1 d . . .
C10 C 1.2841(3) 0.9690(3) 0.87488(15) 0.0367(8) Uani 1 d . . .
N1 N 0.8672(3) 0.9403(3) 0.57792(12) 0.0392(7) Uani 1 d . . .
C30 C 0.4832(3) 0.7269(3) 0.72434(16) 0.0392(8) Uani 1 d . . .
H30A H 0.4246 0.7323 0.7575 0.047 Uiso 1 calc . . R
H30B H 0.5569 0.6920 0.7441 0.047 Uiso 1 calc . . R
C22 C 0.6784(3) 1.1097(3) 0.88508(14) 0.0313(7) Uani 1 d . . .
O9 O 0.5980(2) 1.0838(2) 0.56089(11) 0.0508(7) Uani 1 d . . .
C11 C 1.2430(3) 0.8610(3) 0.88615(16) 0.0385(8) Uani 1 d . . .
H11 H 1.2491 0.8494 0.9326 0.046 Uiso 1 calc . . R
C13 C 1.1820(3) 0.7855(3) 0.76200(15) 0.0380(8) Uani 1 d . . .
C9 C 1.2738(3) 0.9857(3) 0.80638(15) 0.0359(8) Uani 1 d . . .
H9 H 1.3015 1.0597 0.7983 0.043 Uiso 1 calc . . R
C23 C 0.6634(3) 1.1268(3) 0.81707(15) 0.0336(7) Uani 1 d . . .
H23 H 0.6884 1.2014 0.8089 0.040 Uiso 1 calc . . R
C8 C 1.2233(3) 0.8944(3) 0.75009(15) 0.0355(8) Uani 1 d . . .
C26 C 0.5914(3) 0.9080(3) 0.84078(15) 0.0366(8) Uani 1 d . . .
H26 H 0.5676 0.8334 0.8493 0.044 Uiso 1 calc . . R
C14 C 1.3775(3) 1.1655(3) 0.92172(16) 0.0393(8) Uani 1 d . . .
H14A H 1.3072 1.2002 0.8980 0.047 Uiso 1 calc . . R
H14B H 1.4405 1.1558 0.8913 0.047 Uiso 1 calc . . R
C1 C 0.7584(3) 0.9612(3) 0.54370(15) 0.0383(8) Uani 1 d . . .
C29 C 0.6723(3) 1.0256(3) 0.58527(14) 0.0355(8) Uani 1 d . . .
C28 C 0.5894(3) 1.0586(3) 0.68825(14) 0.0364(8) Uani 1 d . . .
H28A H 0.5048 1.0231 0.6632 0.044 Uiso 1 calc . . R
H28B H 0.5949 1.1438 0.6907 0.044 Uiso 1 calc . . R
C21 C 0.7467(3) 1.3127(3) 0.93354(15) 0.0373(8) Uani 1 d . . .
H21A H 0.6690 1.3357 0.9091 0.045 Uiso 1 calc . . R
H21B H 0.8117 1.3176 0.9047 0.045 Uiso 1 calc . . R
C19 C 0.9650(3) 1.4583(3) 1.09216(15) 0.0396(8) Uani 1 d . . .
H19A H 0.9050 1.4800 1.1234 0.048 Uiso 1 calc . . R
H19B H 0.9909 1.5280 1.0746 0.048 Uiso 1 calc . . R
C12 C 1.1932(3) 0.7703(3) 0.83055(16) 0.0411(8) Uani 1 d . . .
H12 H 1.1661 0.6964 0.8390 0.049 Uiso 1 calc . . R
C20 C 0.7883(3) 1.3920(3) 1.00344(15) 0.0383(8) Uani 1 d . . .
H20A H 0.7940 1.4743 0.9983 0.046 Uiso 1 calc . . R
H20B H 0.7267 1.3814 1.0336 0.046 Uiso 1 calc . . R
C18 C 1.0767(3) 1.4190(3) 1.13209(16) 0.0434(9) Uani 1 d . . .
H18A H 1.1069 1.4758 1.1769 0.052 Uiso 1 calc . . R
H18B H 1.0532 1.3422 1.1428 0.052 Uiso 1 calc . . R
C16 C 1.3802(3) 1.3654(3) 1.08678(16) 0.0406(8) Uani 1 d . . .
