#------------------------------------------------------------------------------
#$Date: 2024-12-06 17:10:42 +0200 (Fri, 06 Dec 2024) $
#$Revision: 296280 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/38/7133812.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_7133812
loop_
_publ_author_name
'Qiu, Xujun'
'Pohl, Eric'
'Jung, André'
'Cai, Qianyu'
'Su, Haopu'
'Fuhr, Olaf'
'Schepers, Ute'
'Bräse, Stefan'
_publ_section_title
;
 Modulating the photolysis of aryl azides in a supramolecular host to
 develop photoactivatable fluorophores.
;
_journal_issue                   88
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12856
_journal_page_last               12859
_journal_paper_doi               10.1039/d4cc03907f
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'Cl, 2.5(H2 O), C24 H20 N5'
_chemical_formula_sum            'C24 H25 Cl N5 O2.5'
_chemical_formula_weight         458.94
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-23
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-25 deposited with the CCDC.	2024-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                101.497(2)
_cell_angle_beta                 93.876(2)
_cell_angle_gamma                103.476(2)
_cell_formula_units_Z            4
_cell_length_a                   9.5693(2)
_cell_length_b                   10.1473(2)
_cell_length_c                   24.8566(6)
_cell_measurement_reflns_used    35790
_cell_measurement_temperature    180
_cell_measurement_theta_max      64.52
_cell_measurement_theta_min      3.18
_cell_volume                     2283.56(9)
_computing_cell_refinement
;
X-Area Recipe 2.0.1 (STOE, 2023)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.192.0 (STOE, 2023)
;
_computing_data_reduction
;
X-Area Integrate 2.5.15.0 (STOE, 2023)
X-Area LANA 2.7.12 (STOE, 2023)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.3, Darmstadt 2023
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      180
_diffrn_detector                 'Eiger R 4M'
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            DECTRIS
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
 2047 frames, detector distance = 80 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ga K\a'
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            37773
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         62.499
_diffrn_reflns_theta_min         3.180
_diffrn_source                   'Metal Jet D2+'
_diffrn_source_current           3.57
_diffrn_source_power             0.250
_diffrn_source_target            Ga
_diffrn_source_type              'Metal Jet D2+'
_diffrn_source_voltage           70
_exptl_absorpt_coefficient_mu    1.153
_exptl_absorpt_correction_T_max  0.9678
_exptl_absorpt_correction_T_min  0.8774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         10827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          1.490
_refine_ls_shift/su_mean         0.041
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1465P)²+1.0542P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2164
_refine_ls_wR_factor_ref         0.2283
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8429
_reflns_number_total             10827
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc03907f2.cif
_cod_data_source_block           xqr271s-2
_cod_depositor_comments
'Adding full bibliography for 7133811--7133812.cif.'
_cod_original_formula_sum        'C24 H25 Cl N5 O2.50'
_cod_database_code               7133812
_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   0.966
_shelx_estimated_absorpt_t_min   0.874
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O1(H1A,H1B), O2(H2A,H2B), O3(H3A,H3B), O4(H4A,H4B), O5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
  C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C41(H41), C42(H42), C45(H45),
  C46(H46), C47(H47)
2.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C48(H48A,H48B,H48C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '80.0 mm'
_stoe_detector_pixelsize_x       '0.075 mm'
_stoe_detector_pixelsize_y       '0.075 mm'
_stoe_detector_size_x            '15.5 cm'
_stoe_detector_size_y            '16.2 cm'
_stoe_evaluation_integration_a   18.0
_stoe_evaluation_integration_b   0.4
_stoe_evaluation_integration_ems 0.014
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 97.8
_stoe_evaluation_lana_dxs_max_order -
_stoe_evaluation_lana_dys_max_order -
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 128.2
_stoe_evaluation_lana_max_2theta_desired 125.0
_stoe_evaluation_lana_mean_redundancy 3.5
_stoe_evaluation_lana_number_refls_after_or 37777
_stoe_evaluation_lana_number_refls_outliers 6932
_stoe_evaluation_lana_number_refls_total 44709
_stoe_evaluation_lana_number_refls_unique 10830
_stoe_evaluation_lana_number_refls_written 37777
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group -1
_stoe_evaluation_lana_table
;
#----------------------------------------------------------------------------
2Theta          12.0   25.4   38.8   52.2   65.6   79.0   92.4  105.8  119.2
#----------------------------------------------------------------------------
<Resolution>    5.55   2.91   1.94   1.51   1.24   1.06   0.93   0.84   0.78
N(total)          92    380   1607   6113   8138   7794   8323   7405   4857
<Redundancy>     1.4    1.5    2.3    4.9    4.7    3.8    3.7    3.2    2.4
Complet. [%%]    86.6   92.7   98.5  100.0   99.9   97.2   99.2   99.2   93.6
<I/sigma>      219.3  216.0   78.7   39.5   26.3   15.3    7.9    5.1    4.6
R(int)         0.013  0.019  0.019  0.021  0.022  0.030  0.048  0.070  0.078
#----------------------------------------------------------------------------
;
_stoe_measurement_identifier     XQR271S-2
_stoe_measurement_max_exposure_per_frame '1.0 s'
_stoe_measurement_mean_exposure_per_frame '1.0 s'
_stoe_measurement_min_exposure_per_frame '1.0 s'
_stoe_measurement_total_exposure_time '34 min'
_stoe_measurement_total_frame_number 2047
_stoe_measurement_total_run_number 24
_stoe_measurement_tube_power     '250 W'
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 0.74405(9) 0.75203(8) 0.53064(3) 0.0558(2) Uani 1 1 d . . . . .
