#------------------------------------------------------------------------------
#$Date: 2020-04-23 22:53:32 +0300 (Thu, 23 Apr 2020) $
#$Revision: 251096 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/47/4134790.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_4134790
loop_
_publ_author_name
'Liu, Wenqi'
'Lin, Chenjian'
'Weber, Jacob Andrew'
'Stern, Charlotte L.'
'Young, Ryan M.'
'Wasielewski, Michael R.'
'Stoddart, J. Fraser'
_publ_section_title
;
 Cyclophane-Sustained Ultrastable Porphyrins.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c02311
_journal_year                    2020
_chemical_formula_moiety         'C96 H76 N8, C32 H22 N4, 8(F6 P), 2(C3 H6 O)'
_chemical_formula_sum            'C134 H110 F48 N12 O2 P8'
_chemical_formula_weight         3080.09
_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             2019-08-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                108.9696(10)
_cell_angle_beta                 106.6927(10)
_cell_angle_gamma                102.2968(10)
_cell_formula_units_Z            1
_cell_length_a                   14.66878(16)
_cell_length_b                   17.5021(2)
_cell_length_c                   19.14358(19)
_cell_measurement_reflns_used    21244
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.4730
_cell_measurement_theta_min      2.6410
_cell_volume                     4189.71(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω   -109.00 -55.00   0.50    0.71    --  -47.64-152.00 -39.00  108
  2  ω    -87.00 -31.00   0.50    0.71    --  -47.64 121.00-156.00  112
  3  ω   -108.00 -67.00   0.50    0.71    --  -47.64 152.00   2.00   82
  4  ω     56.00  83.00   0.50    0.71    --   47.64-152.00 -39.00   54
  5  ω     22.00  92.00   0.50    0.71    --   47.64-121.00 120.00  140
  6  ω     62.00  91.00   0.50    0.71    --   47.64 152.00   2.00   58
  7  ω   -130.00 -90.00   0.50    2.83    -- -106.00-121.00 120.00   80
  8  ω   -109.00 -66.00   0.50    2.83    -- -106.00 121.00-156.00   86
  9  ω    -82.00 -50.00   0.50    2.83    -- -106.00 152.00   2.00   64
 10  ω   -134.00-109.00   0.50    2.83    -- -106.00-152.00 -39.00   50
 11  ω     58.00  83.00   0.50    2.83    --  107.75-152.00 -39.00   50
 12  ω     85.00 118.00   0.50    2.83    --  107.75 152.00   2.00   66
 13  ω    103.00 128.00   0.50    2.83    --  107.75 121.00-156.00   50
 14  ω     48.00  73.00   0.50    2.83    --  107.75-121.00 120.00   50
 15  ω   -119.00 -75.00   0.50    0.71    --  -47.64-125.00-150.00   88
 16  ω    -29.00  28.00   0.50    0.71    --  -47.64  19.00  30.00  114
 17  ω     -9.00  22.00   0.50    0.71    --  -47.64  19.00-120.00   62
 18  ω     74.00  99.00   0.50    0.71    --   47.64 125.00-180.00   50
 19  ω    -25.00  21.00   0.50    0.71    --   47.64 -19.00-150.00   92
 20  ω     25.00 120.00   0.50    0.71    --   47.64  77.00-180.00  190
 21  ω     78.00 119.00   0.50    0.71    --   47.64 125.00  90.00   82
 22  ω   -164.00-136.00   0.50    2.83    -- -106.00 -94.00  60.00   56
 23  ω    -70.00 -34.00   0.50    2.83    -- -106.00  61.00-120.00   72
 24  ω   -177.00 -93.00   0.50    2.83    -- -106.00 -45.00 -60.00  168
 25  ω   -107.00 -39.00   0.50    2.83    -- -106.00 108.00-147.80  136
 26  ω   -106.00 -61.00   0.50    2.83    -- -106.00 103.00  50.25   90
 27  ω   -112.00 -48.00   0.50    2.83    -- -106.00 125.00 -60.00  128
 28  ω   -177.00-115.00   0.50    2.83    -- -106.00 -30.00-180.00  124
 29  ω   -166.00 -83.00   0.50    2.83    -- -106.00-125.00-180.00  166
 30  ω    -74.00 -33.00   0.50    2.83    -- -106.00  61.00-180.00   82
 31  ω     97.00 167.00   0.50    2.83    --  107.75  30.00  30.00  140
 32  ω     96.00 178.00   0.50    2.83    --  107.75  45.00   0.00  164
 33  ω     56.00 106.00   0.50    2.83    --  107.75 -96.00 100.55  100
 34  ω     76.00 106.00   0.50    2.83    --  107.75 -94.00 150.00   60
 35  ω     41.00  67.00   0.50    2.83    --  107.75 -94.00 150.00   52
 36  ω     37.00  62.00   0.50    2.83    --  107.75 -61.00 -90.00   50
 37  ω     55.00 107.00   0.50    2.83    --  107.75-108.00  32.78  104
 38  ω     37.00  97.00   0.50    2.83    --  107.75 -77.00  60.00  120
 39  ω     50.00 100.00   0.50    2.83    --  107.75 -77.00 150.00  100
 40  ω     36.00  67.00   0.50    2.83    --  107.75 -61.00   0.00   62
 41  ω     36.00  62.00   0.50    2.83    --  107.75 -61.00  30.00   52
 42  ω     36.00  62.00   0.50    2.83    --  107.75 -61.00 120.00   52
 43  ω     36.00 102.00   0.50    2.83    --  107.75 -77.00 -90.00  132
 44  ω     99.00 175.00   0.50    2.83    --  107.75  45.00 120.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0737649000
_diffrn_orient_matrix_UB_12      0.0312493000
_diffrn_orient_matrix_UB_13      0.0872016000
_diffrn_orient_matrix_UB_21      0.0878863000
_diffrn_orient_matrix_UB_22      -0.0034655000
_diffrn_orient_matrix_UB_23      -0.0283284000
_diffrn_orient_matrix_UB_31      0.0202245000
_diffrn_orient_matrix_UB_32      0.0937736000
_diffrn_orient_matrix_UB_33      0.0100426000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            60466
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.109
_diffrn_reflns_theta_min         2.646
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.665
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.370
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
'CrysAlisPro 1.171.40.57a (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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       needle
_exptl_crystal_F_000             1566
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.989
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1022
_refine_ls_number_reflns         17224
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0571
_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)+(0.0856P)²+2.2179P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14020
_reflns_number_total             17224
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja0c02311_si_002.cif
_cod_data_source_block           cx1598c
_cod_original_cell_volume        4189.71(8)
_cod_database_code               4134790
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C128 H98 F48N12 P8'
_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.
