#------------------------------------------------------------------------------
#$Date: 2021-11-06 21:50:30 +0200 (Sat, 06 Nov 2021) $
#$Revision: 270422 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/37/7243710.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_7243710
loop_
_publ_author_name
'Lombard, Jean'
'Laker, Heinrich'
'Prins, Francis'
'Wahl, Helene'
'le Roex, Tanya'
'Haynes, Delia A.'
_publ_section_title
;
 Selectivity of hosts for guests by liquid-assisted grinding: differences
 between solution and mechanochemistry
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              7380
_journal_page_last               7384
_journal_paper_doi               10.1039/D1CE01286J
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C23 H15 O6, C12 H9 N2, C3 H7 N O'
_chemical_formula_sum            'C38 H31 N3 O7'
_chemical_formula_weight         641.66
_chemical_name_common            '1,10-phenanthrolinium pamoate DMF solvate'
_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     direct
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2021-09-23 deposited with the CCDC.	2021-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                82.162(5)
_cell_angle_beta                 72.106(5)
_cell_angle_gamma                72.058(5)
_cell_formula_units_Z            2
_cell_length_a                   10.6989(18)
_cell_length_b                   11.630(2)
_cell_length_c                   13.421(2)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      28.16
_cell_measurement_theta_min      2.24
_cell_volume                     1510.3(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      105(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0974
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            53114
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.355
_diffrn_reflns_theta_min         1.842
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'symmetry-related measurements'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.070
_exptl_transmission_factor_max   0.7208
_exptl_transmission_factor_min   0.6344
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7485
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0503
_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)+(0.0638P)²+0.6159P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1335
_refine_ls_wR_factor_ref         0.1480
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5803
_reflns_number_total             7485
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce01286j2.cif
_cod_data_source_block           1-DMF
_cod_depositor_comments
'Adding full bibliography for 7243708--7243711.cif.'
_cod_original_cell_volume        1510.4(5)
_cod_database_code               7243710
_shelx_shelxl_version_number     2016/6
_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_min   0.976
_shelx_estimated_absorpt_t_max   0.995
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
O1 O 0.81966(13) 0.70830(11) 0.22509(9) 0.0342(3) Uani 1 1 d . . . . .
O2 O 0.89956(12) 0.86441(11) 0.14875(8) 0.0308(3) Uani 1 1 d . . . . .
C3 C 0.88204(15) 0.78398(14) 0.22301(11) 0.0242(3) Uani 1 1 d . . . . .
C4 C 0.94014(14) 0.78415(13) 0.31147(10) 0.0207(3) Uani 1 1 d . . . . .
C5 C 1.01552(15) 0.86194(13) 0.30771(11) 0.0219(3) Uani 1 1 d . . . . .
H5 H 1.029404 0.916783 0.248809 0.026 Uiso 1 1 calc R U . . .
C6 C 1.07295(14) 0.86237(13) 0.38935(11) 0.0206(3) Uani 1 1 d . . . . .
C7 C 1.15453(15) 0.94058(14) 0.38400(12) 0.0247(3) Uani 1 1 d . . . . .
H7 H 1.171143 0.993684 0.324164 0.030 Uiso 1 1 calc R U . . .
C8 C 1.20927(16) 0.94049(15) 0.46347(12) 0.0269(3) Uani 1 1 d . . . . .
H8 H 1.262038 0.994215 0.459642 0.032 Uiso 1 1 calc R U . . .
C9 C 1.18665(15) 0.85946(14) 0.55181(12) 0.0252(3) Uani 1 1 d . . . . .
H9 H 1.226954 0.857694 0.606177 0.030 Uiso 1 1 calc R U . . .
C10 C 1.10782(14) 0.78382(13) 0.56008(11) 0.0210(3) Uani 1 1 d . . . . .
H10 H 1.094449 0.730326 0.620031 0.025 Uiso 1 1 calc R U . . .
C11 C 1.04522(13) 0.78384(12) 0.48014(10) 0.0181(3) Uani 1 1 d . . . . .
C12 C 0.95876(14) 0.70916(12) 0.48831(10) 0.0181(3) Uani 1 1 d . . . . .
C13 C 0.91358(14) 0.70546(12) 0.40254(11) 0.0195(3) Uani 1 1 d . . . . .
