#------------------------------------------------------------------------------
#$Date: 2020-10-06 10:25:03 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257364 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/74/1557449.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_1557449
loop_
_publ_author_name
'Sharma, Mahendra K.'
'Blomeyer, Sebastian'
'Glodde, Timo'
'Neumann, Beate'
'Stammler, Hans-Georg'
'Hinz, Alexander'
'van Gastel, Maurice'
'Ghadwal, Rajendra S.'
_publ_section_title
;
 Isolation of singlet carbene derived 2-phospha-1,3-butadienes and their
 sequential one-electron oxidation to radical cations and dications
;
_journal_issue                   7
_journal_name_full               'Chemical Science'
_journal_page_first              1975
_journal_page_last               1984
_journal_paper_doi               10.1039/C9SC05598C
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C54 H72 Cl N3 P, C F3 O3 S'
_chemical_formula_sum            'C55 H72 Cl F3 N3 O3 P S'
_chemical_formula_weight         978.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-01
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2019-08-28 deposited with the CCDC.	2020-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                98.063(2)
_cell_angle_beta                 91.131(2)
_cell_angle_gamma                103.315(3)
_cell_formula_units_Z            2
_cell_length_a                   11.0592(4)
_cell_length_b                   12.9006(3)
_cell_length_c                   18.7834(5)
_cell_measurement_reflns_used    21348
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.2750
_cell_measurement_theta_min      3.4950
_cell_volume                     2578.25(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -60.00  29.00   1.00   12.50    --  -38.50  57.00  30.00   89
  2  ω    -58.00  33.00   1.00   12.50    --  -38.50  38.00 -60.00   91
  3  ω    -50.00  31.00   1.00   12.50    --  -38.50  77.00 150.00   81
  4  ω    -66.00 -18.00   1.00   12.50    --  -38.50 -38.00 -30.00   48
  5  ω     19.00  74.00   1.00   12.50    --   42.70  57.00 150.00   55
  6  ω      3.00  75.00   1.00   12.50    --   42.70 -99.00 -90.00   72
  7  ω     15.00  43.00   1.00   12.50    --   42.70  77.00 120.00   28
  8  ω     65.00 108.00   1.00   12.50    --   42.70  77.00 120.00   43
  9  ω     15.00  52.00   1.00   12.50    --   42.70  77.00   0.00   37
 10  ω     20.00  96.00   1.00   12.50    --   42.70  57.00  30.00   76
 11  ω     10.00  67.00   1.00   12.50    --   42.70 -99.00  90.00   57
 12  ω     17.00  61.00   1.00   12.50    --   42.70  77.00-180.00   44
 13  ω     13.00  60.00   1.00   12.50    --   42.70  77.00 -60.00   47
 14  ω     64.00 114.00   1.00   12.50    --   42.70  77.00-180.00   50
 15  ω     13.00 114.00   1.00   12.50    --   42.70  77.00-120.00  101
 16  ω     29.00  57.00   1.00   12.50    --   42.70  38.00   0.00   28
 17  ω     13.00  80.00   1.00   12.50    --   42.70  77.00  60.00   67
 18  ω     31.00  89.00   1.00   49.50    --  111.00 -94.00   0.00   58
 19  ω     81.00 177.00   1.00   49.50    --  111.00  77.00 -30.00   96
 20  ω     41.00 102.00   1.00   49.50    --  111.00-125.00 -30.00   61
 21  ω     43.00 137.00   1.00   49.50    --  111.00 -61.00 150.00   94
 22  ω     81.00 108.00   1.00   49.50    --  111.00  77.00  90.00   27
 23  ω     81.00 176.00   1.00   49.50    --  111.00  77.00 150.00   95
 24  ω     81.00 164.00   1.00   49.50    --  111.00  77.00-120.00   83
 25  ω     85.00 130.00   1.00   49.50    --  111.00  61.00-120.00   45
 26  ω     85.00 177.00   1.00   49.50    --  111.00  61.00 -60.00   92
 27  ω     83.00 110.00   1.00   49.50    --  111.00  68.00 -51.76   27
 28  ω     85.00 178.00   1.00   49.50    --  111.00  62.00  93.47   93
 29  ω    112.00 146.00   1.00   49.50    --  111.00  77.00  60.00   34
 30  ω     81.00 171.00   1.00   49.50    --  111.00  77.00  30.00   90
 31  ω     85.00 112.00   1.00   49.50    --  111.00  61.00  30.00   27
 32  ω     81.00 107.00   1.00   49.50    --  111.00  77.00  60.00   26
 33  ω     43.00 121.00   1.00   49.50    --  111.00-129.00 143.00   78
 34  ω     85.00 112.00   1.00   49.50    --  111.00  61.00  90.00   27
 35  ω     31.00 106.00   1.00   49.50    --  111.00 -94.00 150.00   75
 36  ω     88.00 152.00   1.00   49.50    --  111.00  48.00-154.30   64
 37  ω     81.00 175.00   1.00   49.50    --  111.00  77.00   0.00   94
 38  ω     82.00 108.00   1.00   49.50    --  111.00  77.00-180.00   26
 39  ω     85.00 112.00   1.00   49.50    --  111.00  61.00 120.00   27
 40  ω     81.00 107.00   1.00   49.50    --  111.00  77.00 -90.00   26
 41  ω     91.00 116.00   1.00   49.50    --  111.00-125.00 -90.00   25
 42  ω     81.00 151.00   1.00   49.50    --  111.00  77.00 120.00   70
 43  ω     85.00 111.00   1.00   49.50    --  111.00  61.00  60.00   26
 44  ω     85.00 111.00   1.00   49.50    --  111.00  61.00 150.00   26
 45  ω     81.00 107.00   1.00   49.50    --  111.00  77.00-150.00   26
 46  ω     85.00 111.00   1.00   49.50    --  111.00  61.00-150.00   26
 47  ω     85.00 112.00   1.00   49.50    --  111.00  61.00   0.00   27
 48  ω     85.00 122.00   1.00   49.50    --  111.00  61.00 -30.00   37
 49  ω     45.00 118.00   1.00   49.50    --  111.00-125.00  90.00   73
 50  ω     85.00 112.00   1.00   49.50    --  111.00  61.00 -90.00   27
 51  ω     85.00 112.00   1.00   49.50    --  111.00  61.00-180.00   27
 52  ω     88.00 118.00   1.00   49.50    --  111.00-125.00   0.00   30
 53  ω     58.00  87.00   1.00   49.50    --  111.00-125.00   0.00   29
 54  ω     82.00 178.00   1.00   49.50    --  111.00  73.00-158.66   96
 55  ω     84.00 157.00   1.00   49.50    --  111.00  66.00 -84.59   73
 56  ω     83.00 107.00   1.00   49.50    --  111.00  68.00 120.11   24
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0018531000
_diffrn_orient_matrix_UB_12      -0.0171295000
_diffrn_orient_matrix_UB_13      -0.0828872000
_diffrn_orient_matrix_UB_21      -0.0136864000
_diffrn_orient_matrix_UB_22      -0.1216643000
_diffrn_orient_matrix_UB_23      -0.0004385000
_diffrn_orient_matrix_UB_31      -0.1426921000
_diffrn_orient_matrix_UB_32      -0.0174640000
_diffrn_orient_matrix_UB_33      -0.0033826000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            46168
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.693
_diffrn_reflns_theta_min         2.379
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.785
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.451
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       plate
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.499
_exptl_crystal_size_mid          0.312
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         10686
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0604P)²+0.9870P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1182
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9327
_reflns_number_total             10686
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9sc05598c2.cif
_cod_data_source_block           compound2
_cod_depositor_comments
'Adding full bibliography for 1557449--1557455.cif.'