;
_cell_oxdiff_angle_alpha         108.9696(10)
_cell_oxdiff_angle_beta          106.6927(10)
_cell_oxdiff_angle_gamma         102.2968(10)
_cell_oxdiff_length_a            14.66878(16)
_cell_oxdiff_length_b            17.5021(2)
_cell_oxdiff_length_c            19.14358(19)
_cell_oxdiff_measurement_reflns_used 21244
_cell_oxdiff_volume              4189.71(8)
_diffrn_oxdiff_digest_frames
;
01cbf7fed9320db7d673216e211f4d3da504090ec72
;
_diffrn_oxdiff_digest_hkl
;
014defb7c44be2eb47de6e149f8822ce2bed9b
;
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F8A-F12A \\sim F8A-F10A \\sim F8A-F11A \\sim F8A-F9A \\sim F12A-F7A \\sim
F12A-F11A \\sim F12A-F9A ~
 F7A-F10A \\sim F7A-F11A \\sim F7A-F9A \\sim F10A-F11A \\sim F10A-F9A
 with sigma of 0.02
 P2A-F8A \\sim P2A-F12A \\sim P2A-F7A \\sim P2A-F10A \\sim P2A-F11A \\sim
P2A-F9A
 with sigma of 0.01
 F8-F12 \\sim F8-F10 \\sim F8-F11 \\sim F8-F9 \\sim F12-F7 \\sim F12-F11 \\sim
F12-F9 \\sim F7-F10 \\sim F7-
 F11 \\sim F7-F9 \\sim F10-F11 \\sim F10-F9
 with sigma of 0.02
 P2-F8 \\sim P2-F12 \\sim P2-F7 \\sim P2-F10 \\sim P2-F11 \\sim P2-F9
 with sigma of 0.01
3. Rigid body (RIGU) restrains
 F7, F8, F9, F10, F11, F12, F7A, F8A, F9A, F10A, F11A, F12A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(P2A)=Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(2)
 Sof(P2)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=FVAR(2)
 Fixed Sof: H5(0.5) H6A(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C25(H25A,H25B), C32(H32A,H32B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13),
 C15(H15), C17(H17), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C27(H27),
  C28(H28), C30(H30), C31(H31), C34(H34), C36(H36), C38(H38), C40(H40),
 C41(H41), C42(H42), C43(H43), C45(H45), C46(H46), C47(H47), C48(H48), N5(H5),
 N6(H6A), C50(H50), C51(H51), C53(H53), C55(H55), C56(H56), C60(H60), C61(H61),
 C62(H62), C63(H63), C64(H64)
5.c Idealised Me refined as rotating group:
 C65(H65A,H65B,H65C), C67(H67A,H67B,H67C)
;
_olex2_date_sample_data_collection 2019-08-12
_olex2_date_sample_submission    2019-07-24
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder with Paratone oil'
_olex2_submission_original_sample_id cx1598c
_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 3.885
_oxdiff_exptl_absorpt_empirical_full_min 0.354
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
N1 N 0.24963(14) 0.06477(11) 0.36236(11) 0.0314(4) Uani 1 1 d . . . . .
N2 N 0.31231(13) 0.41689(12) 0.06592(10) 0.0275(4) Uani 1 1 d . . . . .
N3 N 0.96857(13) 0.42409(12) 0.75978(10) 0.0262(3) Uani 1 1 d . . . . .
N4 N 1.00320(12) 0.75774(10) 0.44204(10) 0.0229(3) Uani 1 1 d . . . . .
C1 C -0.03210(15) 0.15340(12) 0.55443(12) 0.0254(4) Uani 1 1 d . . . . .
H1A H -0.104747 0.125003 0.527335 0.030 Uiso 1 1 calc R . . . .
H1B H -0.011569 0.155275 0.608029 0.030 Uiso 1 1 calc R . . . .
C2 C 0.02145(15) 0.10598(12) 0.50885(12) 0.0235(4) Uani 1 1 d . . . . .
C3 C -0.02384(16) 0.06309(13) 0.42625(13) 0.0297(4) Uani 1 1 d . . . . .
H3 H -0.089990 0.058717 0.399782 0.036 Uiso 1 1 calc R . . . .
C4 C 0.02843(17) 0.02657(13) 0.38256(13) 0.0318(4) Uani 1 1 d . . . . .
H4 H -0.002265 -0.001451 0.327044 0.038 Uiso 1 1 calc R . . . .
C5 C 0.12705(16) 0.03205(12) 0.42216(13) 0.0286(4) Uani 1 1 d . . . . .
C6 C 0.17167(16) 0.07343(13) 0.50494(13) 0.0304(4) Uani 1 1 d . . . . .
H6 H 0.237237 0.076622 0.531566 0.036 Uiso 1 1 calc R . . . .
C7 C 0.11950(15) 0.11001(13) 0.54828(12) 0.0278(4) Uani 1 1 d . . . . .