O14 O 0.83848(11) 0.62826(10) 0.40624(8) 0.0252(2) Uani 1 1 d . . . . .
H14 H 0.822(3) 0.641(2) 0.339(2) 0.066(7) Uiso 1 1 d . . . . .
C15 C 0.91200(14) 0.63723(12) 0.58967(10) 0.0195(3) Uani 1 1 d . . . . .
H15A H 0.857432 0.587930 0.578092 0.023 Uiso 1 1 calc R U . . .
H15B H 0.993591 0.581099 0.607504 0.023 Uiso 1 1 calc R U . . .
C16 C 0.82660(14) 0.71684(12) 0.68177(10) 0.0178(3) Uani 1 1 d . . . . .
C17 C 0.69460(14) 0.79753(12) 0.68373(10) 0.0172(3) Uani 1 1 d . . . . .
C18 C 0.63099(15) 0.80217(13) 0.60354(11) 0.0207(3) Uani 1 1 d . . . . .
H18 H 0.676384 0.748876 0.547528 0.025 Uiso 1 1 calc R U . . .
C19 C 0.50557(15) 0.88211(14) 0.60582(12) 0.0249(3) Uani 1 1 d . . . . .
H19 H 0.466058 0.883896 0.550975 0.030 Uiso 1 1 calc R U . . .
C20 C 0.43418(15) 0.96182(14) 0.68834(13) 0.0271(3) Uani 1 1 d . . . . .
H20 H 0.347921 1.017492 0.688383 0.033 Uiso 1 1 calc R U . . .
C21 C 0.48983(15) 0.95855(14) 0.76834(12) 0.0240(3) Uani 1 1 d . . . . .
H21 H 0.440993 1.011275 0.824432 0.029 Uiso 1 1 calc R U . . .
C22 C 0.62024(14) 0.87687(12) 0.76835(10) 0.0186(3) Uani 1 1 d . . . . .
C23 C 0.67928(15) 0.87262(13) 0.85009(10) 0.0202(3) Uani 1 1 d . . . . .
H23 H 0.631626 0.925968 0.905869 0.024 Uiso 1 1 calc R U . . .
C24 C 0.80422(15) 0.79286(13) 0.85047(10) 0.0199(3) Uani 1 1 d . . . . .
C25 C 0.87710(14) 0.71234(12) 0.76630(10) 0.0190(3) Uani 1 1 d . . . . .
O26 O 0.99894(11) 0.63066(10) 0.76835(8) 0.0250(2) Uani 1 1 d . . . . .
H26 H 1.011(2) 0.649(2) 0.831(2) 0.062(7) Uiso 1 1 d . . . . .
H30 H 0.580(2) 0.348(2) 0.1720(18) 0.048(6) Uiso 1 1 d . . . . .
C27 C 0.86567(16) 0.79069(14) 0.93751(11) 0.0233(3) Uani 1 1 d . . . . .
O28 O 0.97881(12) 0.71777(11) 0.93757(9) 0.0330(3) Uani 1 1 d . . . . .
O29 O 0.79619(12) 0.86739(10) 1.00850(8) 0.0309(3) Uani 1 1 d . . . . .
N30 N 0.61666(13) 0.29923(12) 0.11780(11) 0.0248(3) Uani 1 1 d . . . . .
C31 C 0.73944(16) 0.22330(15) 0.11529(14) 0.0307(3) Uani 1 1 d . . . . .
H31 H 0.781502 0.224487 0.167874 0.037 Uiso 1 1 calc R U . . .
C32 C 0.80583(18) 0.14247(15) 0.03578(15) 0.0358(4) Uani 1 1 d . . . . .
H32 H 0.893425 0.088034 0.033568 0.043 Uiso 1 1 calc R U . . .
C33 C 0.74388(18) 0.14184(15) -0.03959(14) 0.0339(4) Uani 1 1 d . . . . .
H33 H 0.788691 0.086111 -0.093823 0.041 Uiso 1 1 calc R U . . .
C34 C 0.61466(17) 0.22281(14) -0.03752(12) 0.0282(3) Uani 1 1 d . . . . .
C35 C 0.5440(2) 0.22690(16) -0.11381(13) 0.0356(4) Uani 1 1 d . . . . .