_cod_original_cell_volume        2578.25(13)
_cod_database_code               1557449
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C55H72ClF3N3O3PS
_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.
;
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.470
_diffrn_oxdiff_digest_frames
;
01b398728a16ea12b9fc2eda7727766f6d0314356fd
;
_diffrn_oxdiff_digest_hkl
;
0123ca9911f43a4794f9ebcb5eeb0c47a3ff5e
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     42.14
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C55B) = Uanis(C55)
Uanis(C13) = Uanis(C13B)
3. Rigid body (RIGU) restrains
 F1, F1B, F2, F2B, F3, F3B, O1, O2, O3, C55, C55B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C13B)=Sof(H13B)=Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15B)=
 Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1)
 Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=
 Sof(H15B)=Sof(H15C)=FVAR(1)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(C55B)=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(C55)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C13B(H13B), C22(H22), C25(H25), C49(H49), C52(H52)
5.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20),
 C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C45(H45), C46(H46), C47(H47)
5.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C14B(H14D,H14E,
 H14F), C15(H15A,H15B,H15C), C15B(H15D,H15E,H15F), C23(H23A,H23B,H23C),
 C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C50(H50A,
 H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C)
;
_olex2_date_sample_data_collection 2019-06-28
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.878
_oxdiff_exptl_absorpt_empirical_full_min 0.376
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-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_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
Cl1 Cl 0.86131(4) 0.57571(3) 0.38621(2) 0.02716(10) Uani 1 1 d . . . . .
P1 P 0.76081(4) 0.55263(3) 0.28406(2) 0.02046(9) Uani 1 1 d . . . . .
N1 N 0.63005(13) 0.30592(11) 0.22222(8) 0.0253(3) Uani 1 1 d . . . . .
N2 N 0.80657(12) 0.26134(10) 0.20542(7) 0.0207(3) Uani 1 1 d . . . . .
N3 N 0.87492(12) 0.77814(10) 0.28621(7) 0.0197(3) Uani 1 1 d . . . . .
C1 C 0.75510(14) 0.34921(12) 0.21856(8) 0.0202(3) Uani 1 1 d . . . . .
C2 C 0.60541(17) 0.19383(13) 0.21099(10) 0.0301(4) Uani 1 1 d . . . . .
H2 H 0.527835 0.146735 0.210972 0.036 Uiso 1 1 calc R . . . .
C3 C 0.71287(16) 0.16662(12) 0.20033(9) 0.0266(3) Uani 1 1 d . . . . .
H3 H 0.724000 0.096791 0.191093 0.032 Uiso 1 1 calc R . . . .
C4 C 0.53007(15) 0.35966(13) 0.23415(9) 0.0271(3) Uani 1 1 d . . . . .
C5 C 0.49668(16) 0.38283(14) 0.30539(10) 0.0300(4) Uani 1 1 d . . . . .
C6 C 0.39990(18) 0.43481(15) 0.31571(12) 0.0379(4) Uani 1 1 d . . . . .
H6 H 0.376848 0.454230 0.362126 0.046 Uiso 1 1 calc R . . . .
C7 C 0.33748(19) 0.45791(17) 0.25731(14) 0.0469(5) Uani 1 1 d . . . . .
H7 H 0.274987 0.495018 0.265088 0.056 Uiso 1 1 calc R . . . .
C8 C 0.36700(19) 0.42653(19) 0.18795(14) 0.0468(5) Uani 1 1 d . . . . .
H8 H 0.321306 0.439672 0.149502 0.056 Uiso 1 1 calc R . . . .
C9 C 0.46441(17) 0.37528(17) 0.17430(11) 0.0374(4) Uani 1 1 d . . . . .
C10 C 0.55781(19) 0.34617(16) 0.36690(10) 0.0366(4) Uani 1 1 d . . . . .
H10 H 0.642128 0.342167 0.353811 0.044 Uiso 1 1 calc R . . . .
C11 C 0.4861(3) 0.23200(18) 0.37798(13) 0.0514(6) Uani 1 1 d . . . . .
H11A H 0.402058 0.233265 0.389233 0.077 Uiso 1 1 calc GR . . . .
H11B H 0.526115 0.209450 0.416903 0.077 Uiso 1 1 calc GR . . . .
H11C H 0.485497 0.182500 0.334686 0.077 Uiso 1 1 calc GR . . . .
C12 C 0.5684(2) 0.42215(19) 0.43781(11) 0.0490(5) Uani 1 1 d . . . . .
H12A H 0.605501 0.494404 0.430155 0.074 Uiso 1 1 calc GR . . . .
H12B H 0.619445 0.400876 0.472370 0.074 Uiso 1 1 calc GR . . . .
H12C H 0.487071 0.419010 0.455576 0.074 Uiso 1 1 calc GR . . . .