H7 H 0.149899 0.137345 0.603844 0.033 Uiso 1 1 calc R . . . .
C8 C 0.18476(18) -0.00430(13) 0.37398(15) 0.0349(5) Uani 1 1 d . . . . .
H8A H 0.226677 -0.029823 0.401597 0.042 Uiso 1 1 calc R . . . .
H8B H 0.137670 -0.048881 0.322282 0.042 Uiso 1 1 calc R . . . .
C9 C 0.20557(19) 0.09868(18) 0.31212(15) 0.0453(6) Uani 1 1 d . . . . .
H9 H 0.135746 0.076917 0.284668 0.054 Uiso 1 1 calc R . . . .
C10 C 0.26160(19) 0.16369(19) 0.30129(15) 0.0451(6) Uani 1 1 d . . . . .
H10 H 0.230108 0.186260 0.267296 0.054 Uiso 1 1 calc R . . . .
C11 C 0.36773(16) 0.19631(14) 0.34215(12) 0.0305(4) Uani 1 1 d . . . . .
C12 C 0.40810(17) 0.16451(16) 0.39611(17) 0.0414(6) Uani 1 1 d . . . . .
H12 H 0.477122 0.187793 0.427072 0.050 Uiso 1 1 calc R . . . .
C13 C 0.34913(18) 0.09924(17) 0.40547(18) 0.0430(6) Uani 1 1 d . . . . .
H13 H 0.378775 0.078833 0.442199 0.052 Uiso 1 1 calc R . . . .
C14 C 0.43063(15) 0.26457(14) 0.32972(12) 0.0283(4) Uani 1 1 d . . . . .
C15 C 0.39039(14) 0.28400(13) 0.26491(12) 0.0263(4) Uani 1 1 d . . . . .
H15 H 0.323021 0.254816 0.230335 0.032 Uiso 1 1 calc R . . . .
C16 C 0.44954(14) 0.34624(13) 0.25143(11) 0.0258(4) Uani 1 1 d . . . . .
C17 C 0.55099(14) 0.38972(13) 0.30344(12) 0.0257(4) Uani 1 1 d . . . . .
H17 H 0.590987 0.430664 0.293620 0.031 Uiso 1 1 calc R . . . .
C18 C 0.59347(14) 0.37301(13) 0.36971(11) 0.0253(4) Uani 1 1 d . . . . .
C19 C 0.53218(15) 0.31074(14) 0.38221(12) 0.0284(4) Uani 1 1 d . . . . .
H19 H 0.558948 0.299256 0.426446 0.034 Uiso 1 1 calc R . . . .
C20 C 0.40486(14) 0.36939(14) 0.18446(12) 0.0266(4) Uani 1 1 d . . . . .
C21 C 0.32147(16) 0.31024(15) 0.11519(13) 0.0329(5) Uani 1 1 d . . . . .
H21 H 0.296676 0.253583 0.108123 0.040 Uiso 1 1 calc R . . . .
C22 C 0.27634(16) 0.33622(15) 0.05763(13) 0.0329(5) Uani 1 1 d . . . . .
H22 H 0.220026 0.297084 0.012331 0.039 Uiso 1 1 calc R . . . .
C23 C 0.39582(15) 0.47451(15) 0.13009(12) 0.0289(4) Uani 1 1 d . . . . .
H23 H 0.421792 0.529732 0.133985 0.035 Uiso 1 1 calc R . . . .
C24 C 0.44223(14) 0.45161(14) 0.18941(12) 0.0278(4) Uani 1 1 d . . . . .
H24 H 0.499420 0.491649 0.233457 0.033 Uiso 1 1 calc R . . . .
C25 C 0.25412(16) 0.44782(15) 0.00937(12) 0.0299(4) Uani 1 1 d . . . . .
H25A H 0.215921 0.400774 -0.042987 0.036 Uiso 1 1 calc R . . . .
H25B H 0.300094 0.492150 0.003770 0.036 Uiso 1 1 calc R . . . .
C26 C 0.18326(15) 0.48329(14) 0.04300(11) 0.0263(4) Uani 1 1 d . . . . .
C27 C 0.09546(15) 0.42761(14) 0.03674(11) 0.0273(4) Uani 1 1 d . . . . .
H27 H 0.077594 0.368805 0.007988 0.033 Uiso 1 1 calc R . . . .
C28 C 0.03404(15) 0.45943(14) 0.07333(12) 0.0282(4) Uani 1 1 d . . . . .
H28 H -0.024790 0.421882 0.068973 0.034 Uiso 1 1 calc R . . . .
C29 C 0.06036(15) 0.54683(14) 0.11617(11) 0.0268(4) Uani 1 1 d . . . . .
C30 C 0.14685(16) 0.60283(14) 0.12112(13) 0.0310(4) Uani 1 1 d . . . . .
H30 H 0.164045 0.661671 0.149266 0.037 Uiso 1 1 calc R . . . .
C31 C 0.20804(15) 0.57122(15) 0.08406(13) 0.0305(4) Uani 1 1 d . . . . .
H31 H 0.265516 0.608962 0.086788 0.037 Uiso 1 1 calc R . . . .
C32 C -0.00191(17) 0.58113(16) 0.16073(12) 0.0313(4) Uani 1 1 d . . . . .
H32A H 0.007256 0.640261 0.168456 0.038 Uiso 1 1 calc R . . . .
H32B H -0.073037 0.547552 0.130119 0.038 Uiso 1 1 calc R . . . .
C33 C 0.70204(14) 0.42115(13) 0.42463(11) 0.0240(4) Uani 1 1 d . . . . .
C34 C 0.76071(14) 0.48530(13) 0.41198(11) 0.0245(4) Uani 1 1 d . . . . .
H34 H 0.731911 0.496341 0.367867 0.029 Uiso 1 1 calc R . . . .