H35 H 0.585623 0.173243 -0.169745 0.043 Uiso 1 1 calc R U . . .
C36 C 0.4193(2) 0.30580(16) -0.10732(13) 0.0359(4) Uani 1 1 d . . . . .
H36 H 0.374200 0.306198 -0.158311 0.043 Uiso 1 1 calc R U . . .
C37 C 0.35406(17) 0.38912(15) -0.02443(12) 0.0290(3) Uani 1 1 d . . . . .
C38 C 0.22376(19) 0.47277(17) -0.01366(14) 0.0369(4) Uani 1 1 d . . . . .
H38 H 0.175387 0.477634 -0.063485 0.044 Uiso 1 1 calc R U . . .
C39 C 0.16776(18) 0.54676(17) 0.06913(15) 0.0383(4) Uani 1 1 d . . . . .
H39 H 0.079963 0.603391 0.077666 0.046 Uiso 1 1 calc R U . . .
C40 C 0.24170(17) 0.53795(15) 0.14137(14) 0.0330(4) Uani 1 1 d . . . . .
H40 H 0.201176 0.589773 0.198636 0.040 Uiso 1 1 calc R U . . .
N41 N 0.36480(13) 0.46152(11) 0.13438(10) 0.0265(3) Uani 1 1 d . . . . .
C42 C 0.41949(16) 0.38793(13) 0.05253(12) 0.0240(3) Uani 1 1 d . . . . .
C43 C 0.55138(15) 0.30294(13) 0.04456(11) 0.0232(3) Uani 1 1 d . . . . .
O44 O 0.62864(14) 0.39454(12) 0.28293(11) 0.0448(3) Uani 1 1 d . . . . .
C45 C 0.61803(18) 0.48442(15) 0.32642(13) 0.0330(4) Uani 1 1 d . . . . .
H45 H 0.700623 0.497265 0.328595 0.040 Uiso 1 1 calc R U . . .
N46 N 0.50172(14) 0.56595(13) 0.37099(11) 0.0323(3) Uani 1 1 d . . . . .
C47 C 0.5008(2) 0.67126(18) 0.41832(17) 0.0464(5) Uani 1 1 d . . . . .
H47A H 0.594391 0.666261 0.417065 0.070 Uiso 1 1 calc R U . . .
H47B H 0.443086 0.673985 0.491016 0.070 Uiso 1 1 calc R U . . .
H47C H 0.464297 0.744662 0.378846 0.070 Uiso 1 1 calc R U . . .
C48 C 0.3703(2) 0.5553(2) 0.37032(18) 0.0493(5) Uani 1 1 d . . . . .
H48A H 0.384875 0.487535 0.328015 0.074 Uiso 1 1 calc R U . . .
H48B H 0.320161 0.630345 0.340249 0.074 Uiso 1 1 calc R U . . .
H48C H 0.317138 0.540952 0.442241 0.074 Uiso 1 1 calc R U . . .
H1 H 0.850(4) 0.860(3) 0.084(3) 0.118(12) Uiso 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C3 O2 H1 112.4(17) . . ?
O1 C3 O2 123.73(13) . . ?
O1 C3 C4 119.82(13) . . ?
O2 C3 C4 116.45(13) . . ?
C5 C4 C13 119.25(13) . . ?
C5 C4 C3 120.59(13) . . ?
C13 C4 C3 120.13(13) . . ?
C4 C5 C6 121.55(13) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C5 C6 C7 121.53(13) . . ?
C5 C6 C11 118.66(13) . . ?
C7 C6 C11 119.80(13) . . ?
C8 C7 C6 121.06(14) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C7 C8 C9 119.41(14) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
C10 C9 C8 121.14(13) . . ?
C10 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
C9 C10 C11 121.16(13) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C12 C11 C10 122.39(12) . . ?
C12 C11 C6 120.24(12) . . ?
C10 C11 C6 117.36(13) . . ?
C13 C12 C11 118.58(12) . . ?
C13 C12 C15 119.96(12) . . ?
C11 C12 C15 121.43(12) . . ?
O14 C13 C12 119.45(12) . . ?
O14 C13 C4 119.19(12) . . ?
C12 C13 C4 121.32(13) . . ?