Cl2 Cl -0.07214(9) 0.23353(12) 0.66749(5) 0.0767(3) Uani 1 1 d . . . . .
O1 O -0.2270(4) 0.2575(5) 0.55506(16) 0.1120(13) Uani 1 1 d G . . . .
H1A H -0.186343 0.201349 0.535969 0.168 Uiso 1 1 d G U . . .
H1B H -0.182332 0.275867 0.587510 0.168 Uiso 1 1 d G U . . .
O2 O 0.0524(5) 1.3046(7) 0.7901(3) 0.153(2) Uani 1 1 d G . . . .
H2A H 0.017350 1.215677 0.786568 0.229 Uiso 1 1 d G U . . .
H2B H 0.140508 1.320188 0.781609 0.229 Uiso 1 1 d G U . . .
O3 O 0.0247(3) 0.6473(4) 0.51024(15) 0.0881(9) Uani 1 1 d G . . . .
H3A H 0.004473 0.561871 0.511481 0.132 Uiso 1 1 d G U . . .
H3B H 0.053589 0.656366 0.479267 0.132 Uiso 1 1 d G U . . .
O4 O 0.5125(3) 0.8730(4) 0.47195(15) 0.0877(9) Uani 1 1 d G . . . .
H4A H 0.430893 0.816689 0.459229 0.131 Uiso 1 1 d G U . . .
H4B H 0.567258 0.830814 0.486068 0.131 Uiso 1 1 d G U . . .
O5 O 0.6989(4) 0.9330(4) 0.64306(14) 0.0934(10) Uani 1 1 d G . . . .
H5A H 0.698240 0.886007 0.610578 0.140 Uiso 1 1 d G U . . .
H5B H 0.758147 1.010594 0.644394 0.140 Uiso 1 1 d G U . . .
N1 N 0.52638(18) 1.12987(19) 0.84892(7) 0.0273(4) Uani 1 1 d . . . . .
N2 N 0.3826(2) 1.5209(2) 0.58651(8) 0.0370(4) Uani 1 1 d . . . . .
N3 N 0.6910(2) 1.4664(3) 0.66667(10) 0.0452(5) Uani 1 1 d . . . . .
N4 N 0.7918(3) 1.5282(3) 0.64496(10) 0.0523(6) Uani 1 1 d . . . . .
N5 N 0.8959(3) 1.5793(4) 0.63001(15) 0.0764(10) Uani 1 1 d . . . . .
C1 C 0.4149(2) 1.0774(2) 0.87982(8) 0.0241(4) Uani 1 1 d . . . . .
C2 C 0.4387(2) 1.1081(2) 0.93766(9) 0.0276(4) Uani 1 1 d . . . . .
H2 H 0.529054 1.165132 0.956318 0.033 Uiso 1 1 calc R U . . .
C3 C 0.3302(2) 1.0552(2) 0.96780(9) 0.0306(4) Uani 1 1 d . . . . .
H3 H 0.347494 1.075008 1.007016 0.037 Uiso 1 1 calc R U . . .
C4 C 0.1974(2) 0.9741(2) 0.94130(10) 0.0326(5) Uani 1 1 d . . . . .
H4 H 0.122990 0.939621 0.962092 0.039 Uiso 1 1 calc R U . . .
C5 C 0.1740(2) 0.9433(2) 0.88374(10) 0.0317(4) Uani 1 1 d . . . . .
H5 H 0.082733 0.888176 0.865262 0.038 Uiso 1 1 calc R U . . .
