#------------------------------------------------------------------------------
#$Date: 2021-04-05 17:25:53 +0300 (Mon, 05 Apr 2021) $
#$Revision: 263700 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/02/1560240.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_1560240
loop_
_publ_author_name
'Wilson, Benjamin H.'
'Abdulla, Louae M.'
'Schurko, Robert W.'
'Loeb, Stephen J.'
_publ_section_title
;
 Translational dynamics of a non-degenerate molecular shuttle imbedded in
 a zirconium metal--organic framework
;
_journal_issue                   11
_journal_name_full               'Chemical Science'
_journal_page_first              3944
_journal_page_last               3951
_journal_paper_doi               10.1039/D0SC06837C
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety
'C38 H29 Br2 N4 O4, B F4, C16 H32 O8, 0.5(C4 H10 O), 0.5(C2 H3 N)'
_chemical_formula_sum            'C57 H67.5 B Br2 F4 N4.5 O12.5'
_chemical_formula_weight         1262.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-12 deposited with the CCDC.	2021-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.34(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.49(2)
_cell_length_b                   10.505(4)
_cell_length_c                   43.418(18)
_cell_measurement_reflns_used    101844
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      65.084
_cell_measurement_theta_min      2.121
_cell_volume                     12470(12)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ApexIII
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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_temperature      170.00
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            98593
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        65.084
_diffrn_reflns_theta_max         65.084
_diffrn_reflns_theta_min         2.121
_diffrn_source                   'I\mS Microfocus Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.270
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.4964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1342 before and 0.0735 after correction. The Ratio of minimum to maximum transmission is 0.6596. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       block
_exptl_crystal_F_000             5216
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile, diethyl ether'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.019
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1512
_refine_ls_number_reflns         21024
_refine_ls_number_restraints     474
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1323
_refine_ls_R_factor_gt           0.1139
_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)+(0.1390P)²+90.5684P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2936
_refine_ls_wR_factor_ref         0.3088
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16902
_reflns_number_total             21024
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc06837c2.cif
_cod_data_source_block           bhw319_2_0m
_cod_depositor_comments
'Adding full bibliography for 1560238--1560240.cif.'
_cod_original_cell_volume        12468(12)
_cod_original_formula_sum        'C57 H67.50 B Br2 F4 N4.50 O12.50'
_cod_database_code               1560240
_shelx_shelxl_version_number     2018/3
_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   0.660
_shelx_estimated_absorpt_t_min   0.464
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C113-C114
 1.5 with sigma of 0.02
 C1A-C113
 1.5 with sigma of 0.02
 F7B-F5B
 2.29 with sigma of 0.02
 F5B-F6B
 2.29 with sigma of 0.02
 F5B-F8B
 2.29 with sigma of 0.02
 F8B-F6B
 2.29 with sigma of 0.02
 F6B-F7B
 2.29 with sigma of 0.02
 F7B-F8B
 2.29 with sigma of 0.02
 F5B-B2
 1.402 with sigma of 0.02
 C106-O24
 1.448 with sigma of 0.02
 C102-C101
 1.504 with sigma of 0.02
 C95-C96
 1.504 with sigma of 0.02
 O17-C108
 1.448 with sigma of 0.02
 O23-C105
 1.448 with sigma of 0.02
 O24-C106
 1.448 with sigma of 0.001
 O24-C107
 1.448 with sigma of 0.001
 C100-C99
 1.448 with sigma of 0.01
 C96-C95
 1.504 with sigma of 0.01
 C97-C98
 1.504 with sigma of 0.01
 C99-C100
 1.504 with sigma of 0.01
 C101-C102
 1.504 with sigma of 0.01
 C103-C104
 1.504 with sigma of 0.01
 C105-C106
 1.504 with sigma of 0.01
 C107-C108
 1.504 with sigma of 0.01
 O17-C93
 1.448 with sigma of 0.01
 O18-C94
 1.448 with sigma of 0.01
 O18-C95
 1.448 with sigma of 0.01
 O19-C97
 1.448 with sigma of 0.01
 O20-C98
 1.448 with sigma of 0.01
 O21-C101
 1.448 with sigma of 0.01
 O21-C100
 1.448 with sigma of 0.01
 C102-O22
 1.448 with sigma of 0.01
 O22-C103
 1.448 with sigma of 0.01
 O23-C104
 1.448 with sigma of 0.01
 C106-C107
 2.3 with sigma of 0.02
 C104-C105
 2.3 with sigma of 0.001
 O23-C106
 2.3 with sigma of 0.001
 C38-C37
 1.5 with sigma of 0.02
 C52-C51
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O2 \\sim C28: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O2 \\sim C27 \\sim C28 \\sim C29: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C113 \\sim C114: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C113 \\sim C1A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C28 \\sim C29: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C82 \\sim C83: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O14 \\sim C82: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O14 \\sim C81: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C78 \\sim C81: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O13 \\sim C81: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C33 \\sim C36: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O4 \\sim C36: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O4 \\sim C37: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C37 \\sim C38: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O3 \\sim C36: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C91 \\sim C92: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Rigid body (RIGU) restrains
 B2, F5A, F7A, F8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B2, F5B, F6B, F7B, F8B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, O6, O7, O8, O9, O10, O11, O12, C39, C40, C41, C42, C43, C44, C45, C46,
 C47, C48, C49, C50, C51, C52, C53, C54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O17, O18, O19, O20, O21, O22, O23, O24, C93, C94, C95, C96, C97, C98, C99,
 C100, C101, C102, C103, C104, C105, C106, C107, C108
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C29, C28, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H11H(0.4) H11I(0.4) H11F(0.6) H11G(0.6) C1A(0.6) H1AA(0.6)
 H1AB(0.6) H1AC(0.6) C114(0.4) H11J(0.4) H11K(0.4) H11L(0.4) F5A(0.6) F6A(0.6)
 F7A(0.6) F8A(0.6) F5B(0.4) F6B(0.4) F7B(0.4) F8B(0.4)
6.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C37(H37A,H37B), C82(H82A,H82B), C91(H91A,H91B), C39(H39A,
 H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B),
 C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B),
  C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,
 H53B), C54(H54A,H54B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B),
 C96(H96A,H96B), C97(H97A,H97B), C98(H98A,H98B), C99(H99A,H99B), C100(H10A,
 H10B), C101(H10C,H10D), C102(H10E,H10F), C103(H10G,H10H), C104(H10I,H10J),
 C105(H10K,H10L), C106(H10M,H10N), C107(H10O,H10P), C108(H10Q,H10R), C111(H11A,
 H11B), C113(H11H,H11I), C113(H11F,H11G)
6.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), N4(H4), C4(H4A), C5(H5), C9(H9), C10(H10), C12(H12), C13(H13),
  C17(H17), C18(H18), C22(H22), C23(H23), C25(H25), C26(H26), C31(H31),
 C32(H32), C34(H34), C35(H35), N5(H5A), N7(H7), N8(H8), C58(H58), C59(H59),
 C63(H63), C64(H64), C66(H66), C67(H67), C71(H71), C72(H72), C76(H76), C77(H77),
  C79(H79), C80(H80), C85(H85), C86(H86), C88(H88), C89(H89)
6.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C38(H38A,H38B,H38C), C83(H83A,H83B,H83C), C92(H92A,H92B,
 H92C), C112(H11C,H11D,H11E), C1A(H1AA,H1AB,H1AC), C114(H11J,H11K,H11L),
 C110(H11M,H11N,H11O)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.19286(4) -0.24678(16) 0.27676(4) 0.1190(7) Uani 1 1 d . . . . .
Br2 Br -0.04458(3) -0.32063(8) 0.24898(2) 0.0508(2) Uani 1 1 d . . . . .