C13 O14 H14 103.4(15) . . ?
C16 C15 C12 113.21(11) . . ?
C16 C15 H15A 108.9 . . ?
C12 C15 H15A 108.9 . . ?
C16 C15 H15B 108.9 . . ?
C12 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
C25 C16 C17 118.50(12) . . ?
C25 C16 C15 119.82(12) . . ?
C17 C16 C15 121.68(12) . . ?
C18 C17 C16 122.21(12) . . ?
C18 C17 C22 117.35(12) . . ?
C16 C17 C22 120.43(12) . . ?
C19 C18 C17 121.23(13) . . ?
C19 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
C18 C19 C20 121.07(13) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 H19 119.5 . . ?
C21 C20 C19 119.72(14) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C20 C21 C22 120.72(13) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C23 C22 C21 121.43(13) . . ?
C23 C22 C17 118.70(12) . . ?
C21 C22 C17 119.87(12) . . ?
C24 C23 C22 121.28(13) . . ?
C24 C23 H23 119.4 . . ?
C22 C23 H23 119.4 . . ?
C23 C24 C25 119.71(12) . . ?
C23 C24 C27 120.40(13) . . ?
C25 C24 C27 119.89(13) . . ?
O26 C25 C16 119.07(12) . . ?
O26 C25 C24 119.69(12) . . ?
C16 C25 C24 121.23(12) . . ?
C25 O26 H26 101.8(15) . . ?
O28 C27 O29 123.63(13) . . ?
O28 C27 C24 120.06(13) . . ?
O29 C27 C24 116.31(13) . . ?
C31 N30 C43 123.02(14) . . ?
C31 N30 H30 114.7(14) . . ?
C43 N30 H30 122.3(14) . . ?
N30 C31 C32 119.90(16) . . ?
N30 C31 H31 120.1 . . ?
C32 C31 H31 120.1 . . ?
C33 C32 C31 119.39(16) . . ?
C33 C32 H32 120.3 . . ?
C31 C32 H32 120.3 . . ?
C32 C33 C34 120.74(15) . . ?
C32 C33 H33 119.6 . . ?
C34 C33 H33 119.6 . . ?
C43 C34 C33 117.80(15) . . ?
C43 C34 C35 118.57(15) . . ?
C33 C34 C35 123.62(15) . . ?
C36 C35 C34 121.08(16) . . ?
C36 C35 H35 119.5 . . ?
C34 C35 H35 119.5 . . ?
C35 C36 C37 120.95(16) . . ?
C35 C36 H36 119.5 . . ?
C37 C36 H36 119.5 . . ?
C38 C37 C42 116.84(16) . . ?
C38 C37 C36 123.25(16) . . ?
C42 C37 C36 119.90(15) . . ?
C39 C38 C37 119.38(16) . . ?
C39 C38 H38 120.3 . . ?
C37 C38 H38 120.3 . . ?
C38 C39 C40 119.12(16) . . ?
C38 C39 H39 120.4 . . ?
C40 C39 H39 120.4 . . ?
N41 C40 C39 123.85(17) . . ?
N41 C40 H40 118.1 . . ?
C39 C40 H40 118.1 . . ?
C40 N41 C42 116.79(14) . . ?
N41 C42 C37 124.02(14) . . ?
N41 C42 C43 117.73(14) . . ?
C37 C42 C43 118.25(14) . . ?
N30 C43 C34 119.14(14) . . ?
N30 C43 C42 119.61(13) . . ?
C34 C43 C42 121.25(14) . . ?
O44 C45 N46 126.25(17) . . ?
O44 C45 H45 116.9 . . ?
N46 C45 H45 116.9 . . ?
C45 N46 C47 121.80(15) . . ?
C45 N46 C48 121.04(15) . . ?
C47 N46 C48 117.11(15) . . ?
N46 C47 H47A 109.5 . . ?
N46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
N46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
N46 C48 H48A 109.5 . . ?
N46 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
N46 C48 H48C 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 C3 1.2508(19) . ?
O2 C3 1.2816(19) . ?
O2 H1 1.17(4) . ?
C3 C4 1.5002(19) . ?
C4 C5 1.372(2) . ?
C4 C13 1.433(2) . ?