C35 C 0.86147(14) 0.53365(12) 0.46343(11) 0.0216(4) Uani 1 1 d . . . . .
C36 C 0.90442(14) 0.51643(12) 0.52946(11) 0.0213(4) Uani 1 1 d . . . . .
H36 H 0.971549 0.547268 0.563898 0.026 Uiso 1 1 calc R . . . .
C37 C 0.84729(14) 0.45352(12) 0.54380(11) 0.0216(4) Uani 1 1 d . . . . .
C38 C 0.74707(14) 0.40582(12) 0.49119(11) 0.0229(4) Uani 1 1 d . . . . .
H38 H 0.709697 0.363077 0.500724 0.027 Uiso 1 1 calc R . . . .
C39 C 0.89124(14) 0.44151(12) 0.61802(11) 0.0221(4) Uani 1 1 d . . . . .
C40 C 0.96796(15) 0.50991(13) 0.68615(11) 0.0254(4) Uani 1 1 d . . . . .
H40 H 0.993859 0.562229 0.684286 0.030 Uiso 1 1 calc R . . . .
C41 C 1.00472(15) 0.49918(14) 0.75577(12) 0.0275(4) Uani 1 1 d . . . . .
H41 H 1.055468 0.544710 0.800841 0.033 Uiso 1 1 calc R . . . .
C42 C 0.89623(15) 0.35668(14) 0.69491(12) 0.0271(4) Uani 1 1 d . . . . .
H42 H 0.872764 0.304804 0.698293 0.032 Uiso 1 1 calc R . . . .
C43 C 0.85663(15) 0.36377(13) 0.62361(12) 0.0249(4) Uani 1 1 d . . . . .
H43 H 0.806853 0.316783 0.579225 0.030 Uiso 1 1 calc R . . . .
C44 C 0.91681(14) 0.60649(12) 0.45230(11) 0.0219(4) Uani 1 1 d . . . . .
C45 C 0.88303(14) 0.61772(12) 0.38121(11) 0.0229(4) Uani 1 1 d . . . . .
H45 H 0.831139 0.573416 0.335913 0.027 Uiso 1 1 calc R . . . .
C46 C 0.92595(14) 0.69367(13) 0.37787(11) 0.0243(4) Uani 1 1 d . . . . .
H46 H 0.901374 0.700892 0.330794 0.029 Uiso 1 1 calc R . . . .
C47 C 1.04403(14) 0.74623(13) 0.50868(12) 0.0264(4) Uani 1 1 d . . . . .
H47 H 1.100844 0.789279 0.550890 0.032 Uiso 1 1 calc R . . . .
C48 C 1.00340(15) 0.67214(13) 0.51554(12) 0.0267(4) Uani 1 1 d . . . . .
H48 H 1.032990 0.665165 0.561968 0.032 Uiso 1 1 calc R . . . .
N5 N 0.42218(15) 0.52830(14) 0.40867(13) 0.0449(5) Uani 1 1 d . . . . .
H5 H 0.458017 0.521393 0.448924 0.054 Uiso 0.5 1 calc R . P . .
N6 N 0.37591(15) 0.40367(14) 0.48368(13) 0.0442(5) Uani 1 1 d . . . . .
H6A H 0.430179 0.443272 0.493918 0.053 Uiso 0.5 1 calc R . P . .
C49 C 0.45427(19) 0.58731(17) 0.38121(16) 0.0458(6) Uani 1 1 d . . . . .
C50 C 0.37095(19) 0.57997(19) 0.31399(16) 0.0483(6) Uani 1 1 d . . . . .
H50 H 0.372146 0.613571 0.285092 0.058 Uiso 1 1 calc R . . . .
C51 C 0.2914(2) 0.51509(19) 0.30143(16) 0.0494(7) Uani 1 1 d . . . . .
H51 H 0.227335 0.495093 0.261393 0.059 Uiso 1 1 calc R . . . .
C52 C 0.32241(18) 0.48180(17) 0.36064(15) 0.0449(6) Uani 1 1 d . . . . .
C53 C 0.26138(18) 0.41484(17) 0.36719(16) 0.0470(7) Uani 1 1 d . . . . .
H53 H 0.195733 0.389483 0.328704 0.056 Uiso 1 1 calc R . . . .
C54 C 0.28365(19) 0.37966(17) 0.42296(16) 0.0459(6) Uani 1 1 d . . . . .
C55 C 0.21357(19) 0.31160(17) 0.42699(17) 0.0493(7) Uani 1 1 d . . . . .
H55 H 0.145886 0.283605 0.392830 0.059 Uiso 1 1 calc R . . . .
C56 C 0.26275(19) 0.29528(17) 0.48880(17) 0.0473(6) Uani 1 1 d . . . . .
H56 H 0.235729 0.254472 0.505296 0.057 Uiso 1 1 calc R . . . .
C57 C 0.36638(19) 0.35404(16) 0.52456(16) 0.0438(6) Uani 1 1 d . . . . .
C58 C 0.44511(19) 0.35630(17) 0.58874(16) 0.0450(6) Uani 1 1 d . . . . .
C59 C 0.42094(19) 0.29936(18) 0.62926(16) 0.0493(7) Uani 1 1 d . . . . .
C60 C 0.3615(2) 0.3146(2) 0.67389(17) 0.0550(8) Uani 1 1 d . . . . .
H60 H 0.336469 0.359694 0.677129 0.066 Uiso 1 1 calc R . . . .
C61 C 0.3390(2) 0.2647(3) 0.71326(18) 0.0701(10) Uani 1 1 d . . . . .
H61 H 0.300467 0.276600 0.743788 0.084 Uiso 1 1 calc R . . . .
C62 C 0.3741(3) 0.1969(3) 0.7070(2) 0.0796(12) Uani 1 1 d . . . . .
H62 H 0.358298 0.162425 0.732888 0.096 Uiso 1 1 calc R . . . .