C13 C 0.4903(2) 0.3248(2) 0.09772(14) 0.0324(6) Uani 0.783(5) 1 d . . P A 1
H13 H 0.572199 0.307962 0.099919 0.039 Uiso 0.783(5) 1 calc R . P A 1
C13B C 0.4775(9) 0.3702(9) 0.0970(6) 0.0324(6) Uani 0.217(5) 1 d . . P A 2
H13B H 0.458397 0.435124 0.082675 0.039 Uiso 0.217(5) 1 calc R . P A 2
C14 C 0.3933(3) 0.2203(3) 0.0723(2) 0.0465(8) Uani 0.783(5) 1 d . . P A 1
H14A H 0.393578 0.170870 0.106055 0.070 Uiso 0.783(5) 1 calc GR . P A 1
H14B H 0.412808 0.188934 0.025847 0.070 Uiso 0.783(5) 1 calc GR . P A 1
H14C H 0.312454 0.235349 0.069173 0.070 Uiso 0.783(5) 1 calc GR . P A 1
C14B C 0.3738(13) 0.2746(14) 0.0652(7) 0.056(3) Uani 0.217(5) 1 d . . P A 2
H14D H 0.380030 0.212690 0.086817 0.084 Uiso 0.217(5) 1 calc GR . P A 2
H14E H 0.381125 0.259620 0.014172 0.084 Uiso 0.217(5) 1 calc GR . P A 2
H14F H 0.294708 0.290955 0.074611 0.084 Uiso 0.217(5) 1 calc GR . P A 2
C15 C 0.4928(3) 0.4041(2) 0.04419(14) 0.0451(7) Uani 0.783(5) 1 d . . P A 1
H15A H 0.413197 0.421426 0.041216 0.068 Uiso 0.783(5) 1 calc GR . P A 1
H15B H 0.511160 0.372006 -0.002384 0.068 Uiso 0.783(5) 1 calc GR . P A 1
H15C H 0.555765 0.468587 0.060115 0.068 Uiso 0.783(5) 1 calc GR . P A 1
C15B C 0.6011(9) 0.3625(8) 0.0702(5) 0.038(2) Uani 0.217(5) 1 d . . P A 2
H15D H 0.663895 0.422170 0.094190 0.057 Uiso 0.217(5) 1 calc GR . P A 2
H15E H 0.600425 0.364022 0.019281 0.057 Uiso 0.217(5) 1 calc GR . P A 2
H15F H 0.618927 0.296272 0.079964 0.057 Uiso 0.217(5) 1 calc GR . P A 2
C16 C 0.93408(15) 0.24969(11) 0.20882(9) 0.0222(3) Uani 1 1 d . . . . .
C17 C 0.97444(16) 0.19394(12) 0.14759(9) 0.0251(3) Uani 1 1 d . . . . .
C18 C 1.08715(17) 0.16337(13) 0.15556(10) 0.0301(4) Uani 1 1 d . . . . .
H18 H 1.116268 0.125913 0.116192 0.036 Uiso 1 1 calc R . . . .
C19 C 1.15570(17) 0.18738(14) 0.22013(11) 0.0337(4) Uani 1 1 d . . . . .
H19 H 1.229964 0.165908 0.224084 0.040 Uiso 1 1 calc R . . . .
C20 C 1.11400(17) 0.24369(14) 0.27940(10) 0.0312(4) Uani 1 1 d . . . . .
H20 H 1.161601 0.260552 0.322637 0.037 Uiso 1 1 calc R . . . .
C21 C 1.00227(16) 0.27538(12) 0.27532(9) 0.0251(3) Uani 1 1 d . . . . .
C22 C 0.90282(17) 0.16398(13) 0.07491(9) 0.0279(3) Uani 1 1 d . . . . .
H22 H 0.833661 0.199882 0.076806 0.033 Uiso 1 1 calc R . . . .
C23 C 0.84841(19) 0.04157(14) 0.05657(10) 0.0343(4) Uani 1 1 d . . . . .
H23A H 0.914443 0.004646 0.057097 0.051 Uiso 1 1 calc GR . . . .
H23B H 0.806820 0.025489 0.009602 0.051 Uiso 1 1 calc GR . . . .
H23C H 0.790081 0.018347 0.091590 0.051 Uiso 1 1 calc GR . . . .
C24 C 0.9859(2) 0.20249(15) 0.01474(10) 0.0379(4) Uani 1 1 d . . . . .
H24A H 1.023393 0.277992 0.027155 0.057 Uiso 1 1 calc GR . . . .
H24B H 0.936356 0.190413 -0.029523 0.057 Uiso 1 1 calc GR . . . .
H24C H 1.049765 0.163154 0.008949 0.057 Uiso 1 1 calc GR . . . .
C25 C 0.95264(18) 0.32868(14) 0.34199(9) 0.0302(4) Uani 1 1 d . . . . .
H25 H 0.909921 0.381215 0.326806 0.036 Uiso 1 1 calc R . . . .
C26 C 0.8554(2) 0.24452(17) 0.37419(10) 0.0371(4) Uani 1 1 d . . . . .
H26A H 0.787875 0.212729 0.339231 0.056 Uiso 1 1 calc GR . . . .
H26B H 0.824435 0.278890 0.416274 0.056 Uiso 1 1 calc GR . . . .
H26C H 0.893436 0.189472 0.387121 0.056 Uiso 1 1 calc GR . . . .
C27 C 1.0547(2) 0.38976(16) 0.39921(10) 0.0406(5) Uani 1 1 d . . . . .
H27A H 1.092703 0.339375 0.418836 0.061 Uiso 1 1 calc GR . . . .
H27B H 1.018735 0.428973 0.437016 0.061 Uiso 1 1 calc GR . . . .
H27C H 1.116571 0.439129 0.377581 0.061 Uiso 1 1 calc GR . . . .
C28 C 0.81989(15) 0.46062(12) 0.22544(8) 0.0202(3) Uani 1 1 d . . . . .
C29 C 0.94152(14) 0.49053(11) 0.19284(8) 0.0201(3) Uani 1 1 d . . . . .
C30 C 0.95926(16) 0.44735(12) 0.12198(9) 0.0241(3) Uani 1 1 d . . . . .
H30 H 0.898488 0.390643 0.097531 0.029 Uiso 1 1 calc R . . . .
C31 C 1.06646(17) 0.48833(13) 0.08798(10) 0.0299(4) Uani 1 1 d . . . . .
H31 H 1.076601 0.458856 0.041010 0.036 Uiso 1 1 calc R . . . .
C32 C 1.15854(17) 0.57275(14) 0.12333(11) 0.0336(4) Uani 1 1 d . . . . .
H32 H 1.228784 0.601596 0.099744 0.040 Uiso 1 1 calc R . . . .
C33 C 1.14474(16) 0.61369(13) 0.19424(10) 0.0308(4) Uani 1 1 d . . . . .