O1 O 0.1974(4) 0.0187(10) 0.5790(2) 0.135(4) Uani 1 1 d . . . . .
O2 O 0.2290(3) 0.1900(9) 0.60485(17) 0.096(2) Uani 1 1 d . U . . .
O3 O -0.0961(2) 0.9413(6) 0.30996(14) 0.0656(17) Uani 1 1 d . U . . .
O4 O -0.1557(2) 0.9316(7) 0.33386(17) 0.089(2) Uani 1 1 d . U . . .
N1 N 0.11144(19) -0.0955(5) 0.30608(12) 0.0353(12) Uani 1 1 d . . . . .
H1 H 0.140827 -0.063343 0.314336 0.042 Uiso 1 1 calc R . . . .
N2 N 0.03065(18) -0.1251(4) 0.29651(11) 0.0275(11) Uani 1 1 d . . . . .
N3 N 0.02246(16) 0.4098(4) 0.39854(10) 0.0227(10) Uani 1 1 d . . . . .
H3 H 0.004069 0.432202 0.379416 0.027 Uiso 1 1 calc R . . . .
N4 N 0.07359(17) 0.3025(4) 0.43608(10) 0.0224(10) Uani 1 1 d . . . . .
H4 H 0.094627 0.243662 0.445695 0.027 Uiso 1 1 calc R . . . .
C1 C 0.0694(2) -0.0608(5) 0.31282(13) 0.0291(13) Uani 1 1 d . . . . .
C2 C 0.0984(3) -0.1919(6) 0.28349(14) 0.0385(15) Uani 1 1 d . . . . .
C3 C 0.1242(3) -0.2695(9) 0.26812(19) 0.056(2) Uani 1 1 d . . . . .
C4 C 0.1000(3) -0.3633(8) 0.24830(18) 0.058(2) Uani 1 1 d . . . . .
H4A H 0.117828 -0.418119 0.238280 0.070 Uiso 1 1 calc R . . . .
C5 C 0.0497(3) -0.3807(7) 0.24236(15) 0.0422(16) Uani 1 1 d . . . . .
H5 H 0.033536 -0.446468 0.228349 0.051 Uiso 1 1 calc R . . . .
C6 C 0.0238(2) -0.3024(6) 0.25684(14) 0.0341(14) Uani 1 1 d . . . . .
C7 C 0.0481(2) -0.2085(6) 0.27768(13) 0.0312(13) Uani 1 1 d . . . . .
C8 C 0.0665(2) 0.0369(5) 0.33616(12) 0.0249(12) Uani 1 1 d . . . . .
C9 C 0.0213(2) 0.0610(5) 0.34103(13) 0.0275(12) Uani 1 1 d . . . . .
H9 H -0.006559 0.015524 0.328858 0.033 Uiso 1 1 calc R . . . .
C10 C 0.0161(2) 0.1502(5) 0.36333(13) 0.0246(12) Uani 1 1 d . . . . .
H10 H -0.015075 0.166319 0.366420 0.029 Uiso 1 1 calc R . . . .
C11 C 0.0572(2) 0.2158(5) 0.38113(12) 0.0239(12) Uani 1 1 d . . . . .
C12 C 0.1031(2) 0.1948(6) 0.37638(13) 0.0289(13) Uani 1 1 d . . . . .
H12 H 0.130845 0.241286 0.388303 0.035 Uiso 1 1 calc R . . . .
C13 C 0.1073(2) 0.1049(5) 0.35395(13) 0.0270(12) Uani 1 1 d . . . . .
H13 H 0.138358 0.089380 0.350618 0.032 Uiso 1 1 calc R . . . .
C14 C 0.0515(2) 0.3088(5) 0.40498(13) 0.0235(11) Uani 1 1 d . . . . .
C15 C 0.0580(2) 0.4043(5) 0.45103(13) 0.0216(11) Uani 1 1 d . . . . .
C16 C 0.0701(2) 0.4395(5) 0.48361(13) 0.0256(12) Uani 1 1 d . . . . .
C17 C 0.0481(2) 0.5524(6) 0.48939(14) 0.0301(13) Uani 1 1 d . . . . .
H17 H 0.055075 0.582616 0.510831 0.036 Uiso 1 1 calc R . . . .
C18 C 0.0161(2) 0.6230(5) 0.46493(14) 0.0299(13) Uani 1 1 d . . . . .
H18 H 0.001744 0.697863 0.470567 0.036 Uiso 1 1 calc R . . . .
C19 C 0.0046(2) 0.5883(5) 0.43285(14) 0.0263(12) Uani 1 1 d . . . . .
C20 C 0.0259(2) 0.4738(5) 0.42680(12) 0.0223(11) Uani 1 1 d . . . . .
C21 C 0.1039(2) 0.3630(6) 0.50909(13) 0.0282(13) Uani 1 1 d . . . . .
C22 C 0.1006(2) 0.2314(6) 0.50850(14) 0.0327(14) Uani 1 1 d . . . . .
H22 H 0.076215 0.190456 0.491964 0.039 Uiso 1 1 calc R . . . .
C23 C 0.1329(3) 0.1587(7) 0.53204(16) 0.0461(18) Uani 1 1 d . . . . .
H23 H 0.130893 0.068446 0.531100 0.055 Uiso 1 1 calc R . . . .
C24 C 0.1673(3) 0.2159(9) 0.55635(17) 0.051(2) Uani 1 1 d . . . . .
C25 C 0.1708(3) 0.3469(9) 0.55745(16) 0.050(2) Uani 1 1 d . . . . .
H25 H 0.195009 0.386827 0.574264 0.061 Uiso 1 1 calc R . . . .
C26 C 0.1389(3) 0.4209(7) 0.53410(15) 0.0409(16) Uani 1 1 d . . . . .
H26 H 0.141148 0.511099 0.535242 0.049 Uiso 1 1 calc R . . . .
C27 C 0.2000(4) 0.1337(13) 0.5823(2) 0.080(3) Uani 1 1 d . U . . .
C28 C 0.2568(5) 0.0857(17) 0.6269(3) 0.127(4) Uani 1 1 d . U . . .
H28A H 0.271354 0.022765 0.615303 0.153 Uiso 1 1 calc R . . . .
H28B H 0.236193 0.041625 0.638521 0.153 Uiso 1 1 calc R . . . .
C29 C 0.3008(8) 0.183(3) 0.6520(6) 0.228(12) Uani 1 1 d . U . . .
H29A H 0.323153 0.214660 0.640322 0.342 Uiso 1 1 calc GR . . . .
H29B H 0.319234 0.133476 0.670690 0.342 Uiso 1 1 calc GR . . . .
H29C H 0.284682 0.254667 0.659265 0.342 Uiso 1 1 calc GR . . . .
C30 C -0.0265(2) 0.6654(5) 0.40664(14) 0.0273(12) Uani 1 1 d . . . . .
C31 C -0.0121(2) 0.6908(5) 0.37879(15) 0.0306(13) Uani 1 1 d . . . . .
H31 H 0.017253 0.654381 0.376536 0.037 Uiso 1 1 calc R . . . .
C32 C -0.0397(2) 0.7671(6) 0.35482(15) 0.0345(14) Uani 1 1 d . . . . .
H32 H -0.029110 0.783835 0.336309 0.041 Uiso 1 1 calc R . . . .
C33 C -0.0829(2) 0.8198(6) 0.35763(17) 0.0406(15) Uani 1 1 d . U . . .
C34 C -0.0981(3) 0.7935(7) 0.38469(17) 0.0438(17) Uani 1 1 d . . . . .
H34 H -0.128113 0.827724 0.386517 0.053 Uiso 1 1 calc R . . . .
C35 C -0.0701(2) 0.7181(6) 0.40882(15) 0.0349(14) Uani 1 1 d . . . . .