C63 C 0.4326(3) 0.1792(3) 0.6626(2) 0.0758(11) Uani 1 1 d . . . . .
H63 H 0.455192 0.132755 0.658253 0.091 Uiso 1 1 calc R . . . .
C64 C 0.4575(2) 0.2313(2) 0.62453(19) 0.0588(8) Uani 1 1 d . . . . .
H64 H 0.498407 0.220715 0.595959 0.071 Uiso 1 1 calc R . . . .
P1 P 0.65713(5) 0.11381(5) 0.48197(7) 0.0622(2) Uani 1 1 d . . . . .
F1 F 0.56277(15) 0.06645(16) 0.39947(17) 0.0921(8) Uani 1 1 d . . . . .
F2 F 0.75359(12) 0.16166(10) 0.56609(13) 0.0611(5) Uani 1 1 d . . . . .
F3 F 0.6400(3) 0.0227(2) 0.4892(3) 0.0660(11) Uani 0.599(5) 1 d . . P A 1
F4 F 0.5823(2) 0.1332(3) 0.5177(2) 0.0661(11) Uani 0.599(5) 1 d . . P A 1
F5 F 0.6695(3) 0.19346(17) 0.45918(19) 0.0616(11) Uani 0.599(5) 1 d . . P A 1
F6 F 0.7277(2) 0.0819(2) 0.43017(17) 0.0611(10) Uani 0.599(5) 1 d . . P A 1
F3A F 0.6932(6) 0.0442(4) 0.4762(5) 0.099(4) Uani 0.401(5) 1 d . . P A 2
F4A F 0.5961(6) 0.0912(5) 0.5405(5) 0.112(3) Uani 0.401(5) 1 d . . P A 2
F5A F 0.6365(3) 0.2139(3) 0.5252(3) 0.0665(17) Uani 0.401(5) 1 d . . P A 2
F6A F 0.7326(4) 0.1706(4) 0.4631(3) 0.0743(18) Uani 0.401(5) 1 d . . P A 2
P2 P 0.0420(3) 0.2566(2) 0.13575(19) 0.0521(10) Uani 0.506(6) 1 d D . P B 1
F7 F 0.1275(3) 0.2185(4) 0.1670(3) 0.0738(17) Uani 0.506(6) 1 d D U P B 1
F8 F -0.0415(4) 0.2958(3) 0.1057(4) 0.0851(17) Uani 0.506(6) 1 d D U P B 1
F9 F 0.1275(4) 0.3464(3) 0.1682(3) 0.0773(17) Uani 0.506(6) 1 d D U P B 1
F10 F 0.0313(4) 0.2833(3) 0.2202(2) 0.0783(18) Uani 0.506(6) 1 d D U P B 1
F11 F -0.0430(6) 0.1661(5) 0.1038(6) 0.061(2) Uani 0.506(6) 1 d D U P B 1
F12 F 0.0518(7) 0.2284(6) 0.0519(4) 0.103(4) Uani 0.506(6) 1 d D U P B 1
P3 P 0.08910(4) 0.20652(4) 0.80773(3) 0.03272(14) Uani 1 1 d . . . . .
F13 F 0.18435(13) 0.20254(12) 0.87045(9) 0.0562(4) Uani 1 1 d . . . . .
F14 F -0.00791(13) 0.21015(11) 0.74427(8) 0.0525(4) Uani 1 1 d . . . . .
F15 F 0.15447(16) 0.29622(10) 0.81572(10) 0.0612(5) Uani 1 1 d . . . . .
F16 F 0.11889(12) 0.15809(9) 0.73552(8) 0.0447(3) Uani 1 1 d . . . . .
F17 F 0.02162(13) 0.11690(9) 0.79843(8) 0.0471(4) Uani 1 1 d . . . . .
F18 F 0.05910(12) 0.25613(9) 0.87921(8) 0.0433(3) Uani 1 1 d . . . . .
P4 P 0.70227(4) 0.45161(4) 0.15627(3) 0.03197(13) Uani 1 1 d . . . . .
F19 F 0.77225(11) 0.42656(10) 0.22086(10) 0.0478(4) Uani 1 1 d . . . . .
F20 F 0.63302(12) 0.47865(13) 0.09475(9) 0.0556(4) Uani 1 1 d . . . . .
F21 F 0.79504(10) 0.53777(10) 0.18567(9) 0.0427(3) Uani 1 1 d . . . . .
F22 F 0.66710(10) 0.50296(9) 0.22425(7) 0.0361(3) Uani 1 1 d . . . . .
F23 F 0.61039(11) 0.36682(10) 0.12971(9) 0.0517(4) Uani 1 1 d . . . . .
F24 F 0.74031(15) 0.40227(14) 0.09128(11) 0.0714(6) Uani 1 1 d . . . . .
O1 O 0.55801(13) 0.34875(13) 0.88998(11) 0.0492(4) Uani 1 1 d . . . . .
C65 C 0.4314(2) 0.3389(3) 0.9414(2) 0.0856(14) Uani 1 1 d . . . . .
H65A H 0.452553 0.357581 0.998295 0.128 Uiso 1 1 calc GR . . . .
H65B H 0.368625 0.291843 0.915017 0.128 Uiso 1 1 calc GR . . . .
H65C H 0.422550 0.385502 0.927335 0.128 Uiso 1 1 calc GR . . . .
C66 C 0.50888(18) 0.31109(17) 0.91608(14) 0.0421(6) Uani 1 1 d . . . . .
C67 C 0.5276(5) 0.2331(3) 0.9241(3) 0.0989(16) Uani 1 1 d . . . . .
H67A H 0.562043 0.211825 0.890336 0.148 Uiso 1 1 calc GR . . . .
H67B H 0.464241 0.189669 0.908229 0.148 Uiso 1 1 calc GR . . . .