C6 C 0.2827(2) 0.9925(2) 0.85313(9) 0.0277(4) Uani 1 1 d . . . . .
H6 H 0.266800 0.968123 0.813875 0.033 Uiso 1 1 calc R U . . .
C7 C 0.6721(2) 1.1470(2) 0.87184(8) 0.0254(4) Uani 1 1 d . . . . .
C8 C 0.7730(2) 1.2740(2) 0.87991(10) 0.0304(4) Uani 1 1 d . . . . .
H8 H 0.746220 1.350381 0.869184 0.036 Uiso 1 1 calc R U . . .
C9 C 0.9134(2) 1.2897(2) 0.90369(11) 0.0356(5) Uani 1 1 d . . . . .
H9 H 0.982398 1.376665 0.909087 0.043 Uiso 1 1 calc R U . . .
C10 C 0.9530(2) 1.1788(2) 0.91954(10) 0.0346(5) Uani 1 1 d . . . . .
H10 H 1.049065 1.189473 0.935585 0.042 Uiso 1 1 calc R U . . .
C11 C 0.8521(2) 1.0524(2) 0.91191(9) 0.0315(4) Uani 1 1 d . . . . .
H11 H 0.878919 0.976464 0.922929 0.038 Uiso 1 1 calc R U . . .
C12 C 0.7118(2) 1.0361(2) 0.88824(9) 0.0277(4) Uani 1 1 d . . . . .
H12 H 0.642828 0.949148 0.883228 0.033 Uiso 1 1 calc R U . . .
C13 C 0.4982(2) 1.1785(2) 0.80121(8) 0.0263(4) Uani 1 1 d . . . . .
C14 C 0.5953(2) 1.1837(2) 0.76151(9) 0.0296(4) Uani 1 1 d . . . . .
H14 H 0.676671 1.146335 0.765443 0.036 Uiso 1 1 calc R U . . .
C15 C 0.5754(2) 1.2422(2) 0.71657(9) 0.0314(4) Uani 1 1 d . . . . .
H15 H 0.643660 1.245113 0.690521 0.038 Uiso 1 1 calc R U . . .
C16 C 0.4559(2) 1.2970(2) 0.70919(9) 0.0294(4) Uani 1 1 d . . . . .
C17 C 0.3543(2) 1.2837(2) 0.74713(9) 0.0301(4) Uani 1 1 d . . . . .
H17 H 0.269149 1.314722 0.741706 0.036 Uiso 1 1 calc R U . . .
C18 C 0.3747(2) 1.2264(2) 0.79236(9) 0.0287(4) Uani 1 1 d . . . . .
H18 H 0.304278 1.219602 0.817513 0.034 Uiso 1 1 calc R U . . .
C19 C 0.4344(3) 1.3724(2) 0.66543(9) 0.0311(4) Uani 1 1 d . . . . .
C20 C 0.5485(3) 1.4549(2) 0.64438(9) 0.0340(5) Uani 1 1 d . . . . .
C21 C 0.5196(3) 1.5279(3) 0.60513(10) 0.0368(5) Uani 1 1 d . . . . .
H21 H 0.597367 1.583296 0.591353 0.044 Uiso 1 1 calc R U . . .
C22 C 0.2708(3) 1.4459(3) 0.60570(10) 0.0401(5) Uani 1 1 d . . . . .
H22 H 0.174635 1.443770 0.592428 0.048 Uiso 1 1 calc R U . . .
C23 C 0.2945(3) 1.3717(3) 0.64466(10) 0.0377(5) Uani 1 1 d . . . . .
H23 H 0.213855 1.318750 0.657793 0.045 Uiso 1 1 calc R U . . .
C24 C 0.3551(3) 1.5965(3) 0.54300(12) 0.0476(6) Uani 1 1 d . . . . .
H24A H 0.440391 1.672266 0.543511 0.071 Uiso 1 1 calc R U . . .
H24B H 0.271394 1.634741 0.550117 0.071 Uiso 1 1 calc R U . . .
H24C H 0.335310 1.532116 0.506706 0.071 Uiso 1 1 calc R U . . .
N6 N 0.51177(19) 0.6236(2) 0.85040(7) 0.0290(4) Uani 1 1 d . . . . .
N7 N 0.1572(2) 0.9726(2) 0.60848(8) 0.0352(4) Uani 1 1 d . . . . .
N8 N 0.0509(3) 0.8492(3) 0.73234(10) 0.0502(6) Uani 1 1 d . . . . .
N9 N -0.0442(3) 0.9126(4) 0.74370(12) 0.0610(7) Uani 1 1 d . . . . .