H35 H -0.080816 0.701857 0.427294 0.042 Uiso 1 1 calc R . . . .
C36 C -0.1115(3) 0.9035(9) 0.3309(2) 0.0592(19) Uani 1 1 d . U . . .
C37 C -0.1897(4) 0.9984(13) 0.3046(3) 0.108(3) Uani 1 1 d D U . . .
H37A H -0.180591 0.981146 0.284590 0.129 Uiso 1 1 calc R . . . .
H37B H -0.224538 0.977414 0.301585 0.129 Uiso 1 1 calc R . . . .
C38 C -0.1778(6) 1.1249(17) 0.3161(5) 0.157(6) Uani 1 1 d D U . . .
H38A H -0.191669 1.185602 0.298805 0.235 Uiso 1 1 calc GR . . . .
H38B H -0.142173 1.134837 0.323322 0.235 Uiso 1 1 calc GR . . . .
H38C H -0.191427 1.141068 0.334098 0.235 Uiso 1 1 calc GR . . . .
Br3 Br 0.54795(3) 0.84824(8) 0.75568(2) 0.0535(2) Uani 1 1 d . . . . .
Br4 Br 0.30823(4) 0.80676(15) 0.70963(3) 0.1061(5) Uani 1 1 d . . . . .
O13 O 0.6094(2) -0.3983(7) 0.69777(16) 0.082(2) Uani 1 1 d . U . . .
O14 O 0.6699(2) -0.3934(8) 0.67441(17) 0.087(2) Uani 1 1 d . U . . .
O15 O 0.2486(3) 0.2009(7) 0.40008(16) 0.083(2) Uani 1 1 d . . . . .
O16 O 0.2908(2) 0.3828(6) 0.40816(13) 0.0653(16) Uani 1 1 d . . . . .
N5 N 0.3942(2) 0.6427(5) 0.68801(12) 0.0389(13) Uani 1 1 d . . . . .
H5A H 0.364925 0.614941 0.677590 0.047 Uiso 1 1 calc R . . . .
N6 N 0.4756(2) 0.6596(5) 0.70355(11) 0.0336(12) Uani 1 1 d . . . . .
N7 N 0.49021(18) 0.1217(4) 0.60347(11) 0.0276(10) Uani 1 1 d . . . . .
H7 H 0.510751 0.106643 0.622439 0.033 Uiso 1 1 calc R . . . .
N8 N 0.43388(17) 0.2126(4) 0.56555(11) 0.0252(10) Uani 1 1 d . . . . .
H8 H 0.410741 0.265896 0.555606 0.030 Uiso 1 1 calc R . . . .
C55 C 0.4375(2) 0.6013(6) 0.68452(14) 0.0314(13) Uani 1 1 d . . . . .
C56 C 0.4565(3) 0.7449(6) 0.72076(15) 0.0362(15) Uani 1 1 d . . . . .
C57 C 0.4792(2) 0.8362(6) 0.74320(14) 0.0363(14) Uani 1 1 d . . . . .
C58 C 0.4509(3) 0.9165(7) 0.75588(16) 0.0470(18) Uani 1 1 d . . . . .
H58 H 0.466342 0.978514 0.771348 0.056 Uiso 1 1 calc R . . . .
C59 C 0.4005(3) 0.9077(8) 0.74636(18) 0.057(2) Uani 1 1 d . . . . .
H59 H 0.381622 0.964028 0.755167 0.068 Uiso 1 1 calc R . . . .
C60 C 0.3774(3) 0.8171(8) 0.72399(18) 0.052(2) Uani 1 1 d . . . . .
C61 C 0.4052(3) 0.7373(7) 0.71117(15) 0.0426(16) Uani 1 1 d . . . . .
C62 C 0.4418(2) 0.5018(5) 0.66165(13) 0.0313(13) Uani 1 1 d . . . . .
C63 C 0.4013(2) 0.4344(6) 0.64338(14) 0.0351(14) Uani 1 1 d . . . . .
H63 H 0.369744 0.452385 0.645611 0.042 Uiso 1 1 calc R . . . .
C64 C 0.4068(2) 0.3413(6) 0.62194(14) 0.0342(14) Uani 1 1 d . . . . .
H64 H 0.379185 0.295935 0.609367 0.041 Uiso 1 1 calc R . . . .
C65 C 0.4529(2) 0.3156(5) 0.61915(13) 0.0275(12) Uani 1 1 d . . . . .
C66 C 0.4941(2) 0.3799(5) 0.63746(13) 0.0291(13) Uani 1 1 d . . . . .
H66 H 0.525683 0.359792 0.635623 0.035 Uiso 1 1 calc R . . . .
C67 C 0.4879(2) 0.4749(6) 0.65867(14) 0.0328(14) Uani 1 1 d . . . . .
H67 H 0.515451 0.520975 0.671044 0.039 Uiso 1 1 calc R . . . .
C68 C 0.4593(2) 0.2181(5) 0.59637(13) 0.0265(12) Uani 1 1 d . . . . .
C69 C 0.4851(2) 0.0482(5) 0.57636(14) 0.0257(12) Uani 1 1 d . . . . .
C70 C 0.5073(2) -0.0667(6) 0.57205(15) 0.0319(13) Uani 1 1 d . . . . .
C71 C 0.4938(2) -0.1124(6) 0.54067(15) 0.0347(14) Uani 1 1 d . . . . .
H71 H 0.508840 -0.187711 0.535925 0.042 Uiso 1 1 calc R . . . .
C72 C 0.4586(2) -0.0512(6) 0.51578(15) 0.0341(14) Uani 1 1 d . . . . .
H72 H 0.450463 -0.088117 0.494965 0.041 Uiso 1 1 calc R . . . .
C73 C 0.4353(2) 0.0603(5) 0.52011(14) 0.0280(12) Uani 1 1 d . . . . .
C74 C 0.4502(2) 0.1079(5) 0.55172(13) 0.0250(12) Uani 1 1 d . . . . .
C75 C 0.5397(2) -0.1383(6) 0.59886(15) 0.0317(13) Uani 1 1 d . . . . .
C76 C 0.5255(2) -0.1587(6) 0.62677(15) 0.0357(14) Uani 1 1 d . . . . .
H76 H 0.495973 -0.121826 0.628607 0.043 Uiso 1 1 calc R . . . .
C77 C 0.5535(3) -0.2313(7) 0.65177(17) 0.0414(16) Uani 1 1 d . . . . .
H77 H 0.543226 -0.244444 0.670519 0.050 Uiso 1 1 calc R . . . .
C78 C 0.5969(3) -0.2849(7) 0.64930(19) 0.0488(17) Uani 1 1 d . U . . .
C79 C 0.6118(3) -0.2634(8) 0.62165(18) 0.0509(19) Uani 1 1 d . . . . .
H79 H 0.641690 -0.298757 0.619957 0.061 Uiso 1 1 calc R . . . .
C80 C 0.5835(3) -0.1913(7) 0.59695(18) 0.0459(17) Uani 1 1 d . . . . .
H80 H 0.593952 -0.177578 0.578286 0.055 Uiso 1 1 calc R . . . .
C81 C 0.6245(3) -0.3657(9) 0.6758(2) 0.063(2) Uani 1 1 d . U . . .
C82 C 0.7003(5) -0.4705(14) 0.7010(3) 0.107(3) Uani 1 1 d . U . . .
H82A H 0.735190 -0.464157 0.701399 0.128 Uiso 1 1 calc R . . . .
H82B H 0.696963 -0.438897 0.721748 0.128 Uiso 1 1 calc R . . . .
C83 C 0.6848(6) -0.5965(19) 0.6963(4) 0.146(6) Uani 1 1 d . U . . .