H33 H 1.206933 0.669039 0.218827 0.037 Uiso 1 1 calc R . . . .
C34 C 1.03837(15) 0.57218(12) 0.22848(9) 0.0243(3) Uani 1 1 d . . . . .
H34 H 1.031152 0.599273 0.276362 0.029 Uiso 1 1 calc R . . . .
C35 C 0.81893(14) 0.68335(12) 0.25080(8) 0.0199(3) Uani 1 1 d . . . . .
C36 C 0.76679(16) 0.69578(12) 0.17626(8) 0.0235(3) Uani 1 1 d . . . . .
C37 C 0.79923(17) 0.81914(13) 0.17806(8) 0.0262(3) Uani 1 1 d . . . . .
H37A H 0.827649 0.837252 0.131843 0.031 Uiso 1 1 calc R . . . .
H37B H 0.726582 0.847561 0.188626 0.031 Uiso 1 1 calc R . . . .
C38 C 0.90181(16) 0.86649(12) 0.23675(8) 0.0230(3) Uani 1 1 d . . . . .
C39 C 0.81750(19) 0.63794(14) 0.11086(9) 0.0302(4) Uani 1 1 d . . . . .
H39A H 0.906756 0.659329 0.113834 0.045 Uiso 1 1 calc GR . . . .
H39B H 0.786231 0.656739 0.067601 0.045 Uiso 1 1 calc GR . . . .
H39C H 0.791330 0.561474 0.110139 0.045 Uiso 1 1 calc GR . . . .
C40 C 0.62432(17) 0.65360(14) 0.17352(9) 0.0301(4) Uani 1 1 d . . . . .
H40A H 0.604274 0.577248 0.174025 0.045 Uiso 1 1 calc GR . . . .
H40B H 0.588598 0.668655 0.130240 0.045 Uiso 1 1 calc GR . . . .
H40C H 0.591339 0.688631 0.214590 0.045 Uiso 1 1 calc GR . . . .
C41 C 1.03099(17) 0.87349(13) 0.20743(9) 0.0283(3) Uani 1 1 d . . . . .
H41A H 1.093330 0.906344 0.245269 0.042 Uiso 1 1 calc GR . . . .
H41B H 1.040645 0.916134 0.169034 0.042 Uiso 1 1 calc GR . . . .
H41C H 1.040101 0.802381 0.189591 0.042 Uiso 1 1 calc GR . . . .
C42 C 0.89321(17) 0.97531(12) 0.27655(9) 0.0271(3) Uani 1 1 d . . . . .
H42A H 0.809924 0.971371 0.291427 0.041 Uiso 1 1 calc GR . . . .
H42B H 0.914174 1.028810 0.245231 0.041 Uiso 1 1 calc GR . . . .
H42C H 0.950089 0.994517 0.318126 0.041 Uiso 1 1 calc GR . . . .
C43 C 0.89335(15) 0.80839(11) 0.36466(8) 0.0205(3) Uani 1 1 d . . . . .
C44 C 0.78771(15) 0.82519(12) 0.40126(8) 0.0231(3) Uani 1 1 d . . . . .
C45 C 0.80155(17) 0.85055(13) 0.47619(9) 0.0266(3) Uani 1 1 d . . . . .
H45 H 0.732740 0.858705 0.502140 0.032 Uiso 1 1 calc R . . . .
C46 C 0.91477(18) 0.86377(14) 0.51258(9) 0.0289(3) Uani 1 1 d . . . . .
H46 H 0.921636 0.879899 0.562545 0.035 Uiso 1 1 calc R . . . .
C47 C 1.01815(17) 0.85298(13) 0.47463(9) 0.0273(3) Uani 1 1 d . . . . .
H47 H 1.094848 0.865157 0.499503 0.033 Uiso 1 1 calc R . . . .
C48 C 1.01026(15) 0.82431(12) 0.39998(8) 0.0229(3) Uani 1 1 d . . . . .
C49 C 0.66116(16) 0.81977(13) 0.36549(9) 0.0264(3) Uani 1 1 d . . . . .
H49 H 0.670218 0.814786 0.313410 0.032 Uiso 1 1 calc R . . . .
C50 C 0.56356(17) 0.72067(15) 0.37942(10) 0.0347(4) Uani 1 1 d . . . . .
H50A H 0.591682 0.656823 0.362881 0.052 Uiso 1 1 calc GR . . . .
H50B H 0.486471 0.718040 0.354035 0.052 Uiso 1 1 calc GR . . . .
H50C H 0.551261 0.724907 0.430103 0.052 Uiso 1 1 calc GR . . . .
C51 C 0.61462(18) 0.92202(15) 0.39089(10) 0.0345(4) Uani 1 1 d . . . . .
H51A H 0.594029 0.923377 0.440372 0.052 Uiso 1 1 calc GR . . . .
H51B H 0.542087 0.921692 0.361850 0.052 Uiso 1 1 calc GR . . . .
H51C H 0.678779 0.984630 0.386263 0.052 Uiso 1 1 calc GR . . . .
C52 C 1.12914(15) 0.81244(13) 0.36385(9) 0.0260(3) Uani 1 1 d . . . . .
H52 H 1.108603 0.787074 0.312421 0.031 Uiso 1 1 calc R . . . .
C53 C 1.18895(18) 0.73106(16) 0.39473(10) 0.0353(4) Uani 1 1 d . . . . .
H53A H 1.218868 0.758837 0.443601 0.053 Uiso 1 1 calc GR . . . .
H53B H 1.257189 0.719158 0.366454 0.053 Uiso 1 1 calc GR . . . .
H53C H 1.128228 0.664240 0.393473 0.053 Uiso 1 1 calc GR . . . .
C54 C 1.22320(18) 0.92202(16) 0.37188(10) 0.0360(4) Uani 1 1 d . . . . .
H54A H 1.184752 0.973933 0.354579 0.054 Uiso 1 1 calc GR . . . .
H54B H 1.293958 0.915267 0.344376 0.054 Uiso 1 1 calc GR . . . .
H54C H 1.249668 0.945348 0.421701 0.054 Uiso 1 1 calc GR . . . .
S1 S 0.43407(4) 0.91198(3) 0.20197(2) 0.03101(11) Uani 1 1 d . . . . .