N10 N -0.1295(5) 0.9643(6) 0.76024(18) 0.1029(16) Uani 1 1 d . . . . .
C25 C 0.4287(2) 0.5936(2) 0.89399(8) 0.0250(4) Uani 1 1 d . . . . .
C26 C 0.3532(2) 0.6865(2) 0.91876(9) 0.0276(4) Uani 1 1 d . . . . .
H26 H 0.357115 0.770508 0.906853 0.033 Uiso 1 1 calc R U . . .
C27 C 0.2720(2) 0.6558(2) 0.96111(9) 0.0296(4) Uani 1 1 d . . . . .
H27 H 0.219795 0.718793 0.977803 0.036 Uiso 1 1 calc R U . . .
C28 C 0.2666(2) 0.5342(2) 0.97917(9) 0.0318(4) Uani 1 1 d . . . . .
H28 H 0.210605 0.513639 1.007968 0.038 Uiso 1 1 calc R U . . .
C29 C 0.3434(3) 0.4430(2) 0.95490(10) 0.0324(4) Uani 1 1 d . . . . .
H29 H 0.340562 0.359781 0.967292 0.039 Uiso 1 1 calc R U . . .
C30 C 0.4248(2) 0.4723(2) 0.91249(9) 0.0292(4) Uani 1 1 d . . . . .
H30 H 0.477785 0.409511 0.896161 0.035 Uiso 1 1 calc R U . . .
C31 C 0.6592(2) 0.6183(2) 0.85473(8) 0.0252(4) Uani 1 1 d . . . . .
C32 C 0.7442(2) 0.6624(2) 0.90575(9) 0.0283(4) Uani 1 1 d . . . . .
H32 H 0.703952 0.696659 0.937946 0.034 Uiso 1 1 calc R U . . .
C33 C 0.8880(2) 0.6563(2) 0.90959(10) 0.0342(5) Uani 1 1 d . . . . .
H33 H 0.945775 0.685564 0.944506 0.041 Uiso 1 1 calc R U . . .
C34 C 0.9473(2) 0.6077(3) 0.86276(11) 0.0369(5) Uani 1 1 d . . . . .
H34 H 1.046146 0.605248 0.865443 0.044 Uiso 1 1 calc R U . . .
C35 C 0.8629(2) 0.5625(3) 0.81201(11) 0.0358(5) Uani 1 1 d . . . . .
H35 H 0.903782 0.528689 0.779921 0.043 Uiso 1 1 calc R U . . .
C36 C 0.7183(2) 0.5666(2) 0.80782(9) 0.0293(4) Uani 1 1 d . . . . .
H36 H 0.659988 0.534186 0.773043 0.035 Uiso 1 1 calc R U . . .
C37 C 0.4510(2) 0.6693(2) 0.80668(8) 0.0277(4) Uani 1 1 d . . . . .
C38 C 0.3021(2) 0.6235(2) 0.78897(9) 0.0304(4) Uani 1 1 d . . . . .
H38 H 0.243023 0.555137 0.804485 0.036 Uiso 1 1 calc R U . . .
C39 C 0.2407(2) 0.6771(2) 0.74910(9) 0.0308(4) Uani 1 1 d . . . . .
H39 H 0.139429 0.645886 0.737838 0.037 Uiso 1 1 calc R U . . .
C40 C 0.3250(2) 0.7762(2) 0.72513(9) 0.0293(4) Uani 1 1 d . . . . .
C41 C 0.4751(2) 0.8143(2) 0.74028(9) 0.0308(4) Uani 1 1 d . . . . .
H41 H 0.534988 0.877185 0.722670 0.037 Uiso 1 1 calc R U . . .
C42 C 0.5374(2) 0.7621(2) 0.78028(9) 0.0311(4) Uani 1 1 d . . . . .
H42 H 0.639398 0.789149 0.789932 0.037 Uiso 1 1 calc R U . . .
C43 C 0.2628(3) 0.8448(2) 0.68524(9) 0.0313(4) Uani 1 1 d . . . . .
C44 C 0.1294(3) 0.8777(3) 0.68791(10) 0.0361(5) Uani 1 1 d . . . . .
C45 C 0.0777(3) 0.9388(3) 0.64851(10) 0.0398(5) Uani 1 1 d . . . . .
H45 H -0.015118 0.957049 0.649746 0.048 Uiso 1 1 calc R U . . .
C46 C 0.2903(3) 0.9538(3) 0.60668(10) 0.0405(5) Uani 1 1 d . . . . .
H46 H 0.347633 0.984902 0.579743 0.049 Uiso 1 1 calc R U . . .