C5 C6 1.413(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.424(2) . ?
C6 C11 1.4311(19) . ?
C7 C8 1.365(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.418(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.368(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.4286(19) . ?
C10 H10 0.9500 . ?
C11 C12 1.4243(19) . ?
C12 C13 1.3888(19) . ?
C12 C15 1.5264(19) . ?
C13 O14 1.3645(17) . ?
O14 H14 0.96(3) . ?
C15 C16 1.5221(19) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C25 1.3875(19) . ?
C16 C17 1.4294(19) . ?
C17 C18 1.4269(19) . ?
C17 C22 1.4327(19) . ?
C18 C19 1.371(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.412(2) . ?
C19 H19 0.9500 . ?
C20 C21 1.370(2) . ?
C20 H20 0.9500 . ?
C21 C22 1.426(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.4131(19) . ?
C23 C24 1.373(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.435(2) . ?
C24 C27 1.5004(19) . ?
C25 O26 1.3617(17) . ?
O26 H26 0.94(3) . ?
C27 O28 1.2459(19) . ?
C27 O29 1.2822(19) . ?
N30 C31 1.331(2) . ?
N30 C43 1.359(2) . ?
N30 H30 0.90(2) . ?
C31 C32 1.387(2) . ?
C31 H31 0.9500 . ?
C32 C33 1.371(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.407(2) . ?
C33 H33 0.9500 . ?
C34 C43 1.405(2) . ?
C34 C35 1.436(2) . ?
C35 C36 1.351(3) . ?
C35 H35 0.9500 . ?
C36 C37 1.437(2) . ?
C36 H36 0.9500 . ?
C37 C38 1.411(2) . ?
C37 C42 1.411(2) . ?
C38 C39 1.367(3) . ?
C38 H38 0.9500 . ?
C39 C40 1.404(3) . ?
C39 H39 0.9500 . ?
C40 N41 1.326(2) . ?
C40 H40 0.9500 . ?
N41 C42 1.355(2) . ?
C42 C43 1.434(2) . ?
O44 C45 1.224(2) . ?
C45 N46 1.333(2) . ?
C45 H45 0.9500 . ?
N46 C47 1.451(2) . ?
N46 C48 1.452(2) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O14 H14 O1 0.96(3) 1.62(3) 2.5272(16) 157(2) .
O26 H26 O28 0.94(3) 1.63(3) 2.5344(16) 159(2) .
N30 H30 O44 0.90(2) 1.91(2) 2.6624(19) 140(2) .
O2 H1 O29 1.17(4) 1.28(4) 2.4506(15) 173(3) 1_554
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
O1 C3 C4 C5 176.28(14) . . . . ?
O2 C3 C4 C5 -4.2(2) . . . . ?
O1 C3 C4 C13 -5.7(2) . . . . ?
O2 C3 C4 C13 173.78(13) . . . . ?
C13 C4 C5 C6 3.0(2) . . . . ?
C3 C4 C5 C6 -179.02(13) . . . . ?
C4 C5 C6 C7 178.11(13) . . . . ?
C4 C5 C6 C11 -3.3(2) . . . . ?
C5 C6 C7 C8 179.83(14) . . . . ?
C11 C6 C7 C8 1.2(2) . . . . ?
C6 C7 C8 C9 1.2(2) . . . . ?
C7 C8 C9 C10 -1.8(2) . . . . ?
C8 C9 C10 C11 -0.1(2) . . . . ?
C9 C10 C11 C12 -177.75(13) . . . . ?
C9 C10 C11 C6 2.5(2) . . . . ?
C5 C6 C11 C12 -1.4(2) . . . . ?
C7 C6 C11 C12 177.21(13) . . . . ?
C5 C6 C11 C10 178.29(12) . . . . ?
C7 C6 C11 C10 -3.07(19) . . . . ?
C10 C11 C12 C13 -173.42(12) . . . . ?
C6 C11 C12 C13 6.29(19) . . . . ?
C10 C11 C12 C15 8.5(2) . . . . ?
C6 C11 C12 C15 -171.78(12) . . . . ?
C11 C12 C13 O14 175.53(12) . . . . ?
C15 C12 C13 O14 -6.37(19) . . . . ?
C11 C12 C13 C4 -6.7(2) . . . . ?