H16A H 1.3949 1.4371 1.0688 0.049 Uiso 1 calc . . R
H16B H 1.4596 1.3528 1.1151 0.049 Uiso 1 calc . . R
C15 C 1.4340(3) 1.2441(4) 0.99029(17) 0.0457(9) Uani 1 d . . .
H15A H 1.4990 1.2061 1.0159 0.055 Uiso 1 calc . . R
H15B H 1.4739 1.3179 0.9826 0.055 Uiso 1 calc . . R
C31 C 0.4203(3) 0.6512(3) 0.65493(17) 0.0447(9) Uani 1 d . . .
H31A H 0.3767 0.5798 0.6634 0.054 Uiso 1 calc . . R
H31B H 0.3563 0.6939 0.6323 0.054 Uiso 1 calc . . R
O13 O 0.9417(3) 0.5425(3) 0.60578(14) 0.0721(9) Uani 1 d . . .
C5 C 0.9414(3) 0.8839(3) 0.53904(16) 0.0438(9) Uani 1 d . . .
C7 C 1.2229(3) 0.9104(3) 0.67694(16) 0.0430(9) Uani 1 d . . .
H7A H 1.2757 0.9835 0.6783 0.052 Uiso 1 calc . . R
H7B H 1.2586 0.8445 0.6507 0.052 Uiso 1 calc . . R
C17 C 1.2817(3) 1.3789(3) 1.13105(16) 0.0427(8) Uani 1 d . . .
H17A H 1.2621 1.3047 1.1456 0.051 Uiso 1 calc . . R
H17B H 1.3130 1.4405 1.1737 0.051 Uiso 1 calc . . R
O1 O 1.1390(3) 0.8124(3) 0.54167(13) 0.0769(10) Uani 1 d . . .
C37 C 1.0870(4) 0.5898(3) 0.71388(18) 0.0488(9) Uani 1 d . . .
H37A H 1.0154 0.6003 0.7382 0.059 Uiso 1 calc A . R
H37B H 1.1517 0.5573 0.7434 0.059 Uiso 1 calc . . R
C2 C 0.7168(3) 0.9267(3) 0.47228(15) 0.0434(9) Uani 1 d . . .
H2 H 0.6385 0.9445 0.4507 0.052 Uiso 1 calc . . R
C6 C 1.0685(3) 0.8651(4) 0.57346(17) 0.0485(10) Uani 1 d . . .
C36 C 1.0458(4) 0.5082(4) 0.64503(18) 0.0544(10) Uani 1 d A . .
H36A H 1.1151 0.5056 0.6187 0.065 Uiso 1 calc . . R
H36B H 1.0246 0.4286 0.6524 0.065 Uiso 1 calc . . R
O12 O 0.7104(7) 0.5906(8) 0.5550(4) 0.062(2) Uani 0.611(9) d A 1 .
F2 F 1.6263(3) 1.4916(2) 1.20997(15) 0.1120(12) Uani 1 d . . .
C3 C 0.7937(4) 0.8648(4) 0.43318(17) 0.0547(10) Uani 1 d . . .
H3 H 0.7679 0.8374 0.3841 0.066 Uiso 1 calc . . R
C33 C 0.6102(4) 0.6471(4) 0.51866(18) 0.0551(10) Uani 1 d . . .
H33A H 0.5563 0.5882 0.4805 0.066 Uiso 0.611(9) calc A 1 R
H33B H 0.6478 0.7079 0.4977 0.066 Uiso 0.611(9) calc A 1 R
H33C H 0.5770 0.5644 0.4984 0.066 Uiso 0.389(9) calc A 2 R
H33D H 0.6094 0.6895 0.4801 0.066 Uiso 0.389(9) calc A 2 R
C4 C 0.9076(4) 0.8442(4) 0.46679(17) 0.0538(10) Uani 1 d . . .
H4 H 0.9626 0.8034 0.4412 0.065 Uiso 1 calc . . R
F5 F 1.5684(5) 1.6301(3) 1.15317(18) 0.1593(19) Uani 1 d . . .
F4 F 1.7091(4) 1.6282(3) 1.30280(13) 0.1098(12) Uani 1 d . . .
C32 C 0.5334(4) 0.7013(3) 0.5691(2) 0.0581(11) Uani 1 d A . .
H32A H 0.5814 0.7721 0.6010 0.070 Uiso 1 calc . . R
H32B H 0.4566 0.7242 0.5436 0.070 Uiso 1 calc . . R
F3 F 1.6567(4) 1.7670(3) 1.24725(16) 0.1187(13) Uani 1 d . . .