C47 C 0.3444(3) 0.8888(3) 0.64430(10) 0.0374(5) Uani 1 1 d . . . . .
H47 H 0.438416 0.873631 0.642362 0.045 Uiso 1 1 calc R U . . .
C48 C 0.0930(3) 1.0292(3) 0.56525(12) 0.0499(7) Uani 1 1 d . . . . .
H48A H 0.021595 0.953967 0.539580 0.075 Uiso 1 1 calc R U . . .
H48B H 0.169353 1.071314 0.544978 0.075 Uiso 1 1 calc R U . . .
H48C H 0.045457 1.099827 0.582500 0.075 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0137 0.0067 '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 0.3281 0.5435 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 '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
H1A O1 H1B 104.5 . . ?
H2A O2 H2B 109.5 . . ?
H3A O3 H3B 109.5 . . ?
H4A O4 H4B 109.5 . . ?
H5A O5 H5B 104.5 . . ?
C1 N1 C7 117.06(16) . . ?
C13 N1 C1 122.40(16) . . ?
C13 N1 C7 120.14(17) . . ?
C21 N2 C24 119.2(2) . . ?
C22 N2 C21 121.3(2) . . ?
C22 N2 C24 119.5(2) . . ?
N4 N3 C20 118.1(2) . . ?
N5 N4 N3 170.6(3) . . ?
C2 C1 N1 120.09(18) . . ?
C6 C1 N1 120.62(18) . . ?
C6 C1 C2 119.27(19) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 C1 120.0(2) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 H3 119.7 . . ?
C4 C3 C2 120.7(2) . . ?
C4 C3 H3 119.7 . . ?
C3 C4 H4 120.4 . . ?
C3 C4 C5 119.2(2) . . ?
C5 C4 H4 120.4 . . ?
C4 C5 H5 119.7 . . ?
C6 C5 C4 120.6(2) . . ?
C6 C5 H5 119.7 . . ?
C1 C6 H6 119.9 . . ?
C5 C6 C1 120.1(2) . . ?
C5 C6 H6 119.9 . . ?
C8 C7 N1 120.91(18) . . ?
C8 C7 C12 119.62(19) . . ?
C12 C7 N1 119.43(18) . . ?
C7 C8 H8 120.0 . . ?
C7 C8 C9 120.03(19) . . ?
C9 C8 H8 120.0 . . ?
C8 C9 H9 119.9 . . ?
C10 C9 C8 120.2(2) . . ?
C10 C9 H9 119.9 . . ?
C9 C10 H10 120.1 . . ?
C11 C10 C9 119.7(2) . . ?
C11 C10 H10 120.1 . . ?
C10 C11 H11 119.8 . . ?
C10 C11 C12 120.38(19) . . ?
C12 C11 H11 119.8 . . ?
C7 C12 H12 120.0 . . ?
C11 C12 C7 120.0(2) . . ?
C11 C12 H12 120.0 . . ?
C14 C13 N1 120.86(18) . . ?
C18 C13 N1 121.37(18) . . ?
C18 C13 C14 117.75(18) . . ?
C13 C14 H14 119.2 . . ?
C15 C14 C13 121.6(2) . . ?
C15 C14 H14 119.2 . . ?
C14 C15 H15 119.6 . . ?
C14 C15 C16 120.7(2) . . ?
C16 C15 H15 119.6 . . ?
C15 C16 C17 117.46(19) . . ?
C15 C16 C19 123.9(2) . . ?
C17 C16 C19 118.64(19) . . ?
C16 C17 H17 119.1 . . ?
C18 C17 C16 121.8(2) . . ?
C18 C17 H17 119.1 . . ?
C13 C18 H18 119.7 . . ?
C17 C18 C13 120.5(2) . . ?
C17 C18 H18 119.7 . . ?
C20 C19 C16 123.9(2) . . ?
C23 C19 C16 120.2(2) . . ?
C23 C19 C20 115.7(2) . . ?
N3 C20 C19 117.9(2) . . ?
C21 C20 N3 121.5(2) . . ?
C21 C20 C19 120.6(2) . . ?
N2 C21 C20 120.4(2) . . ?
N2 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
N2 C22 H22 119.9 . . ?
N2 C22 C23 120.2(2) . . ?
C23 C22 H22 119.9 . . ?
C19 C23 H23 119.1 . . ?
C22 C23 C19 121.8(2) . . ?
C22 C23 H23 119.1 . . ?
N2 C24 H24A 109.5 . . ?
N2 C24 H24B 109.5 . . ?
N2 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C31 N6 C25 118.86(16) . . ?