H67C H 0.568624 0.247754 0.978746 0.148 Uiso 1 1 calc GR . . . .
P2A P 0.0657(2) 0.2357(2) 0.13358(19) 0.0443(8) Uani 0.494(6) 1 d D . P B 2
F7A F 0.1328(3) 0.1745(3) 0.1232(3) 0.0722(14) Uani 0.494(6) 1 d D U P B 2
F8A F 0.0051(4) 0.3016(3) 0.1477(4) 0.0701(16) Uani 0.494(6) 1 d D U P B 2
F9A F 0.1689(3) 0.3164(4) 0.1790(3) 0.0747(18) Uani 0.494(6) 1 d D U P B 2
F10A F 0.0743(3) 0.2327(3) 0.2177(2) 0.0666(15) Uani 0.494(6) 1 d D U P B 2
F11A F -0.0363(5) 0.1561(5) 0.0893(6) 0.057(2) Uani 0.494(6) 1 d D U P B 2
F12A F 0.0615(5) 0.2395(5) 0.0513(3) 0.0458(14) Uani 0.494(6) 1 d 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'
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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 1 -3 0.0880
0 -1 0 0.0019
0 0 -1 0.0200
1 11 -4 0.0375
-9 4 5 0.0999
1 -11 3 0.0074
0 -1 11 0.0186
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
C9 N1 C8 119.51(19) . . ?
C13 N1 C8 120.9(2) . . ?
C13 N1 C9 119.3(2) . . ?
C22 N2 C23 120.79(18) . . ?
C22 N2 C25 120.32(17) . . ?
C23 N2 C25 118.51(19) . . ?
C41 N3 C32 119.03(18) . 2_666 ?
C41 N3 C42 120.55(17) . . ?
C42 N3 C32 120.12(18) . 2_666 ?
C46 N4 C1 120.21(16) . 2_666 ?
C47 N4 C1 118.55(16) . 2_666 ?
C47 N4 C46 120.34(17) . . ?
N4 C1 C2 106.82(15) 2_666 . ?
C3 C2 C1 119.90(18) . . ?
C3 C2 C7 119.31(19) . . ?
C7 C2 C1 120.62(18) . . ?
C2 C3 C4 120.7(2) . . ?
C3 C4 C5 119.8(2) . . ?
C4 C5 C8 119.3(2) . . ?
C6 C5 C4 119.56(19) . . ?
C6 C5 C8 121.1(2) . . ?
C7 C6 C5 120.5(2) . . ?
C6 C7 C2 120.11(19) . . ?
N1 C8 C5 110.19(17) . . ?
C10 C9 N1 121.6(2) . . ?
C9 C10 C11 119.4(2) . . ?
C10 C11 C14 120.7(2) . . ?
C12 C11 C10 117.0(2) . . ?
C12 C11 C14 122.28(19) . . ?
C13 C12 C11 121.7(2) . . ?
N1 C13 C12 120.7(2) . . ?
C15 C14 C11 120.29(18) . . ?
C15 C14 C19 118.68(19) . . ?
C19 C14 C11 121.03(19) . . ?
C16 C15 C14 120.74(18) . . ?
C15 C16 C17 119.41(18) . . ?
C15 C16 C20 120.39(17) . . ?
C17 C16 C20 120.15(18) . . ?
C18 C17 C16 121.48(19) . . ?
C17 C18 C33 120.20(18) . . ?
C19 C18 C17 117.92(18) . . ?
C19 C18 C33 121.88(18) . . ?
C18 C19 C14 121.74(19) . . ?
C21 C20 C16 121.5(2) . . ?
C24 C20 C16 121.04(18) . . ?
C24 C20 C21 117.44(19) . . ?
C22 C21 C20 119.8(2) . . ?
N2 C22 C21 120.93(19) . . ?
N2 C23 C24 120.1(2) . . ?
C23 C24 C20 120.77(19) . . ?
N2 C25 C26 108.01(15) . . ?
C27 C26 C25 119.8(2) . . ?
C27 C26 C31 119.63(19) . . ?
C31 C26 C25 120.45(19) . . ?
C26 C27 C28 120.2(2) . . ?
C29 C28 C27 120.07(19) . . ?
C28 C29 C30 119.90(19) . . ?
C28 C29 C32 120.24(19) . . ?
C30 C29 C32 119.8(2) . . ?
C29 C30 C31 120.1(2) . . ?
C26 C31 C30 120.0(2) . . ?
N3 C32 C29 108.70(16) 2_666 . ?
C34 C33 C18 120.51(17) . . ?
C34 C33 C38 117.74(17) . . ?
C38 C33 C18 121.72(18) . . ?
C33 C34 C35 122.24(18) . . ?
C34 C35 C44 120.08(17) . . ?
C36 C35 C34 118.56(18) . . ?
C36 C35 C44 121.07(17) . . ?
C37 C36 C35 120.28(17) . . ?
C36 C37 C38 119.97(17) . . ?
C36 C37 C39 119.46(17) . . ?
C38 C37 C39 120.45(17) . . ?
C33 C38 C37 121.20(18) . . ?
C40 C39 C37 120.22(18) . . ?
C43 C39 C37 121.96(17) . . ?
C43 C39 C40 117.80(17) . . ?
C41 C40 C39 119.66(19) . . ?
N3 C41 C40 121.18(18) . . ?
N3 C42 C43 120.75(19) . . ?
C42 C43 C39 120.03(18) . . ?
C45 C44 C35 122.35(17) . . ?
C45 C44 C48 116.53(18) . . ?
C48 C44 C35 120.96(17) . . ?
C46 C45 C44 120.56(17) . . ?
N4 C46 C45 120.71(18) . . ?
N4 C47 C48 121.16(18) . . ?
C47 C48 C44 120.13(18) . . ?
C49 N5 C52 107.8(2) . . ?