F1 F 0.2593(4) 0.8403(3) 0.09856(17) 0.0593(8) Uani 0.789(13) 1 d . U P B 1
F1B F 0.313(2) 0.8444(13) 0.0778(14) 0.100(6) Uani 0.211(13) 1 d . U P B 2
F2 F 0.4244(5) 0.7827(2) 0.08004(17) 0.0602(9) Uani 0.789(13) 1 d . U P B 1
F2B F 0.497(3) 0.8149(15) 0.0826(6) 0.078(5) Uani 0.211(13) 1 d . U P B 2
F3 F 0.4253(5) 0.9462(4) 0.0687(3) 0.0663(10) Uani 0.789(13) 1 d . U P B 1
F3B F 0.473(2) 0.9732(15) 0.0731(11) 0.074(5) Uani 0.211(13) 1 d . U P B 2
O1 O 0.38493(14) 0.81605(11) 0.23302(8) 0.0420(3) Uani 1 1 d . U . . .
O2 O 0.56716(13) 0.94320(11) 0.20399(10) 0.0496(4) Uani 1 1 d . U . . .
O3 O 0.37434(13) 0.99921(11) 0.22047(9) 0.0422(3) Uani 1 1 d . U . . .
C55 C 0.3827(6) 0.8685(3) 0.1086(2) 0.0405(9) Uani 0.789(13) 1 d . U P B 1
C55B C 0.4261(18) 0.8839(14) 0.1019(10) 0.0405(9) Uani 0.211(13) 1 d . U P B 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0148
1 8 -3 0.1074
6 2 -1 0.1738
2 -8 3 0.1396
-7 -1 0 0.1824
0 0 -1 0.0148
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
C28 P1 Cl1 107.27(5) . . ?
C28 P1 C35 104.10(7) . . ?
C35 P1 Cl1 102.97(5) . . ?
C1 N1 C2 110.38(13) . . ?
C1 N1 C4 129.35(13) . . ?
C2 N1 C4 120.26(14) . . ?
C1 N2 C3 109.64(13) . . ?
C1 N2 C16 132.70(13) . . ?
C3 N2 C16 116.59(12) . . ?
C35 N3 C38 112.33(12) . . ?
C35 N3 C43 126.97(13) . . ?
C43 N3 C38 119.88(11) . . ?
N1 C1 N2 104.54(13) . . ?
N1 C1 C28 128.74(14) . . ?
N2 C1 C28 126.71(14) . . ?
N1 C2 H2 126.3 . . ?
C3 C2 N1 107.41(15) . . ?
C3 C2 H2 126.3 . . ?
N2 C3 H3 126.0 . . ?
C2 C3 N2 108.02(14) . . ?
C2 C3 H3 126.0 . . ?
C5 C4 N1 117.74(16) . . ?
C9 C4 N1 118.02(15) . . ?
C9 C4 C5 123.88(16) . . ?
C4 C5 C10 121.16(16) . . ?
C6 C5 C4 116.80(18) . . ?
C6 C5 C10 121.92(17) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 C5 120.54(19) . . ?
C7 C6 H6 119.7 . . ?
C6 C7 H7 119.6 . . ?
C8 C7 C6 120.77(18) . . ?
C8 C7 H7 119.6 . . ?
C7 C8 H8 119.4 . . ?
C7 C8 C9 121.2(2) . . ?
C9 C8 H8 119.4 . . ?
C4 C9 C8 116.44(19) . . ?
C4 C9 C13 119.99(19) . . ?
C4 C9 C13B 138.3(5) . . ?
C8 C9 C13 123.2(2) . . ?
C8 C9 C13B 104.3(5) . . ?
C5 C10 H10 107.9 . . ?
C5 C10 C11 110.28(18) . . ?
C5 C10 C12 113.64(17) . . ?
C11 C10 H10 107.9 . . ?
C12 C10 H10 107.9 . . ?
C12 C10 C11 109.14(17) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13 108.3 . . ?
C14 C13 C9 110.8(2) . . ?
C14 C13 H13 108.3 . . ?
C14 C13 C15 110.4(2) . . ?
C15 C13 C9 110.9(2) . . ?
C15 C13 H13 108.3 . . ?
C9 C13B H13B 107.8 . . ?
C9 C13B C14B 103.5(8) . . ?
C9 C13B C15B 116.7(8) . . ?
C14B C13B H13B 107.8 . . ?
C15B C13B H13B 107.8 . . ?
C15B C13B C14B 112.8(10) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13B C14B H14D 109.5 . . ?
C13B C14B H14E 109.5 . . ?
C13B C14B H14F 109.5 . . ?
H14D C14B H14E 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13B C15B H15D 109.5 . . ?
C13B C15B H15E 109.5 . . ?
C13B C15B H15F 109.5 . . ?
H15D C15B H15E 109.5 . . ?
H15D C15B H15F 109.5 . . ?
H15E C15B H15F 109.5 . . ?
C17 C16 N2 116.98(14) . . ?
C21 C16 N2 119.34(14) . . ?
C21 C16 C17 122.57(15) . . ?
C16 C17 C22 124.10(15) . . ?
C18 C17 C16 116.94(16) . . ?
C18 C17 C22 118.96(15) . . ?
C17 C18 H18 119.2 . . ?
C19 C18 C17 121.67(16) . . ?
C19 C18 H18 119.2 . . ?
C18 C19 H19 120.0 . . ?
C18 C19 C20 119.97(17) . . ?
C20 C19 H19 120.0 . . ?
C19 C20 H20 119.4 . . ?
C19 C20 C21 121.24(17) . . ?
C21 C20 H20 119.4 . . ?
C16 C21 C25 121.63(15) . . ?
C20 C21 C16 117.60(15) . . ?
C20 C21 C25 120.63(16) . . ?
C17 C22 H22 108.2 . . ?
C17 C22 C23 111.88(14) . . ?
C17 C22 C24 111.03(15) . . ?
C23 C22 H22 108.2 . . ?
C24 C22 H22 108.2 . . ?
C24 C22 C23 109.21(14) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 H25 107.4 . . ?
C21 C25 C26 110.00(14) . . ?
C21 C25 C27 113.56(16) . . ?
C26 C25 H25 107.4 . . ?
C27 C25 H25 107.4 . . ?
C27 C25 C26 110.70(15) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C1 C28 P1 117.01(11) . . ?
C1 C28 C29 119.62(13) . . ?
C29 C28 P1 122.66(11) . . ?
C30 C29 C28 121.31(14) . . ?
C34 C29 C28 120.92(14) . . ?
C34 C29 C30 117.35(14) . . ?
C29 C30 H30 119.6 . . ?
C31 C30 C29 120.80(16) . . ?