C37 N6 C25 119.68(16) . . ?
C37 N6 C31 121.21(17) . . ?
C45 N7 C48 118.5(2) . . ?
C46 N7 C45 121.4(2) . . ?
C46 N7 C48 120.1(2) . . ?
N9 N8 C44 117.6(2) . . ?
N10 N9 N8 171.0(3) . . ?
C26 C25 N6 120.20(18) . . ?
C26 C25 C30 119.79(19) . . ?
C30 C25 N6 119.99(18) . . ?
C25 C26 H26 120.2 . . ?
C25 C26 C27 119.63(19) . . ?
C27 C26 H26 120.2 . . ?
C26 C27 H27 119.6 . . ?
C28 C27 C26 120.71(19) . . ?
C28 C27 H27 119.6 . . ?
C27 C28 H28 120.3 . . ?
C29 C28 C27 119.4(2) . . ?
C29 C28 H28 120.3 . . ?
C28 C29 H29 119.8 . . ?
C28 C29 C30 120.5(2) . . ?
C30 C29 H29 119.8 . . ?
C25 C30 H30 120.0 . . ?
C29 C30 C25 119.95(19) . . ?
C29 C30 H30 120.0 . . ?
C32 C31 N6 120.39(19) . . ?
C32 C31 C36 119.74(19) . . ?
C36 C31 N6 119.86(19) . . ?
C31 C32 H32 120.0 . . ?
C33 C32 C31 119.9(2) . . ?
C33 C32 H32 120.0 . . ?
C32 C33 H33 119.9 . . ?
C34 C33 C32 120.2(2) . . ?
C34 C33 H33 119.9 . . ?
C33 C34 H34 120.0 . . ?
C33 C34 C35 120.1(2) . . ?
C35 C34 H34 120.0 . . ?
C34 C35 H35 119.9 . . ?
C34 C35 C36 120.2(2) . . ?
C36 C35 H35 119.9 . . ?
C31 C36 H36 120.1 . . ?
C35 C36 C31 119.8(2) . . ?
C35 C36 H36 120.1 . . ?
C38 C37 N6 120.52(19) . . ?
C42 C37 N6 120.77(19) . . ?
C42 C37 C38 118.71(19) . . ?
C37 C38 H38 119.8 . . ?
C39 C38 C37 120.4(2) . . ?
C39 C38 H38 119.8 . . ?
C38 C39 H39 119.5 . . ?
C38 C39 C40 121.0(2) . . ?
C40 C39 H39 119.5 . . ?
C39 C40 C41 118.15(19) . . ?
C39 C40 C43 123.1(2) . . ?
C41 C40 C43 118.8(2) . . ?
C40 C41 H41 119.4 . . ?
C42 C41 C40 121.2(2) . . ?
C42 C41 H41 119.4 . . ?
C37 C42 H42 119.9 . . ?
C41 C42 C37 120.2(2) . . ?
C41 C42 H42 119.9 . . ?
C44 C43 C40 123.8(2) . . ?
C44 C43 C47 116.5(2) . . ?
C47 C43 C40 119.6(2) . . ?
C43 C44 N8 118.3(2) . . ?
C45 C44 N8 121.4(2) . . ?
C45 C44 C43 120.3(2) . . ?
N7 C45 C44 120.7(2) . . ?
N7 C45 H45 119.6 . . ?
C44 C45 H45 119.6 . . ?
N7 C46 H46 120.2 . . ?
N7 C46 C47 119.7(2) . . ?
C47 C46 H46 120.2 . . ?
C43 C47 H47 119.4 . . ?
C46 C47 C43 121.1(2) . . ?
C46 C47 H47 119.4 . . ?
N7 C48 H48A 109.5 . . ?
N7 C48 H48B 109.5 . . ?
N7 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
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
O1 H1A 0.8498 . ?
O1 H1B 0.8511 . ?
O2 H2A 0.8700 . ?
O2 H2B 0.8695 . ?
O3 H3A 0.8503 . ?
O3 H3B 0.8502 . ?
O4 H4A 0.8500 . ?
O4 H4B 0.8492 . ?
O5 H5A 0.8506 . ?
O5 H5B 0.8499 . ?
N1 C1 1.421(3) . ?
N1 C7 1.428(3) . ?
N1 C13 1.405(2) . ?
N2 C21 1.341(3) . ?
N2 C22 1.337(3) . ?
N2 C24 1.488(3) . ?
N3 N4 1.241(3) . ?
N3 C20 1.406(3) . ?
N4 N5 1.133(4) . ?
C1 C2 1.400(3) . ?