H83A H 0.692612 -0.630814 0.677372 0.219 Uiso 1 1 calc GR . . . .
H83B H 0.649394 -0.600509 0.693153 0.219 Uiso 1 1 calc GR . . . .
H83C H 0.701514 -0.646993 0.715234 0.219 Uiso 1 1 calc GR . . . .
C84 C 0.3967(2) 0.1189(6) 0.49376(13) 0.0303(13) Uani 1 1 d . . . . .
C85 C 0.3931(3) 0.2491(6) 0.48899(15) 0.0366(15) Uani 1 1 d . . . . .
H85 H 0.415567 0.304490 0.503063 0.044 Uiso 1 1 calc R . . . .
C86 C 0.3561(3) 0.2991(7) 0.46334(15) 0.0403(16) Uani 1 1 d . . . . .
H86 H 0.353668 0.388352 0.459694 0.048 Uiso 1 1 calc R . . . .
C87 C 0.3230(3) 0.2168(7) 0.44331(15) 0.0416(16) Uani 1 1 d . . . . .
C88 C 0.3263(3) 0.0888(7) 0.44812(16) 0.0464(17) Uani 1 1 d . . . . .
H88 H 0.303507 0.033692 0.434158 0.056 Uiso 1 1 calc R . . . .
C89 C 0.3625(3) 0.0392(7) 0.47315(15) 0.0405(16) Uani 1 1 d . . . . .
H89 H 0.364375 -0.050215 0.476518 0.049 Uiso 1 1 calc R . . . .
C90 C 0.2827(3) 0.2656(9) 0.4149(2) 0.055(2) Uani 1 1 d . . . . .
C91 C 0.2531(4) 0.4345(10) 0.3806(2) 0.074(3) Uani 1 1 d . U . . .
H91A H 0.220642 0.432610 0.384668 0.089 Uiso 1 1 calc R . . . .
H91B H 0.251489 0.384800 0.360968 0.089 Uiso 1 1 calc R . . . .
C92 C 0.2683(5) 0.5661(13) 0.3772(3) 0.113(4) Uani 1 1 d . U . . .
H92A H 0.243743 0.607741 0.359653 0.170 Uiso 1 1 calc GR . . . .
H92B H 0.299906 0.565859 0.372378 0.170 Uiso 1 1 calc GR . . . .
H92C H 0.271335 0.612488 0.397233 0.170 Uiso 1 1 calc GR . . . .
F1 F -0.3000(4) 0.3031(12) 0.3860(3) 0.198(6) Uani 1 1 d . . . . .
F2 F -0.29937(18) 0.4384(6) 0.34816(13) 0.0839(17) Uani 1 1 d . . . . .
F3 F -0.2281(3) 0.3874(11) 0.3852(3) 0.174(5) Uani 1 1 d . . . . .
F4 F -0.2797(4) 0.5023(13) 0.3992(2) 0.180(5) Uani 1 1 d . . . . .
B1 B -0.2754(4) 0.3995(17) 0.3791(4) 0.093(5) Uani 1 1 d . . . . .
O5 O 0.1153(3) 0.0463(5) 0.45198(12) 0.0674(16) Uani 1 1 d . U . . .
O6 O 0.1750(2) 0.2529(8) 0.45328(13) 0.0726(17) Uani 1 1 d . U . . .
O7 O 0.1614(2) 0.4931(7) 0.41947(16) 0.0740(16) Uani 1 1 d . U . . .
O8 O 0.0850(2) 0.5221(6) 0.36135(15) 0.0673(15) Uani 1 1 d . U . . .
O9 O -0.0128(3) 0.4528(6) 0.33028(14) 0.0741(17) Uani 1 1 d . U . . .
O10 O -0.0803(3) 0.3466(10) 0.3592(2) 0.115(3) Uani 1 1 d . U . . .
O11 O -0.0581(4) 0.2562(10) 0.4266(3) 0.117(3) Uani 1 1 d . U . . .
O12 O 0.0142(3) 0.0731(6) 0.44064(16) 0.083(2) Uani 1 1 d . U . . .
C39 C 0.1646(5) 0.0346(11) 0.4493(2) 0.093(3) Uani 1 1 d . U . . .
H39A H 0.178488 -0.048248 0.458270 0.111 Uiso 1 1 calc R . . . .
H39B H 0.163829 0.036768 0.426355 0.111 Uiso 1 1 calc R . . . .
C40 C 0.1953(4) 0.1362(14) 0.4661(2) 0.096(3) Uani 1 1 d . U . . .
H40A H 0.197452 0.132353 0.489289 0.115 Uiso 1 1 calc R . . . .
H40B H 0.228701 0.127272 0.463779 0.115 Uiso 1 1 calc R . . . .
C41 C 0.2056(3) 0.3686(13) 0.4638(2) 0.086(3) Uani 1 1 d . U . . .
H41A H 0.233394 0.368709 0.454353 0.104 Uiso 1 1 calc R . . . .
H41B H 0.218825 0.368847 0.487474 0.104 Uiso 1 1 calc R . . . .
C42 C 0.1741(4) 0.4859(11) 0.4529(2) 0.081(3) Uani 1 1 d . U . . .
H42A H 0.144185 0.480590 0.460164 0.097 Uiso 1 1 calc R . . . .
H42B H 0.192419 0.563193 0.462382 0.097 Uiso 1 1 calc R . . . .
C43 C 0.1409(4) 0.6160(9) 0.4076(3) 0.074(2) Uani 1 1 d . U . . .
H43A H 0.115120 0.640512 0.417681 0.089 Uiso 1 1 calc R . . . .
H43B H 0.166718 0.682227 0.412549 0.089 Uiso 1 1 calc R . . . .
C44 C 0.1209(3) 0.6029(11) 0.3737(3) 0.093(3) Uani 1 1 d . U . . .
H44A H 0.109281 0.688213 0.365163 0.112 Uiso 1 1 calc R . . . .
H44B H 0.148233 0.580326 0.364832 0.112 Uiso 1 1 calc R . . . .
C45 C 0.0648(5) 0.5248(10) 0.3275(2) 0.087(3) Uani 1 1 d . U . . .
H45A H 0.090952 0.505585 0.317299 0.104 Uiso 1 1 calc R . . . .
H45B H 0.052748 0.611901 0.321000 0.104 Uiso 1 1 calc R . . . .
C46 C 0.0230(4) 0.4312(9) 0.3152(2) 0.078(2) Uani 1 1 d . U . . .
H46A H 0.009201 0.441486 0.291735 0.094 Uiso 1 1 calc R . . . .
H46B H 0.035410 0.343025 0.319480 0.094 Uiso 1 1 calc R . . . .
C47 C -0.0566(4) 0.4053(10) 0.3127(2) 0.087(3) Uani 1 1 d . U . . .
H47A H -0.052593 0.315580 0.306922 0.104 Uiso 1 1 calc R . . . .
H47B H -0.068686 0.454752 0.292620 0.104 Uiso 1 1 calc R . . . .
C48 C -0.0954(4) 0.4134(12) 0.3332(4) 0.105(3) Uani 1 1 d . U . . .
H48A H -0.099623 0.503231 0.338806 0.126 Uiso 1 1 calc R . . . .
H48B H -0.127512 0.380887 0.320266 0.126 Uiso 1 1 calc R . . . .
C49 C -0.1102(4) 0.3594(11) 0.3812(4) 0.111(4) Uani 1 1 d . U . . .
H49A H -0.145526 0.346782 0.370636 0.133 Uiso 1 1 calc R . . . .
H49B H -0.104772 0.440794 0.393193 0.133 Uiso 1 1 calc R . . . .
C50 C -0.0863(7) 0.2448(13) 0.4019(4) 0.145(6) Uani 1 1 d . U . . .