C31 C30 H30 119.6 . . ?
C30 C31 H31 119.7 . . ?
C32 C31 C30 120.69(16) . . ?
C32 C31 H31 119.7 . . ?
C31 C32 H32 120.4 . . ?
C31 C32 C33 119.29(16) . . ?
C33 C32 H32 120.4 . . ?
C32 C33 H33 120.0 . . ?
C34 C33 C32 120.06(17) . . ?
C34 C33 H33 120.0 . . ?
C29 C34 H34 119.2 . . ?
C33 C34 C29 121.68(16) . . ?
C33 C34 H34 119.2 . . ?
N3 C35 P1 130.02(12) . . ?
N3 C35 C36 110.22(13) . . ?
C36 C35 P1 117.55(11) . . ?
C37 C36 C35 102.60(12) . . ?
C39 C36 C35 116.05(13) . . ?
C39 C36 C37 112.01(14) . . ?
C39 C36 C40 108.58(14) . . ?
C40 C36 C35 107.82(13) . . ?
C40 C36 C37 109.51(13) . . ?
C36 C37 H37A 110.3 . . ?
C36 C37 H37B 110.3 . . ?
H37A C37 H37B 108.5 . . ?
C38 C37 C36 107.14(12) . . ?
C38 C37 H37A 110.3 . . ?
C38 C37 H37B 110.3 . . ?
C37 C38 N3 100.07(12) . . ?
C37 C38 C41 111.65(13) . . ?
C41 C38 N3 109.41(12) . . ?
C42 C38 N3 111.51(12) . . ?
C42 C38 C37 113.56(14) . . ?
C42 C38 C41 110.24(14) . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C36 C40 H40A 109.5 . . ?
C36 C40 H40B 109.5 . . ?
C36 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C38 C42 H42A 109.5 . . ?
C38 C42 H42B 109.5 . . ?
C38 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 N3 115.85(14) . . ?
C48 C43 N3 121.59(14) . . ?
C48 C43 C44 122.50(14) . . ?
C43 C44 C49 125.23(14) . . ?
C45 C44 C43 117.05(15) . . ?
C45 C44 C49 117.71(14) . . ?
C44 C45 H45 119.2 . . ?
C46 C45 C44 121.55(16) . . ?
C46 C45 H45 119.2 . . ?
C45 C46 H46 120.1 . . ?
C45 C46 C47 119.84(15) . . ?
C47 C46 H46 120.1 . . ?
C46 C47 H47 119.2 . . ?
C46 C47 C48 121.65(16) . . ?
C48 C47 H47 119.2 . . ?
C43 C48 C52 125.48(14) . . ?
C47 C48 C43 117.22(15) . . ?
C47 C48 C52 117.30(15) . . ?
C44 C49 H49 108.0 . . ?
C44 C49 C50 111.93(14) . . ?
C44 C49 C51 111.47(14) . . ?
C50 C49 H49 108.0 . . ?
C50 C49 C51 109.32(14) . . ?
C51 C49 H49 108.0 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C49 C51 H51A 109.5 . . ?
C49 C51 H51B 109.5 . . ?
C49 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C48 C52 H52 108.3 . . ?
C48 C52 C53 112.29(15) . . ?
C48 C52 C54 110.17(13) . . ?
C53 C52 H52 108.3 . . ?
C53 C52 C54 109.31(15) . . ?
C54 C52 H52 108.3 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C52 C54 H54A 109.5 . . ?
C52 C54 H54B 109.5 . . ?
C52 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
O1 S1 C55 101.61(16) . . ?
O1 S1 C55B 111.6(6) . . ?
O2 S1 O1 114.33(9) . . ?
O2 S1 O3 114.74(9) . . ?
O2 S1 C55 106.5(2) . . ?
O2 S1 C55B 91.1(6) . . ?
O3 S1 O1 115.75(9) . . ?
O3 S1 C55 101.53(15) . . ?
O3 S1 C55B 106.2(6) . . ?
F1 C55 S1 112.9(3) . . ?
F1 C55 F2 106.4(3) . . ?
F1 C55 F3 107.7(4) . . ?
F2 C55 S1 112.1(3) . . ?
F3 C55 S1 111.2(3) . . ?
F3 C55 F2 106.3(4) . . ?
F1B C55B S1 110.3(12) . . ?
F1B C55B F2B 111.0(16) . . ?
F1B C55B F3B 109.3(16) . . ?
F2B C55B S1 107.7(12) . . ?
F2B C55B F3B 106.9(16) . . ?
F3B C55B S1 111.5(14) . . ?
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
Cl1 P1 2.1467(5) . ?
P1 C28 1.7514(15) . ?
P1 C35 1.8599(16) . ?
N1 C1 1.374(2) . ?
N1 C2 1.393(2) . ?
N1 C4 1.440(2) . ?
N2 C1 1.3762(19) . ?
N2 C3 1.399(2) . ?
N2 C16 1.453(2) . ?
N3 C35 1.314(2) . ?
N3 C38 1.5499(19) . ?
N3 C43 1.4681(18) . ?
C1 C28 1.437(2) . ?
C2 H2 0.9300 . ?
C2 C3 1.326(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.405(2) . ?
C4 C9 1.389(3) . ?
C5 C6 1.391(3) . ?
C5 C10 1.512(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.388(3) . ?
C7 H7 0.9300 . ?
C7 C8 1.378(3) . ?
C8 H8 0.9300 . ?
C8 C9 1.398(3) . ?
C9 C13 1.554(3) . ?
C9 C13B 1.456(11) . ?
C10 H10 0.9800 . ?
C10 C11 1.548(3) . ?
C10 C12 1.524(3) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13 0.9800 . ?
C13 C14 1.526(4) . ?
C13 C15 1.528(4) . ?
C13B H13B 0.9800 . ?
C13B C14B 1.519(16) . ?
C13B C15B 1.486(14) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C14B H14D 0.9600 . ?
C14B H14E 0.9600 . ?
C14B H14F 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15B H15D 0.9600 . ?
C15B H15E 0.9600 . ?
C15B H15F 0.9600 . ?
C16 C17 1.405(2) . ?
C16 C21 1.404(2) . ?
C17 C18 1.403(2) . ?
C17 C22 1.519(2) . ?
C18 H18 0.9300 . ?
C18 C19 1.375(3) . ?
C19 H19 0.9300 . ?
C19 C20 1.388(3) . ?
C20 H20 0.9300 . ?
C20 C21 1.392(2) . ?