C35 C 0.8777(6) 0.4737(6) 0.5510(3) 0.052(2) Uani 0.611(9) d A 1 .
H35A H 0.8312 0.4091 0.5649 0.062 Uiso 0.611(9) calc A 1 R
H35B H 0.9350 0.4393 0.5211 0.062 Uiso 0.611(9) calc A 1 R
F1 F 1.7652(4) 1.6334(4) 1.2029(2) 0.1635(18) Uani 1 d . . .
C34 C 0.7862(8) 0.5364(9) 0.5094(4) 0.056(2) Uani 0.611(9) d A 1 .
H34A H 0.8319 0.5960 0.4910 0.067 Uiso 0.611(9) calc A 1 R
H34B H 0.7337 0.4799 0.4694 0.067 Uiso 0.611(9) calc A 1 R
F6 F 1.5125(4) 1.6228(6) 1.2484(4) 0.220(3) Uani 1 d . . .
N2 N 0.9942(3) 1.1141(3) 0.78807(14) 0.0442(7) Uani 1 d . . .
C43 C 1.0032(4) 1.1504(4) 0.72252(18) 0.0558(10) Uani 1 d . . .
H43A H 0.9585 1.2189 0.7198 0.084 Uiso 1 calc . . GR
H43B H 0.9659 1.0863 0.6830 0.084 Uiso 1 calc . . GR
H43C H 1.0912 1.1701 0.7208 0.084 Uiso 1 calc . . GR
C42 C 1.0337(3) 1.1906(4) 0.84931(18) 0.0551(11) Uani 1 d . . .
H42 H 1.0659 1.2684 0.8500 0.066 Uiso 1 calc . . R
C38 C 0.9482(4) 1.0051(4) 0.7865(2) 0.0576(11) Uani 1 d . . .
H38 H 0.9208 0.9524 0.7426 0.069 Uiso 1 calc . . R
C40 C 0.9787(5) 1.0409(8) 0.9102(3) 0.103(2) Uani 1 d . . D
C41 C 1.0273(5) 1.1556(6) 0.9115(2) 0.0839(18) Uani 1 d . . .
H41 H 1.0558 1.2091 0.9550 0.101 Uiso 1 calc . . R
C39 C 0.9396(5) 0.9677(5) 0.8460(3) 0.0815(16) Uani 1 d . . .
H39 H 0.9059 0.8895 0.8431 0.098 Uiso 1 calc . . R
N3 N 0.8014(4) 1.3433(4) 0.7276(2) 0.0769(11) Uani 1 d . . .
C45 C 0.7281(5) 1.3628(4) 0.6861(2) 0.0679(12) Uani 1 d . . .
C46 C 0.6327(7) 1.3845(6) 0.6310(3) 0.134(3) Uani 1 d . . .
H46A H 0.6674 1.3832 0.5884 0.201 Uiso 1 calc . . GR
H46B H 0.6048 1.4611 0.6460 0.201 Uiso 1 calc . . GR
H46C H 0.5616 1.3237 0.6213 0.201 Uiso 1 calc . . GR
O15 O 0.8190(5) 0.7384(4) 0.70728(17) 0.1132(14) Uani 1 d . . .
H15C H 0.7747 0.7895 0.6947 0.170 Uiso 1 d . . G
H15D H 0.8388 0.6966 0.6716 0.170 Uiso 1 d . . G
C44 C 0.9585(9) 0.9761(9) 0.9688(5) 0.086(2) Uani 0.610(9) d . 1 D
H44A H 0.8719 0.9802 0.9768 0.103 Uiso 0.610(9) calc . 1 R
H44B H 0.9696 0.8927 0.9537 0.103 Uiso 0.610(9) calc . 1 R
C35A C 0.9372(8) 0.6098(9) 0.5626(5) 0.047(3) Uani 0.389(9) d A 2 .
H35C H 1.0010 0.5920 0.5333 0.056 Uiso 0.389(9) calc A 2 R
H35D H 0.9590 0.6916 0.5891 0.056 Uiso 0.389(9) calc A 2 R
C34A C 0.8138(13) 0.6001(11) 0.5160(6) 0.045(3) Uani 0.389(9) d A 2 .
H34C H 0.8219 0.6388 0.4767 0.054 Uiso 0.389(9) calc A 2 R
H34D H 0.7824 0.5167 0.4963 0.054 Uiso 0.389(9) calc A 2 R
O12A O 0.7277(10) 0.6546(9) 0.5555(5) 0.047(2) Uani 0.389(9) d A 2 .