H50A H -0.113335 0.192572 0.405374 0.173 Uiso 1 1 calc R . . . .
H50B H -0.070511 0.193066 0.388585 0.173 Uiso 1 1 calc R . . . .
C51 C -0.0472(6) 0.1820(14) 0.4504(5) 0.135(5) Uani 1 1 d D U . . .
H51A H -0.077032 0.170249 0.457568 0.161 Uiso 1 1 calc R . . . .
H51B H -0.022907 0.226044 0.468016 0.161 Uiso 1 1 calc R . . . .
C52 C -0.0284(5) 0.0593(11) 0.4471(3) 0.105(4) Uani 1 1 d D U . . .
H52A H -0.023896 0.010226 0.467149 0.126 Uiso 1 1 calc R . . . .
H52B H -0.051592 0.012462 0.429431 0.126 Uiso 1 1 calc R . . . .
C53 C 0.0410(5) -0.0485(8) 0.4464(2) 0.093(3) Uani 1 1 d . U . . .
H53A H 0.049850 -0.068553 0.469585 0.111 Uiso 1 1 calc R . . . .
H53B H 0.019395 -0.117274 0.434777 0.111 Uiso 1 1 calc R . . . .
C54 C 0.0847(5) -0.0455(8) 0.4361(2) 0.090(3) Uani 1 1 d . U . . .
H54A H 0.101266 -0.129161 0.440169 0.108 Uiso 1 1 calc R . . . .
H54B H 0.076041 -0.028670 0.412713 0.108 Uiso 1 1 calc R . . . .
O17 O 0.5178(3) 0.0741(7) 0.67267(16) 0.096(2) Uani 1 1 d D U . . .
O18 O 0.4211(2) 0.0100(6) 0.63812(17) 0.0817(18) Uani 1 1 d D U . . .
O19 O 0.3431(3) 0.0562(8) 0.58241(17) 0.091(2) Uani 1 1 d D U . . .
O20 O 0.3383(2) 0.3038(7) 0.54866(14) 0.0773(18) Uani 1 1 d D U . . .
O21 O 0.4057(3) 0.4845(6) 0.54683(15) 0.091(2) Uani 1 1 d D U . . .
O22 O 0.5094(4) 0.4214(9) 0.5614(2) 0.131(3) Uani 1 1 d D U . . .
O23 O 0.5954(4) 0.2935(11) 0.5980(3) 0.202(6) Uani 1 1 d D U . . .
O24 O 0.5857(3) 0.1618(11) 0.6480(2) 0.164(5) Uani 1 1 d D U . . .
C93 C 0.4791(5) 0.0995(11) 0.6860(3) 0.106(3) Uani 1 1 d D U . . .
H93A H 0.466373 0.186723 0.680411 0.128 Uiso 1 1 calc R . . . .
H93B H 0.490319 0.091715 0.709677 0.128 Uiso 1 1 calc R . . . .
C94 C 0.4409(5) 0.0041(13) 0.6722(2) 0.105(3) Uani 1 1 d D U . . .
H94A H 0.454883 -0.081813 0.678014 0.125 Uiso 1 1 calc R . . . .
H94B H 0.413889 0.015131 0.682136 0.125 Uiso 1 1 calc R . . . .
C95 C 0.3848(4) -0.0819(10) 0.6253(3) 0.101(3) Uani 1 1 d D U . . .
H95A H 0.357870 -0.072729 0.635428 0.121 Uiso 1 1 calc R . . . .
H95B H 0.398930 -0.168147 0.630338 0.121 Uiso 1 1 calc R . . . .
C96 C 0.3650(4) -0.0672(11) 0.5897(3) 0.097(3) Uani 1 1 d D U . . .
H96A H 0.391713 -0.077125 0.579424 0.116 Uiso 1 1 calc R . . . .
H96B H 0.340208 -0.134001 0.581063 0.116 Uiso 1 1 calc R . . . .
C97 C 0.3204(4) 0.0770(12) 0.5495(2) 0.105(4) Uani 1 1 d D U . . .
H97A H 0.293139 0.015663 0.542275 0.126 Uiso 1 1 calc R . . . .
H97B H 0.344410 0.058513 0.537498 0.126 Uiso 1 1 calc R . . . .
C98 C 0.3008(3) 0.2079(11) 0.5410(3) 0.103(3) Uani 1 1 d D U . . .
H98A H 0.283950 0.211240 0.517766 0.124 Uiso 1 1 calc R . . . .
H98B H 0.276360 0.226724 0.552708 0.124 Uiso 1 1 calc R . . . .
C99 C 0.3226(4) 0.4222(11) 0.5368(2) 0.103(3) Uani 1 1 d D U . . .
H99A H 0.291356 0.442455 0.541392 0.124 Uiso 1 1 calc R . . . .
H99B H 0.316767 0.422400 0.513170 0.124 Uiso 1 1 calc R . . . .
C100 C 0.3594(4) 0.5198(9) 0.5513(2) 0.103(3) Uani 1 1 d D U . . .
H10A H 0.349039 0.603426 0.541141 0.124 Uiso 1 1 calc R . . . .
H10B H 0.362408 0.527306 0.574520 0.124 Uiso 1 1 calc R . . . .
C101 C 0.4459(5) 0.5688(9) 0.5618(3) 0.120(4) Uani 1 1 d D U . . .
H10C H 0.454540 0.557671 0.585387 0.143 Uiso 1 1 calc R . . . .
H10D H 0.435248 0.658102 0.556911 0.143 Uiso 1 1 calc R . . . .
C102 C 0.4904(6) 0.5442(11) 0.5505(5) 0.167(7) Uani 1 1 d D U . . .
H10E H 0.481516 0.547707 0.526818 0.200 Uiso 1 1 calc R . . . .
H10F H 0.515462 0.610061 0.559202 0.200 Uiso 1 1 calc R . . . .
C103 C 0.5554(7) 0.4281(17) 0.5541(6) 0.225(10) Uani 1 1 d D U . . .
H10G H 0.578887 0.488809 0.567655 0.270 Uiso 1 1 calc R . . . .
H10H H 0.552438 0.440896 0.531064 0.270 Uiso 1 1 calc R . . . .
C104 C 0.5633(6) 0.2937(14) 0.5648(4) 0.188(7) Uani 1 1 d D U . . .
H10I H 0.531684 0.252701 0.563989 0.226 Uiso 1 1 calc R . . . .
H10J H 0.578840 0.245745 0.550675 0.226 Uiso 1 1 calc R . . . .
C105 C 0.6130(5) 0.1688(15) 0.6043(4) 0.201(7) Uani 1 1 d D U . . .
H10K H 0.639824 0.153608 0.594368 0.242 Uiso 1 1 calc R . . . .
H10L H 0.586440 0.107133 0.595133 0.242 Uiso 1 1 calc R . . . .
C106 C 0.6306(4) 0.1532(15) 0.6386(3) 0.216(7) Uani 1 1 d D U . . .
H10M H 0.653792 0.221666 0.648627 0.259 Uiso 1 1 calc R . . . .
H10N H 0.646651 0.069556 0.644448 0.259 Uiso 1 1 calc R . . . .
C107 C 0.6010(5) 0.1031(15) 0.6794(3) 0.178(6) Uani 1 1 d D U . . .
H10O H 0.631941 0.140560 0.692669 0.214 Uiso 1 1 calc R . . . .
H10P H 0.605257 0.010079 0.677685 0.214 Uiso 1 1 calc R . . . .
C108 C 0.5597(5) 0.1323(12) 0.6929(3) 0.133(4) Uani 1 1 d D U . . .
H10Q H 0.566532 0.098178 0.715016 0.160 Uiso 1 1 calc R . . . .