C1 C6 1.390(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.391(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.381(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.393(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.388(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.387(3) . ?
C7 C12 1.393(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.391(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.385(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.383(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.388(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.400(3) . ?
C13 C18 1.399(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.387(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.400(3) . ?
C16 C17 1.403(3) . ?
C16 C19 1.478(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.387(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.412(3) . ?
C19 C23 1.400(3) . ?
C20 C21 1.388(3) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C22 C23 1.377(3) . ?
C23 H23 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
N6 C25 1.426(3) . ?
N6 C31 1.422(3) . ?
N6 C37 1.406(2) . ?
N7 C45 1.343(3) . ?
N7 C46 1.333(3) . ?
N7 C48 1.477(3) . ?
N8 N9 1.247(3) . ?
N8 C44 1.416(3) . ?
N9 N10 1.127(4) . ?
C25 C26 1.391(3) . ?
C25 C30 1.391(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.392(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.386(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.384(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.391(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.391(3) . ?
C31 C36 1.392(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.390(3) . ?
C33 H33 0.9500 . ?
C33 C34 1.382(4) . ?
C34 H34 0.9500 . ?
C34 C35 1.383(4) . ?
C35 H35 0.9500 . ?
C35 C36 1.392(3) . ?
C36 H36 0.9500 . ?
C37 C38 1.402(3) . ?
C37 C42 1.399(3) . ?
C38 H38 0.9500 . ?
C38 C39 1.381(3) . ?
C39 H39 0.9500 . ?
C39 C40 1.394(3) . ?
C40 C41 1.401(3) . ?
C40 C43 1.487(3) . ?
C41 H41 0.9500 . ?
C41 C42 1.379(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.395(3) . ?
C43 C47 1.404(3) . ?
C44 C45 1.381(3) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C46 C47 1.385(3) . ?
C47 H47 0.9500 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
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
N1 C1 C2 C3 -179.15(18) . . . . ?
N1 C1 C6 C5 -179.18(18) . . . . ?
N1 C7 C8 C9 178.3(2) . . . . ?
N1 C7 C12 C11 -178.32(19) . . . . ?
N1 C13 C14 C15 -174.5(2) . . . . ?
N1 C13 C18 C17 175.1(2) . . . . ?
N2 C22 C23 C19 0.2(4) . . . . ?
N3 C20 C21 N2 -176.6(2) . . . . ?
N4 N3 C20 C19 173.6(3) . . . . ?
N4 N3 C20 C21 -9.9(4) . . . . ?
C1 N1 C7 C8 -125.4(2) . . . . ?
C1 N1 C7 C12 52.1(3) . . . . ?
C1 N1 C13 C14 -157.6(2) . . . . ?
C1 N1 C13 C18 24.0(3) . . . . ?
C1 C2 C3 C4 -1.1(3) . . . . ?
C2 C1 C6 C5 2.4(3) . . . . ?
C2 C3 C4 C5 1.2(3) . . . . ?
C3 C4 C5 C6 0.5(3) . . . . ?
C4 C5 C6 C1 -2.3(3) . . . . ?
C6 C1 C2 C3 -0.7(3) . . . . ?
C7 N1 C1 C2 31.9(3) . . . . ?
C7 N1 C1 C6 -146.47(19) . . . . ?
C7 N1 C13 C14 29.9(3) . . . . ?
C7 N1 C13 C18 -148.5(2) . . . . ?
C7 C8 C9 C10 -0.2(4) . . . . ?
C8 C7 C12 C11 -0.7(3) . . . . ?
C8 C9 C10 C11 -0.4(4) . . . . ?
C9 C10 C11 C12 0.3(4) . . . . ?
C10 C11 C12 C7 0.2(3) . . . . ?
C12 C7 C8 C9 0.7(3) . . . . ?
C13 N1 C1 C2 -140.8(2) . . . . ?
C13 N1 C1 C6 40.8(3) . . . . ?
C13 N1 C7 C8 47.5(3) . . . . ?
C13 N1 C7 C12 -134.9(2) . . . . ?
C13 C14 C15 C16 -0.6(3) . . . . ?
C14 C13 C18 C17 -3.3(3) . . . . ?
C14 C15 C16 C17 -3.3(3) . . . . ?
C14 C15 C16 C19 174.1(2) . . . . ?
C15 C16 C17 C18 3.9(3) . . . . ?
C15 C16 C19 C20 -31.8(3) . . . . ?
C15 C16 C19 C23 152.3(2) . . . . ?
C16 C17 C18 C13 -0.6(3) . . . . ?
C16 C19 C20 N3 -0.3(3) . . . . ?