C44A C 1.0057(15) 1.0598(16) 0.9944(6) 0.086(2) Uani 0.390(9) d . 2 D
H44C H 1.0904 1.1004 1.0149 0.103 Uiso 0.390(9) calc . 2 R
H44D H 0.9435 1.1053 1.0149 0.103 Uiso 0.390(9) calc . 2 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'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 '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
F2 P1 F3 178.81(16) .
F5 P1 F2 90.56(17) .
F5 P1 F3 90.60(17) .
F4 P1 F2 89.48(15) .
F4 P1 F5 178.6(3) .
F4 P1 F3 89.36(16) .
F1 P1 F2 90.7(2) .
F1 P1 F5 91.1(3) .
F1 P1 F4 90.3(3) .
F1 P1 F3 89.1(2) .
F6 P1 F2 88.5(3) .
F6 P1 F5 85.7(3) .
F6 P1 F4 92.9(3) .
F6 P1 F3 91.8(3) .
F6 P1 F1 176.7(3) .
C10 O3 C14 116.7(2) .
C22 O7 C21 117.2(2) .
C25 O10 C30 117.6(2) .
C19 O6 C20 111.6(2) .
C29 O8 C28 113.6(2) .
C13 O14 C37 117.0(2) .
C6 O2 C7 116.2(2) .
C16 O4 C15 111.3(3) .
C32 O11 C31 115.7(3) .
C18 O5 C17 111.1(2) .
C22 C27 H27 119.5 .
C22 C27 C26 121.0(3) .
C26 C27 H27 119.5 .
C25 C24 C28 121.2(3) .
C23 C24 C25 119.4(3) .
C23 C24 C28 119.2(3) .
O10 C25 C24 115.3(2) .
O10 C25 C26 124.8(3) .
C26 C25 C24 119.9(3) .
O3 C10 C11 116.6(3) .
O3 C10 C9 124.0(3) .
C11 C10 C9 119.4(3) .
C1 N1 C5 116.5(3) .
O10 C30 H30A 109.8 .
O10 C30 H30B 109.8 .
O10 C30 C31 109.2(3) .
H30A C30 H30B 108.3 .
C31 C30 H30A 109.8 .
C31 C30 H30B 109.8 .
O7 C22 C27 116.5(2) .
O7 C22 C23 124.2(3) .
C27 C22 C23 119.3(3) .
C10 C11 H11 119.8 .
C12 C11 C10 120.5(3) .
C12 C11 H11 119.8 .
O14 C13 C8 115.7(3) .
O14 C13 C12 125.1(3) .
C12 C13 C8 119.1(3) .
C10 C9 H9 119.9 .
C8 C9 C10 120.2(3) .
C8 C9 H9 119.9 .
C24 C23 H23 119.7 .
C22 C23 C24 120.5(3) .
C22 C23 H23 119.7 .
C13 C8 C7 120.3(3) .
C9 C8 C13 119.9(3) .
C9 C8 C7 119.6(3) .
C27 C26 H26 120.1 .
C25 C26 C27 119.9(3) .
C25 C26 H26 120.1 .
O3 C14 H14A 109.8 .
O3 C14 H14B 109.8 .
O3 C14 C15 109.2(3) .
H14A C14 H14B 108.3 .
C15 C14 H14A 109.8 .
C15 C14 H14B 109.8 .
N1 C1 C29 118.4(3) .
N1 C1 C2 124.9(3) .
C2 C1 C29 116.7(3) .
O8 C29 C1 113.5(3) .
O9 C29 O8 123.7(3) .
O9 C29 C1 122.8(3) .
O8 C28 C24 109.1(2) .
O8 C28 H28A 109.9 .
O8 C28 H28B 109.9 .
C24 C28 H28A 109.9 .
C24 C28 H28B 109.9 .
H28A C28 H28B 108.3 .
O7 C21 H21A 110.0 .
O7 C21 H21B 110.0 .
O7 C21 C20 108.3(2) .
H21A C21 H21B 108.4 .
C20 C21 H21A 110.0 .
C20 C21 H21B 110.0 .
O6 C19 H19A 109.7 .
O6 C19 H19B 109.7 .
O6 C19 C18 109.7(3) .
H19A C19 H19B 108.2 .
C18 C19 H19A 109.7 .