H10R H 0.554939 0.225457 0.693649 0.160 Uiso 1 1 calc R . . . .
O25 O 0.2056(2) 0.0241(7) 0.32981(15) 0.0686(17) Uani 1 1 d . . . . .
C111 C 0.2430(3) -0.0430(12) 0.3520(3) 0.097(4) Uani 1 1 d . . . . .
H11A H 0.269275 0.016551 0.363088 0.116 Uiso 1 1 calc R . . . .
H11B H 0.257232 -0.107578 0.340704 0.116 Uiso 1 1 calc R . . . .
C112 C 0.2220(5) -0.1067(13) 0.3761(3) 0.110(4) Uani 1 1 d . . . . .
H11C H 0.195338 -0.163492 0.364945 0.164 Uiso 1 1 calc GR . . . .
H11D H 0.209336 -0.041948 0.387926 0.164 Uiso 1 1 calc GR . . . .
H11E H 0.247584 -0.156168 0.391124 0.164 Uiso 1 1 calc GR . . . .
C113 C 0.2242(5) 0.1115(18) 0.3092(4) 0.135(6) Uani 1 1 d D U . . .
H11H H 0.228364 0.067116 0.290071 0.162 Uiso 0.4 1 calc R . P A 2
H11I H 0.255710 0.150211 0.321220 0.162 Uiso 0.4 1 calc R . P A 2
H11F H 0.245128 0.065120 0.298276 0.162 Uiso 0.6 1 calc R . P B 1
H11G H 0.243561 0.180998 0.322206 0.162 Uiso 0.6 1 calc R . P B 1
C1A C 0.1789(9) 0.165(3) 0.2848(7) 0.146(9) Uani 0.6 1 d D U P C 1
H1AA H 0.160800 0.095163 0.271697 0.219 Uiso 0.6 1 calc GR . P C 1
H1AB H 0.189012 0.226325 0.270911 0.219 Uiso 0.6 1 calc GR . P C 1
H1AC H 0.157950 0.207214 0.296077 0.219 Uiso 0.6 1 calc GR . P C 1
C114 C 0.1838(14) 0.211(4) 0.3000(11) 0.146(11) Uani 0.4 1 d D U P C 2
H11J H 0.152713 0.169232 0.289239 0.219 Uiso 0.4 1 calc GR . P C 2
H11K H 0.191749 0.273414 0.285529 0.219 Uiso 0.4 1 calc GR . P C 2
H11L H 0.180807 0.254055 0.319415 0.219 Uiso 0.4 1 calc GR . P C 2
N9 N 0.1382(4) 0.7962(10) 0.5090(3) 0.107(3) Uani 1 1 d . . . . .
C109 C 0.1772(4) 0.7694(9) 0.5214(2) 0.063(2) Uani 1 1 d . . . . .
C110 C 0.2242(4) 0.7374(17) 0.5382(4) 0.128(6) Uani 1 1 d . . . . .
H11M H 0.234620 0.662775 0.528326 0.192 Uiso 1 1 calc GR . . . .
H11N H 0.225385 0.717724 0.560504 0.192 Uiso 1 1 calc GR . . . .
H11O H 0.246097 0.808984 0.537851 0.192 Uiso 1 1 calc GR . . . .
B2 B 0.3000(5) 0.7290(13) 0.4718(3) 0.088(3) Uani 1 1 d D U . . .
F5A F 0.3201(7) 0.7809(13) 0.4995(3) 0.108(4) Uani 0.6 1 d . U P D 1
F6A F 0.3133(6) 0.7763(18) 0.4472(3) 0.084(4) Uani 0.6 1 d . . P D 1
F7A F 0.2474(6) 0.7830(15) 0.4603(5) 0.140(5) Uani 0.6 1 d . U P D 1
F8A F 0.2946(8) 0.6024(16) 0.4687(6) 0.119(7) Uani 0.6 1 d . U P D 1
F5B F 0.3528(5) 0.7277(19) 0.4874(5) 0.121(7) Uani 0.4 1 d D U P D 2
F6B F 0.2939(10) 0.765(3) 0.4420(5) 0.135(12) Uani 0.4 1 d D U P D 2
F7B F 0.2829(12) 0.833(2) 0.4889(8) 0.188(12) Uani 0.4 1 d D U P D 2
F8B F 0.2813(9) 0.620(2) 0.4786(9) 0.127(12) Uani 0.4 1 d D U P D 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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 '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'
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
C27 O2 C28 105.5(11) . . ?
C36 O4 C37 114.5(7) . . ?
C1 N1 C2 105.7(5) . . ?
C1 N2 C7 104.9(5) . . ?
C14 N3 C20 108.6(4) . . ?
C14 N4 C15 108.5(5) . . ?
N1 C1 C8 124.2(5) . . ?
N2 C1 N1 113.7(5) . . ?
N2 C1 C8 122.1(5) . . ?
N1 C2 C3 134.1(7) . . ?
N1 C2 C7 106.1(5) . . ?
C3 C2 C7 119.8(6) . . ?
C2 C3 Br1 119.1(6) . . ?
C4 C3 Br1 121.7(6) . . ?
C4 C3 C2 119.1(7) . . ?
C3 C4 C5 121.6(7) . . ?
C6 C5 C4 119.7(6) . . ?
C5 C6 Br2 121.2(5) . . ?
C5 C6 C7 119.5(6) . . ?
C7 C6 Br2 119.3(5) . . ?
N2 C7 C2 109.5(5) . . ?
N2 C7 C6 129.9(6) . . ?
C6 C7 C2 120.5(6) . . ?
C9 C8 C1 118.0(5) . . ?
C9 C8 C13 119.1(5) . . ?
C13 C8 C1 122.9(5) . . ?
C8 C9 C10 121.2(5) . . ?
C9 C10 C11 118.9(5) . . ?
C10 C11 C12 121.1(5) . . ?
C10 C11 C14 118.6(5) . . ?
C12 C11 C14 120.3(5) . . ?
C13 C12 C11 118.8(5) . . ?
C12 C13 C8 120.9(5) . . ?
N3 C14 C11 124.8(5) . . ?
N4 C14 N3 110.2(5) . . ?
N4 C14 C11 125.0(5) . . ?
N4 C15 C16 130.7(5) . . ?
N4 C15 C20 106.2(5) . . ?
C20 C15 C16 123.1(5) . . ?
C15 C16 C21 122.1(5) . . ?
C17 C16 C15 114.0(5) . . ?
C17 C16 C21 123.8(5) . . ?
C16 C17 C18 122.8(5) . . ?
C19 C18 C17 122.8(5) . . ?
C18 C19 C20 114.8(5) . . ?
C18 C19 C30 123.6(5) . . ?
C20 C19 C30 121.6(5) . . ?
N3 C20 C15 106.5(5) . . ?
N3 C20 C19 131.1(5) . . ?
C15 C20 C19 122.3(5) . . ?
C22 C21 C16 120.1(5) . . ?
C22 C21 C26 118.7(6) . . ?
C26 C21 C16 121.2(6) . . ?
C21 C22 C23 120.4(6) . . ?
C24 C23 C22 120.6(7) . . ?
C23 C24 C25 119.7(7) . . ?
C23 C24 C27 118.9(9) . . ?
C25 C24 C27 121.4(9) . . ?
C24 C25 C26 120.4(7) . . ?
C21 C26 C25 120.1(7) . . ?
O1 C27 O2 124.8(10) . . ?
O1 C27 C24 118.5(11) . . ?
O2 C27 C24 116.7(11) . . ?
O2 C28 C29 97.4(13) . . ?
C31 C30 C19 120.8(5) . . ?
C35 C30 C19 121.5(5) . . ?
C35 C30 C31 117.7(5) . . ?
C32 C31 C30 121.4(6) . . ?