C16 C19 C20 C21 -176.9(2) . . . . ?
C16 C19 C23 C22 177.0(2) . . . . ?
C17 C16 C19 C20 145.6(2) . . . . ?
C17 C16 C19 C23 -30.3(3) . . . . ?
C18 C13 C14 C15 4.0(3) . . . . ?
C19 C16 C17 C18 -173.6(2) . . . . ?
C19 C20 C21 N2 -0.2(4) . . . . ?
C20 C19 C23 C22 0.7(4) . . . . ?
C21 N2 C22 C23 -1.2(4) . . . . ?
C22 N2 C21 C20 1.2(4) . . . . ?
C23 C19 C20 N3 175.8(2) . . . . ?
C23 C19 C20 C21 -0.8(3) . . . . ?
C24 N2 C21 C20 -177.9(2) . . . . ?
C24 N2 C22 C23 177.9(2) . . . . ?
N6 C25 C26 C27 179.74(19) . . . . ?
N6 C25 C30 C29 -179.8(2) . . . . ?
N6 C31 C32 C33 179.71(19) . . . . ?
N6 C31 C36 C35 179.48(19) . . . . ?
N6 C37 C38 C39 174.7(2) . . . . ?
N6 C37 C42 C41 -175.1(2) . . . . ?
N7 C46 C47 C43 -1.4(4) . . . . ?
N8 C44 C45 N7 176.0(3) . . . . ?
N9 N8 C44 C43 159.9(3) . . . . ?
N9 N8 C44 C45 -18.9(4) . . . . ?
C25 N6 C31 C32 -36.5(3) . . . . ?
C25 N6 C31 C36 142.4(2) . . . . ?
C25 N6 C37 C38 -32.1(3) . . . . ?
C25 N6 C37 C42 147.4(2) . . . . ?
C25 C26 C27 C28 0.6(3) . . . . ?
C26 C25 C30 C29 1.3(3) . . . . ?
C26 C27 C28 C29 0.3(3) . . . . ?
C27 C28 C29 C30 -0.4(3) . . . . ?
C28 C29 C30 C25 -0.4(3) . . . . ?
C30 C25 C26 C27 -1.4(3) . . . . ?
C31 N6 C25 C26 127.3(2) . . . . ?
C31 N6 C25 C30 -51.6(3) . . . . ?
C31 N6 C37 C38 153.6(2) . . . . ?
C31 N6 C37 C42 -26.9(3) . . . . ?
C31 C32 C33 C34 0.6(3) . . . . ?
C32 C31 C36 C35 -1.6(3) . . . . ?
C32 C33 C34 C35 -1.2(3) . . . . ?
C33 C34 C35 C36 0.4(3) . . . . ?
C34 C35 C36 C31 1.0(3) . . . . ?
C36 C31 C32 C33 0.8(3) . . . . ?
C37 N6 C25 C26 -47.1(3) . . . . ?
C37 N6 C25 C30 134.0(2) . . . . ?
C37 N6 C31 C32 137.9(2) . . . . ?
C37 N6 C31 C36 -43.2(3) . . . . ?
C37 C38 C39 C40 0.8(3) . . . . ?
C38 C37 C42 C41 4.4(3) . . . . ?
C38 C39 C40 C41 3.6(3) . . . . ?
C38 C39 C40 C43 -175.2(2) . . . . ?
C39 C40 C41 C42 -4.0(3) . . . . ?
C39 C40 C43 C44 34.5(3) . . . . ?
C39 C40 C43 C47 -150.0(2) . . . . ?
C40 C41 C42 C37 0.0(3) . . . . ?
C40 C43 C44 N8 2.6(4) . . . . ?
C40 C43 C44 C45 -178.6(2) . . . . ?
C40 C43 C47 C46 -179.6(2) . . . . ?
C41 C40 C43 C44 -144.3(2) . . . . ?
C41 C40 C43 C47 31.2(3) . . . . ?
C42 C37 C38 C39 -4.8(3) . . . . ?
C43 C40 C41 C42 174.9(2) . . . . ?
C43 C44 C45 N7 -2.7(4) . . . . ?
C44 C43 C47 C46 -3.7(4) . . . . ?
C45 N7 C46 C47 4.8(4) . . . . ?
C46 N7 C45 C44 -2.8(4) . . . . ?
C47 C43 C44 N8 -173.1(2) . . . . ?
C47 C43 C44 C45 5.7(4) . . . . ?
C48 N7 C45 C44 176.0(3) . . . . ?
C48 N7 C46 C47 -174.0(3) . . . . ?