C18 C19 H19B 109.7 .
C11 C12 C13 120.8(3) .
C11 C12 H12 119.6 .
C13 C12 H12 119.6 .
O6 C20 C21 109.8(2) .
O6 C20 H20A 109.7 .
O6 C20 H20B 109.7 .
C21 C20 H20A 109.7 .
C21 C20 H20B 109.7 .
H20A C20 H20B 108.2 .
O5 C18 C19 110.1(2) .
O5 C18 H18A 109.6 .
O5 C18 H18B 109.6 .
C19 C18 H18A 109.6 .
C19 C18 H18B 109.6 .
H18A C18 H18B 108.2 .
O4 C16 H16A 109.9 .
O4 C16 H16B 109.9 .
O4 C16 C17 108.7(3) .
H16A C16 H16B 108.3 .
C17 C16 H16A 109.9 .
C17 C16 H16B 109.9 .
O4 C15 C14 109.3(3) .
O4 C15 H15A 109.8 .
O4 C15 H15B 109.8 .
C14 C15 H15A 109.8 .
C14 C15 H15B 109.8 .
H15A C15 H15B 108.3 .
O11 C31 C30 114.8(3) .
O11 C31 H31A 108.6 .
O11 C31 H31B 108.6 .
C30 C31 H31A 108.6 .
C30 C31 H31B 108.6 .
H31A C31 H31B 107.6 .
C35 O13 C36 121.3(4) .
C35A O13 C36 129.4(5) .
C35A O13 C35 79.7(5) .
N1 C5 C6 119.3(3) .
N1 C5 C4 123.1(3) .
C4 C5 C6 117.6(3) .
O2 C7 C8 110.5(2) .
O2 C7 H7A 109.5 .
O2 C7 H7B 109.5 .
C8 C7 H7A 109.5 .
C8 C7 H7B 109.5 .
H7A C7 H7B 108.1 .
O5 C17 C16 109.9(2) .
O5 C17 H17A 109.7 .
O5 C17 H17B 109.7 .
C16 C17 H17A 109.7 .
C16 C17 H17B 109.7 .
H17A C17 H17B 108.2 .
O14 C37 H37A 109.8 .
O14 C37 H37B 109.8 .
O14 C37 C36 109.2(3) .
H37A C37 H37B 108.3 .
C36 C37 H37A 109.8 .
C36 C37 H37B 109.8 .
C1 C2 H2 121.2 .
C1 C2 C3 117.7(3) .
C3 C2 H2 121.2 .
O2 C6 C5 113.1(3) .
O1 C6 O2 124.3(3) .
O1 C6 C5 122.6(3) .
O13 C36 C37 111.5(3) .
O13 C36 H36A 109.3 .
O13 C36 H36B 109.3 .
C37 C36 H36A 109.3 .
C37 C36 H36B 109.3 .
H36A C36 H36B 108.0 .
C34 O12 C33 112.8(6) .
C2 C3 H3 120.6 .
C4 C3 C2 118.8(3) .
C4 C3 H3 120.6 .
O12 C33 H33A 109.6 .
O12 C33 H33B 109.6 .
O12 C33 H33C 81.2 .
O12 C33 H33D 131.0 .
O12 C33 C32 110.1(4) .
H33A C33 H33B 108.1 .
H33A C33 H33C 30.9 .
H33A C33 H33D 80.9 .
H33B C33 H33C 131.2 .
H33B C33 H33D 29.4 .
H33C C33 H33D 108.6 .
C32 C33 H33A 109.6 .
C32 C33 H33B 109.6 .
C32 C33 H33C 110.4 .
C32 C33 H33D 110.4 .
O12A C33 O12 30.6(4) .
O12A C33 H33A 135.1 .
O12A C33 H33B 83.3 .
O12A C33 H33C 110.4 .
O12A C33 H33D 110.4 .
O12A C33 C32 106.4(5) .
C5 C4 H4 120.5 .
C3 C4 C5 119.0(3) .
C3 C4 H4 120.5 .
O11 C32 C33 108.0(3) .
O11 C32 H32A 110.1 .
O11 C32 H32B 110.1 .
C33 C32 H32A 110.1 .
C33 C32 H32B 110.1 .
H32A C32 H32B 108.4 .
O13 C35 H35A 109.2 .
O13 C35 H35B 109.2 .
O13 C35 C34 111.9(6) .
H35A C35 H35B 107.9 .
C34 C35 H35A 109.2 .