C31 C32 C33 119.9(6) . . ?
C32 C33 C34 119.5(6) . . ?
C32 C33 C36 117.9(6) . . ?
C34 C33 C36 122.6(6) . . ?
C35 C34 C33 120.4(6) . . ?
C34 C35 C30 121.1(6) . . ?
O3 C36 O4 124.3(7) . . ?
O3 C36 C33 123.6(7) . . ?
O4 C36 C33 112.1(6) . . ?
C38 C37 O4 96.0(13) . . ?
C81 O14 C82 116.3(7) . . ?
C90 O16 C91 113.4(8) . . ?
C55 N5 C61 106.6(6) . . ?
C55 N6 C56 105.2(5) . . ?
C68 N7 C69 109.1(5) . . ?
C68 N8 C74 108.3(5) . . ?
N5 C55 C62 123.7(6) . . ?
N6 C55 N5 113.3(5) . . ?
N6 C55 C62 123.0(6) . . ?
N6 C56 C57 130.9(6) . . ?
N6 C56 C61 109.9(6) . . ?
C57 C56 C61 119.1(6) . . ?
C56 C57 Br3 119.2(5) . . ?
C58 C57 Br3 121.3(5) . . ?
C58 C57 C56 119.5(6) . . ?
C59 C58 C57 120.8(7) . . ?
C58 C59 C60 120.3(7) . . ?
C59 C60 Br4 121.0(6) . . ?
C61 C60 Br4 119.7(6) . . ?
C61 C60 C59 119.2(7) . . ?
N5 C61 C56 105.0(6) . . ?
C60 C61 N5 134.0(7) . . ?
C60 C61 C56 121.0(6) . . ?
C63 C62 C55 122.1(6) . . ?
C67 C62 C55 118.0(6) . . ?
C67 C62 C63 119.8(5) . . ?
C64 C63 C62 120.5(6) . . ?
C65 C64 C63 119.1(6) . . ?
C64 C65 C66 121.6(5) . . ?
C64 C65 C68 119.8(5) . . ?
C66 C65 C68 118.6(5) . . ?
C65 C66 C67 118.6(6) . . ?
C62 C67 C66 120.3(6) . . ?
N7 C68 N8 109.8(5) . . ?
N7 C68 C65 125.3(5) . . ?
N8 C68 C65 124.9(5) . . ?
N7 C69 C70 130.8(6) . . ?
N7 C69 C74 106.6(5) . . ?
C74 C69 C70 122.6(5) . . ?
C69 C70 C75 122.7(5) . . ?
C71 C70 C69 114.7(6) . . ?
C71 C70 C75 122.5(5) . . ?
C70 C71 C72 122.4(6) . . ?
C73 C72 C71 123.2(6) . . ?
C72 C73 C74 114.1(5) . . ?
C72 C73 C84 121.8(5) . . ?
C74 C73 C84 124.0(5) . . ?
N8 C74 C73 130.8(5) . . ?
C69 C74 N8 106.1(5) . . ?
C69 C74 C73 123.0(5) . . ?
C76 C75 C70 119.7(5) . . ?
C80 C75 C70 122.1(6) . . ?
C80 C75 C76 118.2(6) . . ?
C77 C76 C75 121.5(6) . . ?
C76 C77 C78 119.5(6) . . ?
C77 C78 C79 119.4(7) . . ?
C77 C78 C81 117.7(6) . . ?
C79 C78 C81 122.8(7) . . ?
C80 C79 C78 120.3(7) . . ?
C79 C80 C75 121.0(6) . . ?
O13 C81 O14 122.7(7) . . ?
O13 C81 C78 123.7(7) . . ?
O14 C81 C78 113.5(7) . . ?
C83 C82 O14 108.4(14) . . ?
C85 C84 C73 122.3(6) . . ?
C85 C84 C89 119.1(6) . . ?
C89 C84 C73 118.5(6) . . ?
C84 C85 C86 119.8(6) . . ?
C87 C86 C85 119.3(6) . . ?
C86 C87 C90 121.6(7) . . ?
C88 C87 C86 121.0(7) . . ?
C88 C87 C90 117.5(7) . . ?
C87 C88 C89 120.0(7) . . ?
C88 C89 C84 120.8(7) . . ?
O15 C90 O16 125.4(8) . . ?
O15 C90 C87 123.6(8) . . ?
O16 C90 C87 111.0(8) . . ?
O16 C91 C92 105.2(9) . . ?
F1 B1 F2 107.5(11) . . ?
F1 B1 F4 107.5(14) . . ?
F2 B1 F4 105.6(12) . . ?
F3 B1 F1 117.7(14) . . ?
F3 B1 F2 115.2(12) . . ?
F3 B1 F4 102.3(12) . . ?
C54 O5 C39 113.5(8) . . ?
C40 O6 C41 116.8(8) . . ?
C42 O7 C43 112.2(8) . . ?
C44 O8 C45 116.7(9) . . ?
C47 O9 C46 111.0(8) . . ?
C48 O10 C49 114.1(10) . . ?
C50 O11 C51 130.1(16) . . ?
C52 O12 C53 109.4(8) . . ?
C40 C39 O5 111.1(7) . . ?
O6 C40 C39 108.8(8) . . ?
O6 C41 C42 108.9(7) . . ?
O7 C42 C41 109.0(8) . . ?
C44 C43 O7 106.5(8) . . ?
O8 C44 C43 121.3(12) . . ?
O8 C45 C46 113.6(8) . . ?
O9 C46 C45 109.7(8) . . ?
O9 C47 C48 109.6(8) . . ?
O10 C48 C47 110.0(9) . . ?
O10 C49 C50 93.8(10) . . ?
O11 C50 C49 122.6(13) . . ?
O11 C51 C52 119.3(15) . . ?
O12 C52 C51 108.5(10) . . ?
C54 C53 O12 112.4(7) . . ?
O5 C54 C53 110.3(8) . . ?
C93 O17 C108 106.6(10) . . ?
C95 O18 C94 114.2(9) . . ?
C97 O19 C96 114.2(9) . . ?
C99 O20 C98 114.0(8) . . ?
C100 O21 C101 114.9(8) . . ?
C102 O22 C103 99.6(10) . . ?
C105 O23 C104 106.2(8) . . ?
C106 O24 C107 100.5(8) . . ?
O17 C93 C94 106.1(9) . . ?
O18 C94 C93 115.0(10) . . ?
O18 C95 C96 111.0(8) . . ?
O19 C96 C95 109.5(9) . . ?
O19 C97 C98 115.3(10) . . ?
O20 C98 C97 112.8(8) . . ?
O20 C99 C100 110.6(8) . . ?
O21 C100 C99 109.3(8) . . ?
O21 C101 C102 112.3(10) . . ?
O22 C102 C101 108.9(11) . . ?
O22 C103 C104 87.3(11) . . ?
O23 C104 C103 107.8(14) . . ?
O23 C105 C106 107.9(10) . . ?
C105 C106 O24 101.8(11) . . ?
O24 C107 C108 103.0(10) . . ?
O17 C108 C107 106.8(10) . . ?
C111 O25 C113 113.2(9) . . ?
O25 C111 C112 109.1(8) . . ?
O25 C113 C1A 105.8(15) . . ?
O25 C113 C114 102(2) . . ?
N9 C109 C110 176.8(13) . . ?
F5A B2 F6A 115.8(12) . . ?
F5A B2 F7A 106.3(15) . . ?
F5A B2 F8A 121.1(17) . . ?
F6A B2 F7A 94.3(13) . . ?
F6A B2 F8A 110.0(17) . . ?
F8A B2 F7A 105.0(14) . . ?
F5B B2 F7B 102.3(15) . . ?
F6B B2 F5B 107.1(15) . . ?