C21 C25 1.517(2) . ?
C22 H22 0.9800 . ?
C22 C23 1.541(2) . ?
C22 C24 1.535(2) . ?
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 H25 0.9800 . ?
C25 C26 1.540(3) . ?
C25 C27 1.535(3) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C29 1.481(2) . ?
C29 C30 1.405(2) . ?
C29 C34 1.400(2) . ?
C30 H30 0.9300 . ?
C30 C31 1.389(2) . ?
C31 H31 0.9300 . ?
C31 C32 1.387(3) . ?
C32 H32 0.9300 . ?
C32 C33 1.387(3) . ?
C33 H33 0.9300 . ?
C33 C34 1.386(2) . ?
C34 H34 0.9300 . ?
C35 C36 1.547(2) . ?
C36 C37 1.544(2) . ?
C36 C39 1.531(2) . ?
C36 C40 1.541(2) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 C38 1.522(2) . ?
C38 C41 1.529(2) . ?
C38 C42 1.519(2) . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 C44 1.411(2) . ?
C43 C48 1.400(2) . ?
C44 C45 1.397(2) . ?
C44 C49 1.523(2) . ?
C45 H45 0.9300 . ?
C45 C46 1.378(3) . ?
C46 H46 0.9300 . ?
C46 C47 1.383(3) . ?
C47 H47 0.9300 . ?
C47 C48 1.395(2) . ?
C48 C52 1.520(2) . ?
C49 H49 0.9800 . ?
C49 C50 1.529(3) . ?
C49 C51 1.542(2) . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 H52 0.9800 . ?
C52 C53 1.534(2) . ?
C52 C54 1.536(2) . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
S1 O1 1.4395(14) . ?
S1 O2 1.4320(15) . ?
S1 O3 1.4371(14) . ?
S1 C55 1.803(4) . ?
S1 C55B 1.860(18) . ?
F1 C55 1.331(5) . ?
F1B C55B 1.282(19) . ?
F2 C55 1.343(4) . ?
F2B C55B 1.337(19) . ?
F3 C55 1.341(5) . ?
F3B C55B 1.341(18) . ?
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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl1 P1 C28 C1 94.74(12) . . . . ?
Cl1 P1 C28 C29 -75.55(13) . . . . ?
Cl1 P1 C35 N3 -19.48(15) . . . . ?
Cl1 P1 C35 C36 179.23(10) . . . . ?
P1 C28 C29 C30 -143.17(13) . . . . ?
P1 C28 C29 C34 29.3(2) . . . . ?
P1 C35 C36 C37 162.06(11) . . . . ?
P1 C35 C36 C39 -75.48(17) . . . . ?
P1 C35 C36 C40 46.50(15) . . . . ?
N1 C1 C28 P1 33.1(2) . . . . ?
N1 C1 C28 C29 -156.25(15) . . . . ?
N1 C2 C3 N2 0.6(2) . . . . ?
N1 C4 C5 C6 179.98(15) . . . . ?
N1 C4 C5 C10 -3.9(2) . . . . ?
N1 C4 C9 C8 179.23(17) . . . . ?
N1 C4 C9 C13 6.4(3) . . . . ?
N1 C4 C9 C13B -14.1(7) . . . . ?
N2 C1 C28 P1 -148.02(13) . . . . ?
N2 C1 C28 C29 22.6(2) . . . . ?
N2 C16 C17 C18 -167.30(14) . . . . ?
N2 C16 C17 C22 11.7(2) . . . . ?
N2 C16 C21 C20 167.67(14) . . . . ?
N2 C16 C21 C25 -8.1(2) . . . . ?
N3 C35 C36 C37 -2.77(17) . . . . ?
N3 C35 C36 C39 119.69(16) . . . . ?
N3 C35 C36 C40 -118.32(14) . . . . ?
N3 C43 C44 C45 177.93(13) . . . . ?
N3 C43 C44 C49 -3.2(2) . . . . ?
N3 C43 C48 C47 179.94(13) . . . . ?
N3 C43 C48 C52 -0.4(2) . . . . ?
C1 N1 C2 C3 -0.1(2) . . . . ?
C1 N1 C4 C5 -92.3(2) . . . . ?
C1 N1 C4 C9 94.3(2) . . . . ?
C1 N2 C3 C2 -0.87(19) . . . . ?
C1 N2 C16 C17 -127.77(17) . . . . ?
C1 N2 C16 C21 64.0(2) . . . . ?
C1 C28 C29 C30 46.8(2) . . . . ?
C1 C28 C29 C34 -140.78(15) . . . . ?
C2 N1 C1 N2 -0.45(18) . . . . ?
C2 N1 C1 C28 178.58(15) . . . . ?
C2 N1 C4 C5 89.0(2) . . . . ?
C2 N1 C4 C9 -84.5(2) . . . . ?
C3 N2 C1 N1 0.79(17) . . . . ?
C3 N2 C1 C28 -178.26(15) . . . . ?
C3 N2 C16 C17 65.48(18) . . . . ?
C3 N2 C16 C21 -102.78(17) . . . . ?
C4 N1 C1 N2 -179.31(15) . . . . ?
C4 N1 C1 C28 -0.3(3) . . . . ?
C4 N1 C2 C3 178.91(15) . . . . ?
C4 C5 C6 C7 2.5(3) . . . . ?
C4 C5 C10 C11 -88.7(2) . . . . ?
C4 C5 C10 C12 148.37(17) . . . . ?
C4 C9 C13 C14 98.8(3) . . . . ?
C4 C9 C13 C15 -138.4(2) . . . . ?
C4 C9 C13B C14B 112.4(9) . . . . ?
C4 C9 C13B C15B -12.1(13) . . . . ?
C5 C4 C9 C8 6.2(3) . . . . ?
C5 C4 C9 C13 -166.62(19) . . . . ?
C5 C4 C9 C13B 172.8(7) . . . . ?
C5 C6 C7 C8 2.3(3) . . . . ?
C6 C5 C10 C11 87.2(2) . . . . ?
C6 C5 C10 C12 -35.7(3) . . . . ?
C6 C7 C8 C9 -3.1(3) . . . . ?
C7 C8 C9 C4 -1.0(3) . . . . ?
C7 C8 C9 C13 171.6(2) . . . . ?
C7 C8 C9 C13B -171.8(5) . . . . ?
C8 C9 C13 C14 -73.5(3) . . . . ?
C8 C9 C13 C15 49.3(3) . . . . ?