C34 C35 H35B 109.2 .
O12 C34 C35 107.8(6) .
O12 C34 H34A 110.2 .
O12 C34 H34B 110.2 .
C35 C34 H34A 110.2 .
C35 C34 H34B 110.2 .
H34A C34 H34B 108.5 .
C42 N2 C43 119.8(4) .
C38 N2 C43 119.6(3) .
C38 N2 C42 120.6(3) .
N2 C43 H43A 109.5 .
N2 C43 H43B 109.5 .
N2 C43 H43C 109.5 .
H43A C43 H43B 109.5 .
H43A C43 H43C 109.5 .
H43B C43 H43C 109.5 .
N2 C42 H42 120.1 .
N2 C42 C41 119.7(5) .
C41 C42 H42 120.1 .
N2 C38 H38 119.3 .
N2 C38 C39 121.5(5) .
C39 C38 H38 119.3 .
C41 C40 C44 132.5(7) .
C41 C40 C44A 93.4(8) .
C39 C40 C41 117.3(4) .
C39 C40 C44 110.2(7) .
C39 C40 C44A 149.1(9) .
C44 C40 C44A 39.2(5) .
C42 C41 C40 119.9(5) .
C42 C41 H41 120.1 .
C40 C41 H41 120.1 .
C38 C39 C40 120.9(6) .
C38 C39 H39 119.5 .
C40 C39 H39 119.5 .
N3 C45 C46 178.2(6) .
C45 C46 H46A 109.5 .
C45 C46 H46B 109.5 .
C45 C46 H46C 109.5 .
H46A C46 H46B 109.5 .
H46A C46 H46C 109.5 .
H46B C46 H46C 109.5 .
H15C O15 H15D 109.5 .
C40 C44 H44A 109.3 .
C40 C44 H44B 109.3 .
C44 C44 C40 111.8(10) 2_777
C44 C44 H44A 109.3 2_777
C44 C44 H44B 109.3 2_777
H44A C44 H44B 107.9 .
O13 C35A H35C 108.7 .
O13 C35A H35D 108.7 .
O13 C35A C34A 114.2(8) .
H35C C35A H35D 107.6 .
C34A C35A H35C 108.7 .
C34A C35A H35D 108.7 .
C35A C34A H34C 109.9 .
C35A C34A H34D 109.9 .
H34C C34A H34D 108.3 .
O12A C34A C35A 109.1(9) .
O12A C34A H34C 109.9 .
O12A C34A H34D 109.9 .
C33 O12A C34A 114.2(8) .
C40 C44A H44C 111.2 .
C40 C44A H44D 111.2 .
C44A C44A C40 103.0(13) 2_777
C44A C44A H44C 111.2 2_777
C44A C44A H44D 111.2 2_777
H44C C44A H44D 109.1 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 F2 1.573(3) .
P1 F5 1.560(3) .
P1 F4 1.551(2) .
P1 F3 1.578(3) .
P1 F1 1.528(4) .
P1 F6 1.523(4) .
O3 C10 1.371(4) .
O3 C14 1.434(4) .
O7 C22 1.373(4) .
O7 C21 1.435(4) .
O10 C25 1.373(4) .
O10 C30 1.442(4) .
O6 C19 1.418(4) .
O6 C20 1.421(4) .
O8 C29 1.336(3) .
O8 C28 1.470(3) .
O14 C13 1.368(4) .
O14 C37 1.433(4) .
O2 C7 1.457(4) .
O2 C6 1.334(4) .
O4 C16 1.415(4) .
O4 C15 1.421(4) .
O11 C31 1.418(4) .
O11 C32 1.418(4) .
O5 C18 1.407(4) .
O5 C17 1.419(4) .
C27 H27 0.9500 .
C27 C22 1.386(5) .
C27 C26 1.390(5) .
C24 C25 1.404(4) .
C24 C23 1.396(4) .
C24 C28 1.498(4) .
C25 C26 1.382(4) .
C10 C11 1.385(5) .
C10 C9 1.399(4) .
N1 C1 1.332(4) .
N1 C5 1.338(4) .
C30 H30A 0.9900 .
C30 H30B 0.9900 .
C30 C31 1.505(5) .
C22 C23 1.388(4) .
O9 C29 1.203(4) .
C11 H11 0.9500 .
C11 C12 1.376(5) .
C13 C8 1.400(5) .
C13 C12 1.393(4) .