F6B B2 F7B 108.0(17) . . ?
F6B B2 F8B 121.3(19) . . ?
F8B B2 F5B 108.2(15) . . ?
F8B B2 F7B 108.4(16) . . ?
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
Br1 C3 1.899(8) . ?
Br2 C6 1.889(7) . ?
O1 C27 1.215(16) . ?
O2 C27 1.240(14) . ?
O2 C28 1.522(15) . ?
O3 C36 1.183(9) . ?
O4 C36 1.335(9) . ?
O4 C37 1.534(13) . ?
N1 C1 1.360(8) . ?
N1 C2 1.386(8) . ?
N2 C1 1.318(8) . ?
N2 C7 1.382(8) . ?
N3 C14 1.326(7) . ?
N3 C20 1.378(7) . ?
N4 C14 1.321(7) . ?
N4 C15 1.388(7) . ?
C1 C8 1.461(8) . ?
C2 C3 1.390(9) . ?
C2 C7 1.394(10) . ?
C3 C4 1.361(11) . ?
C4 C5 1.395(11) . ?
C5 C6 1.371(9) . ?
C6 C7 1.385(9) . ?
C8 C9 1.385(8) . ?
C8 C13 1.397(8) . ?
C9 C10 1.385(8) . ?
C10 C11 1.391(8) . ?
C11 C12 1.395(8) . ?
C11 C14 1.465(7) . ?
C12 C13 1.386(8) . ?
C15 C16 1.408(8) . ?
C15 C20 1.390(8) . ?
C16 C17 1.397(8) . ?
C16 C21 1.482(8) . ?
C17 C18 1.401(9) . ?
C18 C19 1.387(8) . ?
C19 C20 1.406(8) . ?
C19 C30 1.472(8) . ?
C21 C22 1.386(9) . ?
C21 C26 1.391(9) . ?
C22 C23 1.395(9) . ?
C23 C24 1.362(11) . ?
C24 C25 1.379(12) . ?
C24 C27 1.514(11) . ?
C25 C26 1.392(10) . ?
C28 C29 1.74(3) . ?
C30 C31 1.407(8) . ?
C30 C35 1.388(9) . ?
C31 C32 1.372(9) . ?
C32 C33 1.386(9) . ?
C33 C34 1.391(9) . ?
C33 C36 1.500(9) . ?
C34 C35 1.375(9) . ?
C37 C38 1.426(15) . ?
Br3 C57 1.884(7) . ?
Br4 C60 1.895(8) . ?
O13 C81 1.201(9) . ?
O14 C81 1.344(10) . ?
O14 C82 1.475(12) . ?
O15 C90 1.211(11) . ?
O16 C90 1.302(11) . ?
O16 C91 1.468(10) . ?
N5 C55 1.355(8) . ?
N5 C61 1.385(8) . ?
N6 C55 1.316(8) . ?
N6 C56 1.373(8) . ?
N7 C68 1.321(7) . ?
N7 C69 1.381(7) . ?
N8 C68 1.332(7) . ?
N8 C74 1.394(7) . ?
C55 C62 1.470(8) . ?
C56 C57 1.390(9) . ?
C56 C61 1.407(10) . ?
C57 C58 1.383(10) . ?
C58 C59 1.379(12) . ?
C59 C60 1.387(11) . ?
C60 C61 1.373(10) . ?
C62 C63 1.395(9) . ?
C62 C67 1.384(9) . ?
C63 C64 1.390(8) . ?
C64 C65 1.379(9) . ?
C65 C66 1.392(9) . ?
C65 C68 1.470(8) . ?
C66 C67 1.402(8) . ?
C69 C70 1.399(8) . ?
C69 C74 1.388(8) . ?
C70 C71 1.393(9) . ?
C70 C75 1.472(9) . ?
C71 C72 1.405(9) . ?
C72 C73 1.385(8) . ?
C73 C74 1.409(8) . ?
C73 C84 1.481(8) . ?
C75 C76 1.397(9) . ?
C75 C80 1.391(9) . ?
C76 C77 1.382(9) . ?
C77 C78 1.389(10) . ?
C78 C79 1.400(10) . ?
C78 C81 1.468(10) . ?
C79 C80 1.374(10) . ?
C82 C83 1.39(2) . ?
C84 C85 1.383(9) . ?
C84 C89 1.399(9) . ?
C85 C86 1.402(10) . ?
C86 C87 1.389(10) . ?
C87 C88 1.360(11) . ?
C87 C90 1.520(11) . ?
C88 C89 1.373(10) . ?
C91 C92 1.468(17) . ?
F1 B1 1.315(16) . ?
F2 B1 1.385(14) . ?
F3 B1 1.303(14) . ?
F4 B1 1.42(2) . ?
O5 C39 1.447(13) . ?
O5 C54 1.352(13) . ?
O6 C40 1.403(13) . ?
O6 C41 1.490(13) . ?
O7 C42 1.396(11) . ?
O7 C43 1.451(11) . ?
O8 C44 1.320(12) . ?
O8 C45 1.418(11) . ?
O9 C46 1.377(12) . ?
O9 C47 1.361(12) . ?
O10 C48 1.296(16) . ?
O10 C49 1.454(15) . ?
O11 C50 1.151(16) . ?
O11 C51 1.263(17) . ?
O12 C52 1.327(13) . ?
O12 C53 1.474(14) . ?
C39 C40 1.442(18) . ?
C41 C42 1.519(16) . ?
C43 C44 1.429(15) . ?
C45 C46 1.520(16) . ?
C47 C48 1.605(18) . ?
C49 C50 1.54(2) . ?
C51 C52 1.419(14) . ?
C53 C54 1.436(17) . ?
O17 C93 1.407(9) . ?
O17 C108 1.409(12) . ?
O18 C94 1.428(8) . ?
O18 C95 1.410(8) . ?
O19 C96 1.435(14) . ?
O19 C97 1.408(8) . ?
O20 C98 1.437(8) . ?
O20 C99 1.372(12) . ?
O21 C100 1.435(8) . ?
O21 C101 1.448(9) . ?
O22 C102 1.427(9) . ?
O22 C103 1.434(9) . ?
O23 C104 1.474(9) . ?
O23 C105 1.401(15) . ?
O24 C106 1.4477(14) . ?
O24 C107 1.4476(12) . ?
C93 C94 1.477(18) . ?
C95 C96 1.500(8) . ?
C97 C98 1.490(9) . ?
C99 C100 1.476(7) . ?
C101 C102 1.504(9) . ?
C103 C104 1.484(10) . ?
C105 C106 1.444(9) . ?
C107 C108 1.486(9) . ?
O25 C111 1.408(13) . ?
O25 C113 1.479(15) . ?
C111 C112 1.499(17) . ?
C113 C1A 1.527(18) . ?
C113 C114 1.52(2) . ?
N9 C109 1.126(13) . ?
C109 C110 1.374(16) . ?
B2 F5A 1.298(17) . ?
B2 F6A 1.327(19) . ?
B2 F7A 1.55(2) . ?
B2 F8A 1.34(2) . ?
B2 F5B 1.467(15) . ?
B2 F6B 1.31(2) . ?
B2 F7B 1.48(2) . ?
B2 F8B 1.33(2) . ?
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 0.257 0.106 0.220 222.0 45.7 ?
2 0.257 0.394 0.720 222.0 45.8 ?
3 0.174 -0.001 0.811 12.7 0.0 ?
4 0.174 0.501 0.311 12.7 0.0 ?
5 0.743 0.606 0.280 222.0 45.8 ?
6 0.743 0.894 0.780 222.0 45.9 ?
7 0.826 0.001 0.189 12.7 0.4 ?
8 0.826 0.499 0.689 12.7 0.4 ?