C57 N6 C54 108.2(2) . . ?
N5 C49 C50 109.3(2) . . ?
N5 C49 C58 125.1(3) . 2_666 ?
C58 C49 C50 125.5(3) 2_666 . ?
C51 C50 C49 106.5(3) . . ?
C50 C51 C52 108.3(2) . . ?
N5 C52 C51 108.1(3) . . ?
N5 C52 C53 126.5(3) . . ?
C53 C52 C51 125.4(2) . . ?
C52 C53 C54 129.5(2) . . ?
N6 C54 C53 126.3(3) . . ?
N6 C54 C55 108.1(3) . . ?
C53 C54 C55 125.6(2) . . ?
C56 C55 C54 108.3(2) . . ?
C55 C56 C57 106.5(3) . . ?
N6 C57 C56 109.0(2) . . ?
N6 C57 C58 125.5(2) . . ?
C58 C57 C56 125.5(3) . . ?
C49 C58 C59 118.4(3) 2_666 . ?
C57 C58 C49 122.9(3) . 2_666 ?
C57 C58 C59 118.7(2) . . ?
C60 C59 C58 119.7(3) . . ?
C60 C59 C64 118.6(3) . . ?
C64 C59 C58 121.7(3) . . ?
C61 C60 C59 121.5(3) . . ?
C60 C61 C62 119.2(4) . . ?
C61 C62 C63 120.9(4) . . ?
C62 C63 C64 119.7(4) . . ?
C63 C64 C59 120.0(3) . . ?
F1 P1 F2 179.68(12) . . ?
F1 P1 F3 87.84(17) . . ?
F1 P1 F6 87.09(14) . . ?
F1 P1 F4A 97.2(3) . . ?
F1 P1 F5A 101.35(17) . . ?
F2 P1 F3 91.89(15) . . ?
F2 P1 F6 92.72(12) . . ?
F2 P1 F4A 82.8(3) . . ?
F2 P1 F5A 78.97(15) . . ?
F3 P1 F6 85.5(2) . . ?
F4 P1 F1 85.20(17) . . ?
F4 P1 F2 94.98(16) . . ?
F4 P1 F3 92.2(2) . . ?
F4 P1 F5 93.6(3) . . ?
F4 P1 F6 172.05(18) . . ?
F5 P1 F1 84.68(14) . . ?
F5 P1 F2 95.57(12) . . ?
F5 P1 F3 170.1(2) . . ?
F5 P1 F6 87.7(2) . . ?
F3A P1 F1 97.0(3) . . ?
F3A P1 F2 82.7(3) . . ?
F3A P1 F4A 91.7(6) . . ?
F3A P1 F5A 160.3(3) . . ?
F3A P1 F6A 101.4(6) . . ?
F4A P1 F5A 79.0(4) . . ?
F6A P1 F1 102.6(2) . . ?
F6A P1 F2 77.5(2) . . ?
F6A P1 F4A 154.6(3) . . ?
F6A P1 F5A 81.6(3) . . ?
F8 P2 F7 179.1(4) . . ?
F8 P2 F10 90.0(3) . . ?
F8 P2 F11 90.4(4) . . ?
F9 P2 F7 89.0(3) . . ?
F9 P2 F8 90.2(3) . . ?
F9 P2 F10 90.2(3) . . ?
F9 P2 F11 179.4(5) . . ?
F10 P2 F7 89.7(3) . . ?
F11 P2 F7 90.4(4) . . ?
F11 P2 F10 89.7(4) . . ?
F12 P2 F7 90.0(4) . . ?
F12 P2 F8 90.3(4) . . ?
F12 P2 F9 90.8(4) . . ?
F12 P2 F10 179.0(4) . . ?
F12 P2 F11 89.4(5) . . ?
F13 P3 F14 179.64(11) . . ?
F13 P3 F16 90.63(9) . . ?
F13 P3 F18 90.06(8) . . ?
F15 P3 F13 90.91(11) . . ?
F15 P3 F14 89.41(11) . . ?
F15 P3 F16 89.71(8) . . ?
F15 P3 F17 178.76(11) . . ?
F15 P3 F18 89.52(9) . . ?
F16 P3 F14 89.51(8) . . ?
F17 P3 F13 90.33(10) . . ?
F17 P3 F14 89.34(9) . . ?
F17 P3 F16 90.32(8) . . ?
F17 P3 F18 90.44(8) . . ?
F18 P3 F14 89.81(8) . . ?
F18 P3 F16 178.97(9) . . ?
F19 P4 F22 88.57(8) . . ?
F20 P4 F19 178.21(10) . . ?
F20 P4 F21 90.61(9) . . ?
F20 P4 F22 89.72(9) . . ?
F20 P4 F23 90.31(9) . . ?
F21 P4 F19 88.81(8) . . ?
F21 P4 F22 88.60(7) . . ?
F23 P4 F19 90.23(9) . . ?
F23 P4 F21 178.32(9) . . ?
F23 P4 F22 90.00(8) . . ?
F24 P4 F19 90.17(11) . . ?
F24 P4 F20 91.53(11) . . ?
F24 P4 F21 90.18(10) . . ?
F24 P4 F22 178.26(9) . . ?
F24 P4 F23 91.19(10) . . ?
O1 C66 C65 122.5(3) . . ?
O1 C66 C67 118.6(3) . . ?
C65 C66 C67 118.8(4) . . ?
F8A P2A F7A 176.5(3) . . ?
F8A P2A F9A 88.5(3) . . ?
F9A P2A F7A 88.0(3) . . ?
F10A P2A F7A 89.8(3) . . ?
F10A P2A F8A 89.5(3) . . ?
F10A P2A F9A 89.2(3) . . ?
F11A P2A F7A 92.1(4) . . ?
F11A P2A F8A 91.4(4) . . ?
F11A P2A F9A 179.6(4) . . ?