C8 C9 C13B C14B -79.9(9) . . . . ?
C8 C9 C13B C15B 155.6(8) . . . . ?
C9 C4 C5 C6 -7.0(3) . . . . ?
C9 C4 C5 C10 169.12(18) . . . . ?
C10 C5 C6 C7 -173.57(18) . . . . ?
C16 N2 C1 N1 -166.63(15) . . . . ?
C16 N2 C1 C28 14.3(3) . . . . ?
C16 N2 C3 C2 168.82(14) . . . . ?
C16 C17 C18 C19 -0.4(2) . . . . ?
C16 C17 C22 C23 -110.14(18) . . . . ?
C16 C17 C22 C24 127.56(16) . . . . ?
C16 C21 C25 C26 78.23(19) . . . . ?
C16 C21 C25 C27 -157.08(15) . . . . ?
C17 C16 C21 C20 0.1(2) . . . . ?
C17 C16 C21 C25 -175.67(15) . . . . ?
C17 C18 C19 C20 -0.3(3) . . . . ?
C18 C17 C22 C23 68.8(2) . . . . ?
C18 C17 C22 C24 -53.48(19) . . . . ?
C18 C19 C20 C21 1.0(3) . . . . ?
C19 C20 C21 C16 -0.9(2) . . . . ?
C19 C20 C21 C25 174.93(16) . . . . ?
C20 C21 C25 C26 -97.40(19) . . . . ?
C20 C21 C25 C27 27.3(2) . . . . ?
C21 C16 C17 C18 0.6(2) . . . . ?
C21 C16 C17 C22 179.53(14) . . . . ?
C22 C17 C18 C19 -179.48(15) . . . . ?
C28 P1 C35 N3 -131.32(14) . . . . ?
C28 P1 C35 C36 67.39(12) . . . . ?
C28 C29 C30 C31 169.63(15) . . . . ?
C28 C29 C34 C33 -168.99(15) . . . . ?
C29 C30 C31 C32 0.1(3) . . . . ?
C30 C29 C34 C33 3.7(2) . . . . ?
C30 C31 C32 C33 2.3(3) . . . . ?
C31 C32 C33 C34 -1.7(3) . . . . ?
C32 C33 C34 C29 -1.4(3) . . . . ?
C34 C29 C30 C31 -3.1(2) . . . . ?
C35 P1 C28 C1 -156.57(12) . . . . ?
C35 P1 C28 C29 33.14(14) . . . . ?
C35 N3 C38 C37 26.27(16) . . . . ?
C35 N3 C38 C41 -91.11(16) . . . . ?
C35 N3 C38 C42 146.68(14) . . . . ?
C35 N3 C43 C44 -76.10(19) . . . . ?
C35 N3 C43 C48 106.80(18) . . . . ?
C35 C36 C37 C38 19.29(16) . . . . ?
C36 C37 C38 N3 -26.37(15) . . . . ?
C36 C37 C38 C41 89.33(15) . . . . ?
C36 C37 C38 C42 -145.29(14) . . . . ?
C38 N3 C35 P1 -177.38(11) . . . . ?
C38 N3 C35 C36 -15.02(17) . . . . ?
C38 N3 C43 C44 92.67(17) . . . . ?
C38 N3 C43 C48 -84.43(18) . . . . ?
C39 C36 C37 C38 -105.86(15) . . . . ?
C40 C36 C37 C38 133.61(14) . . . . ?
C43 N3 C35 P1 -7.9(2) . . . . ?
C43 N3 C35 C36 154.45(14) . . . . ?
C43 N3 C38 C37 -144.05(13) . . . . ?
C43 N3 C38 C41 98.58(15) . . . . ?
C43 N3 C38 C42 -23.6(2) . . . . ?
C43 C44 C45 C46 3.1(2) . . . . ?
C43 C44 C49 C50 109.47(18) . . . . ?
C43 C44 C49 C51 -127.74(16) . . . . ?
C43 C48 C52 C53 -123.41(17) . . . . ?
C43 C48 C52 C54 114.49(18) . . . . ?
C44 C43 C48 C47 3.0(2) . . . . ?
C44 C43 C48 C52 -177.28(15) . . . . ?
C44 C45 C46 C47 0.7(3) . . . . ?
C45 C44 C49 C50 -71.67(18) . . . . ?
C45 C44 C49 C51 51.1(2) . . . . ?
C45 C46 C47 C48 -2.8(3) . . . . ?
C46 C47 C48 C43 1.0(2) . . . . ?
C46 C47 C48 C52 -178.76(15) . . . . ?
C47 C48 C52 C53 56.3(2) . . . . ?
C47 C48 C52 C54 -65.83(19) . . . . ?
C48 C43 C44 C45 -5.0(2) . . . . ?
C48 C43 C44 C49 173.88(15) . . . . ?
C49 C44 C45 C46 -175.89(15) . . . . ?
O1 S1 C55 F1 62.1(3) . . . . ?
O1 S1 C55 F2 -58.0(3) . . . . ?
O1 S1 C55 F3 -176.7(3) . . . . ?
O1 S1 C55B F1B 58.8(15) . . . . ?
O1 S1 C55B F2B -62.5(12) . . . . ?
O1 S1 C55B F3B -179.4(12) . . . . ?
O2 S1 C55 F1 -177.9(2) . . . . ?
O2 S1 C55 F2 62.0(3) . . . . ?
O2 S1 C55 F3 -56.8(4) . . . . ?
O2 S1 C55B F1B 175.7(14) . . . . ?
O2 S1 C55B F2B 54.3(12) . . . . ?
O2 S1 C55B F3B -62.6(13) . . . . ?
O3 S1 C55 F1 -57.5(3) . . . . ?
O3 S1 C55 F2 -177.6(2) . . . . ?
O3 S1 C55 F3 63.6(4) . . . . ?
O3 S1 C55B F1B -68.1(15) . . . . ?
O3 S1 C55B F2B 170.6(11) . . . . ?
O3 S1 C55B F3B 53.6(14) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0005 0.0065 0.9979 -0.0828 -0.0012 -0.0036
0.9707 7.7982 -2.5539 0.0763 -0.9609 -0.2661
6.2610 2.3035 -0.9767 0.0299 -0.3655 -0.9303
2.1712 -8.3236 2.6066 -0.0775 0.9818 -0.1733
-6.8585 -0.5536 0.4340 -0.0138 0.1610 0.9869
-0.0005 -0.0065 -0.9979 0.0828 0.0012 0.0036