C9 H9 0.9500 .
C9 C8 1.390(5) .
C23 H23 0.9500 .
C8 C7 1.499(4) .
C26 H26 0.9500 .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C14 C15 1.490(5) .
C1 C29 1.507(4) .
C1 C2 1.382(4) .
C28 H28A 0.9900 .
C28 H28B 0.9900 .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C21 C20 1.488(5) .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
C19 C18 1.497(5) .
C12 H12 0.9500 .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C16 C17 1.500(4) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C31 H31A 0.9900 .
C31 H31B 0.9900 .
O13 C36 1.400(5) .
O13 C35 1.278(6) .
O13 C35A 1.273(9) .
C5 C6 1.495(5) .
C5 C4 1.394(4) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
O1 C6 1.210(4) .
C37 H37A 0.9900 .
C37 H37B 0.9900 .
C37 C36 1.484(5) .
C2 H2 0.9500 .
C2 C3 1.390(5) .
C36 H36A 0.9900 .
C36 H36B 0.9900 .
O12 C33 1.482(8) .
O12 C34 1.422(11) .
C3 H3 0.9500 .
C3 C4 1.374(5) .
C33 H33A 0.9900 .
C33 H33B 0.9900 .
C33 H33C 0.9900 .
C33 H33D 0.9900 .
C33 C32 1.494(5) .
C33 O12A 1.354(12) .
C4 H4 0.9500 .
C32 H32A 0.9900 .
C32 H32B 0.9900 .
C35 H35A 0.9900 .
C35 H35B 0.9900 .
C35 C34 1.518(12) .
C34 H34A 0.9900 .
C34 H34B 0.9900 .
N2 C43 1.462(4) .
N2 C42 1.344(5) .
N2 C38 1.331(5) .
C43 H43A 0.9800 .
C43 H43B 0.9800 .
C43 H43C 0.9800 .
C42 H42 0.9500 .
C42 C41 1.387(6) .
C38 H38 0.9500 .
C38 C39 1.353(6) .
C40 C41 1.402(9) .
C40 C39 1.370(8) .
C40 C44 1.546(9) .
C40 C44A 1.614(12) .
C41 H41 0.9500 .
C39 H39 0.9500 .
N3 C45 1.120(5) .
C45 C46 1.455(7) .
C46 H46A 0.9800 .
C46 H46B 0.9800 .
C46 H46C 0.9800 .
O15 H15C 0.8499 .
O15 H15D 0.8499 .
C44 C44 1.39(2) 2_777
C44 H44A 0.9900 .
C44 H44B 0.9900 .
C35A H35C 0.9900 .
C35A H35D 0.9900 .
C35A C34A 1.484(17) .
C34A H34C 0.9900 .
C34A H34D 0.9900 .
C34A O12A 1.434(16) .
C44A C44A 1.46(4) 2_777
C44A H44C 0.9900 .
C44A H44D 0.9900 .
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
O3 C10 C11 C12 -179.5(3) .
O3 C10 C9 C8 179.6(3) .
O3 C14 C15 O4 -66.3(3) .
O7 C22 C23 C24 -178.2(3) .
O7 C21 C20 O6 66.1(3) .
O10 C25 C26 C27 -177.8(3) .
O10 C30 C31 O11 71.8(3) .
O6 C19 C18 O5 70.7(4) .
O14 C13 C8 C9 -178.4(2) .
O14 C13 C8 C7 -3.3(4) .
O14 C13 C12 C11 178.3(3) .
O14 C37 C36 O13 -68.3(4) .
O4 C16 C17 O5 -65.9(4) .
C27 C22 C23 C24 0.7(4) .
C24 C25 C26 C27 0.9(4) .
C25 O10 C30 C31 176.6(2) .
C25 C24 C23 C22 0.1(4) .
C25 C24 C28 O8 -78.1(4) .
C10 O3 C14 C15 -176.8(2) .
C10 C11 C12 C13 -0.7(5) .
C10 C9 C8 C13 0.3(4) .
C10 C9 C8 C7 -174.8(3) .
N1 C1 C29 O8 -29.4(4) .
N1 C1 C29 O9 152.8(3) .
N1 C1 C2 C3 0.5(6) .
N1 C5 C6 O2 -3.8(5) .
N1 C5 C6 O1 178.2(4) .
N1 C5 C4 C3 0.9(6) .
C30 O10 C25 C24 179.3(3) .
C30 O10 C25 C26 -1.9(4) .