F11A P2A F10A 90.4(4) . . ?
F12A P2A F7A 88.8(3) . . ?
F12A P2A F8A 91.8(3) . . ?
F12A P2A F9A 89.2(3) . . ?
F12A P2A F10A 177.9(3) . . ?
F12A P2A F11A 91.2(4) . . ?
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
N1 C8 1.491(3) . ?
N1 C9 1.368(3) . ?
N1 C13 1.336(3) . ?
N2 C22 1.336(3) . ?
N2 C23 1.353(3) . ?
N2 C25 1.497(3) . ?
N3 C32 1.498(2) 2_666 ?
N3 C41 1.344(3) . ?
N3 C42 1.348(3) . ?
N4 C1 1.496(2) 2_666 ?
N4 C46 1.347(2) . ?
N4 C47 1.344(3) . ?
C1 C2 1.506(3) . ?
C2 C3 1.385(3) . ?
C2 C7 1.393(3) . ?
C3 C4 1.388(3) . ?
C4 C5 1.393(3) . ?
C5 C6 1.386(3) . ?
C5 C8 1.506(3) . ?
C6 C7 1.383(3) . ?
C9 C10 1.366(4) . ?
C10 C11 1.412(3) . ?
C11 C12 1.375(3) . ?
C11 C14 1.475(3) . ?
C12 C13 1.374(3) . ?
C14 C15 1.394(3) . ?
C14 C19 1.408(3) . ?
C15 C16 1.384(3) . ?
C16 C17 1.400(3) . ?
C16 C20 1.485(3) . ?
C17 C18 1.396(3) . ?
C18 C19 1.389(3) . ?
C18 C33 1.497(3) . ?
C20 C21 1.401(3) . ?
C20 C24 1.388(3) . ?
C21 C22 1.376(3) . ?
C23 C24 1.372(3) . ?
C25 C26 1.510(3) . ?
C26 C27 1.387(3) . ?
C26 C31 1.389(3) . ?
C27 C28 1.391(3) . ?
C28 C29 1.383(3) . ?
C29 C30 1.386(3) . ?
C29 C32 1.507(3) . ?
C30 C31 1.392(3) . ?
C33 C34 1.394(3) . ?
C33 C38 1.395(3) . ?
C34 C35 1.400(3) . ?
C35 C36 1.399(3) . ?
C35 C44 1.471(3) . ?
C36 C37 1.388(3) . ?
C37 C38 1.397(3) . ?
C37 C39 1.485(3) . ?
C39 C40 1.403(3) . ?
C39 C43 1.397(3) . ?
C40 C41 1.377(3) . ?
C42 C43 1.379(3) . ?
C44 C45 1.402(3) . ?
C44 C48 1.411(3) . ?
C45 C46 1.374(3) . ?
C47 C48 1.371(3) . ?
N5 C49 1.361(4) . ?
N5 C52 1.372(3) . ?
N6 C54 1.377(3) . ?
N6 C57 1.356(4) . ?
C49 C50 1.445(4) . ?
C49 C58 1.416(4) 2_666 ?
C50 C51 1.344(4) . ?
C51 C52 1.441(5) . ?
C52 C53 1.380(4) . ?
C53 C54 1.392(5) . ?
C54 C55 1.437(4) . ?
C55 C56 1.349(4) . ?
C56 C57 1.455(3) . ?
C57 C58 1.407(4) . ?
C58 C59 1.494(5) . ?
C59 C60 1.393(4) . ?
C59 C64 1.394(5) . ?
C60 C61 1.375(5) . ?
C61 C62 1.375(6) . ?
C62 C63 1.383(6) . ?
C63 C64 1.393(6) . ?
P1 F1 1.582(3) . ?
P1 F2 1.614(2) . ?
P1 F3 1.617(3) . ?
P1 F4 1.492(3) . ?
P1 F5 1.581(3) . ?
P1 F6 1.686(3) . ?
P1 F3A 1.413(5) . ?
P1 F4A 1.711(7) . ?
P1 F5A 1.810(4) . ?
P1 F6A 1.529(5) . ?
P2 F7 1.600(4) . ?
P2 F8 1.586(5) . ?
P2 F9 1.583(4) . ?
P2 F10 1.594(4) . ?
P2 F11 1.589(6) . ?
P2 F12 1.578(6) . ?
P3 F13 1.5907(17) . ?
P3 F14 1.6125(16) . ?
P3 F15 1.5894(17) . ?
P3 F16 1.6011(14) . ?
P3 F17 1.5898(16) . ?
P3 F18 1.5988(14) . ?
P4 F19 1.6092(16) . ?
P4 F20 1.5884(16) . ?
P4 F21 1.6052(14) . ?
P4 F22 1.6095(13) . ?
P4 F23 1.5941(15) . ?
P4 F24 1.5844(16) . ?
O1 C66 1.192(3) . ?
C65 C66 1.470(4) . ?
C66 C67 1.494(5) . ?
P2A F7A 1.606(4) . ?
P2A F8A 1.601(4) . ?
P2A F9A 1.605(4) . ?
P2A F10A 1.598(4) . ?
P2A F11A 1.586(5) . ?
P2A F12A 1.582(5) . ?
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
5.0100 0.9974 -3.0092 0.1383 0.5221 0.1646
-0.0011 -0.9998 0.0010 -0.0312 0.0033 -0.0938
-0.0017 0.0008 -0.9998 -0.0873 0.0282 -0.0100
0.6380 10.8755 -4.2330 0.0178 0.1383 0.9902
-9.1943 4.1438 4.8439 -0.1263 -0.9596 0.2513
0.7527 -11.1891 3.3910 0.0016 0.0089 -1.0000
-0.1689 -1.2808 11.4118 0.9426 -0.3337 -0.0089
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.445 0.000 0.000 1215.7 327.5 ?