C22 O7 C21 C20 176.1(2) .
C22 C27 C26 C25 -0.1(4) .
C11 C10 C9 C8 -0.3(4) .
C13 O14 C37 C36 -178.5(3) .
C13 C8 C7 O2 75.0(4) .
C9 C10 C11 C12 0.5(5) .
C9 C8 C7 O2 -110.0(3) .
C23 C24 C25 O10 177.9(2) .
C23 C24 C25 C26 -0.9(4) .
C23 C24 C28 O8 105.9(3) .
C8 C13 C12 C11 0.7(5) .
C26 C27 C22 O7 178.3(2) .
C26 C27 C22 C23 -0.7(5) .
C14 O3 C10 C11 179.2(3) .
C14 O3 C10 C9 -0.7(4) .
C1 N1 C5 C6 175.7(3) .
C1 N1 C5 C4 -2.2(5) .
C1 C2 C3 C4 -1.8(6) .
C29 O8 C28 C24 -179.3(3) .
C29 C1 C2 C3 -178.6(3) .
C28 O8 C29 O9 5.0(5) .
C28 O8 C29 C1 -172.7(3) .
C28 C24 C25 O10 2.0(4) .
C28 C24 C25 C26 -176.9(3) .
C28 C24 C23 C22 176.1(3) .
C21 O7 C22 C27 -171.9(3) .
C21 O7 C22 C23 7.0(4) .
C19 O6 C20 C21 164.5(3) .
C12 C13 C8 C9 -0.5(4) .
C12 C13 C8 C7 174.6(3) .
C20 O6 C19 C18 169.2(2) .
C18 O5 C17 C16 177.9(3) .
C16 O4 C15 C14 -164.4(3) .
C15 O4 C16 C17 -174.3(3) .
C31 O11 C32 C33 -175.3(3) .
O13 C35 C34 O12 -55.5(8) .
O13 C35A C34A O12A 73.5(11) .
C5 N1 C1 C29 -179.4(3) .
C5 N1 C1 C2 1.5(5) .
C7 O2 C6 C5 -174.4(3) .
C7 O2 C6 O1 3.5(5) .
C17 O5 C18 C19 176.6(3) .
C37 O14 C13 C8 -176.5(3) .
C37 O14 C13 C12 5.8(4) .
C2 C1 C29 O8 149.7(3) .
C2 C1 C29 O9 -28.1(5) .
C2 C3 C4 C5 1.2(6) .
C6 O2 C7 C8 -143.3(3) .
C6 C5 C4 C3 -177.0(4) .
C36 O13 C35 C34 -168.8(5) .
C36 O13 C35A C34A 163.4(6) .
O12 C33 C32 O11 -47.9(6) .
O12 C33 O12A C34A 74.6(12) .
C33 O12 C34 C35 -175.5(7) .
C4 C5 C6 O2 174.2(3) .
C4 C5 C6 O1 -3.8(6) .
C32 O11 C31 C30 -82.2(4) .
C32 C33 O12A C34A 176.4(7) .
C35 O13 C36 C37 -166.9(4) .
C35 O13 C35A C34A 41.1(8) .
C34 O12 C33 C32 179.5(5) .
C34 O12 C33 O12A -92.1(12) .
N2 C42 C41 C40 -0.5(6) .
N2 C38 C39 C40 -0.4(6) .
C43 N2 C42 C41 -178.8(3) .
C43 N2 C38 C39 179.2(3) .
C42 N2 C38 C39 0.1(5) .
C38 N2 C42 C41 0.4(5) .
C41 C40 C39 C38 0.2(7) .
C41 C40 C44 C44 -26.4(16) 2_777
C41 C40 C44A C44A -164.5(15) 2_777
C39 C40 C41 C42 0.2(7) .
C39 C40 C44 C44 153.7(11) 2_777
C39 C40 C44A C44A 10(3) 2_777
C44 C40 C41 C42 -179.6(6) .
C44 C40 C39 C38 -179.9(5) .
C44 C40 C44A C44A 19.2(10) 2_777
C35A O13 C36 C37 89.8(7) .
C35A O13 C35 C34 -38.7(7) .
C35A C34A O12A C33 -177.6(9) .
O12A C33 C32 O11 -80.0(6) .
C44A C40 C41 C42 177.2(7) .
C44A C40 C39 C38 -173.8(13) .
C44A C40 C44 C44 -21.3(12) 2_777