C15 C12 C13 C4 171.43(12) . . . . ?
C5 C4 C13 O14 179.92(12) . . . . ?
C3 C4 C13 O14 1.92(19) . . . . ?
C5 C4 C13 C12 2.1(2) . . . . ?
C3 C4 C13 C12 -175.88(12) . . . . ?
C13 C12 C15 C16 -116.22(14) . . . . ?
C11 C12 C15 C16 61.82(17) . . . . ?
C12 C15 C16 C25 -113.86(14) . . . . ?
C12 C15 C16 C17 65.84(16) . . . . ?
C25 C16 C17 C18 -175.76(12) . . . . ?
C15 C16 C17 C18 4.5(2) . . . . ?
C25 C16 C17 C22 3.65(19) . . . . ?
C15 C16 C17 C22 -176.05(12) . . . . ?
C16 C17 C18 C19 -178.58(13) . . . . ?
C22 C17 C18 C19 2.0(2) . . . . ?
C17 C18 C19 C20 -0.7(2) . . . . ?
C18 C19 C20 C21 -0.9(2) . . . . ?
C19 C20 C21 C22 1.1(2) . . . . ?
C20 C21 C22 C23 179.79(14) . . . . ?
C20 C21 C22 C17 0.3(2) . . . . ?
C18 C17 C22 C23 178.70(12) . . . . ?
C16 C17 C22 C23 -0.74(19) . . . . ?
C18 C17 C22 C21 -1.76(19) . . . . ?
C16 C17 C22 C21 178.80(12) . . . . ?
C21 C22 C23 C24 179.24(13) . . . . ?
C17 C22 C23 C24 -1.2(2) . . . . ?
C22 C23 C24 C25 0.3(2) . . . . ?
C22 C23 C24 C27 179.41(12) . . . . ?
C17 C16 C25 O26 176.05(12) . . . . ?
C15 C16 C25 O26 -4.24(19) . . . . ?
C17 C16 C25 C24 -4.69(19) . . . . ?
C15 C16 C25 C24 175.02(12) . . . . ?
C23 C24 C25 O26 -177.93(12) . . . . ?
C27 C24 C25 O26 2.91(19) . . . . ?
C23 C24 C25 C16 2.8(2) . . . . ?
C27 C24 C25 C16 -176.34(12) . . . . ?
C23 C24 C27 O28 179.72(13) . . . . ?
C25 C24 C27 O28 -1.1(2) . . . . ?
C23 C24 C27 O29 -0.9(2) . . . . ?
C25 C24 C27 O29 178.24(12) . . . . ?
C43 N30 C31 C32 -0.6(2) . . . . ?
N30 C31 C32 C33 0.0(2) . . . . ?
C31 C32 C33 C34 0.6(3) . . . . ?
C32 C33 C34 C43 -0.6(2) . . . . ?
C32 C33 C34 C35 -179.92(15) . . . . ?
C43 C34 C35 C36 0.0(2) . . . . ?
C33 C34 C35 C36 179.31(15) . . . . ?
C34 C35 C36 C37 0.7(2) . . . . ?
C35 C36 C37 C38 -179.60(15) . . . . ?
C35 C36 C37 C42 -0.9(2) . . . . ?
C42 C37 C38 C39 -0.3(2) . . . . ?
C36 C37 C38 C39 178.39(15) . . . . ?
C37 C38 C39 C40 0.2(2) . . . . ?
C38 C39 C40 N41 0.3(3) . . . . ?
C39 C40 N41 C42 -0.6(2) . . . . ?
C40 N41 C42 C37 0.5(2) . . . . ?
C40 N41 C42 C43 -178.82(13) . . . . ?
C38 C37 C42 N41 -0.1(2) . . . . ?
C36 C37 C42 N41 -178.82(14) . . . . ?
C38 C37 C42 C43 179.27(13) . . . . ?
C36 C37 C42 C43 0.5(2) . . . . ?
C31 N30 C43 C34 0.5(2) . . . . ?
C31 N30 C43 C42 -179.65(13) . . . . ?
C33 C34 C43 N30 0.0(2) . . . . ?
C35 C34 C43 N30 179.42(13) . . . . ?
C33 C34 C43 C42 -179.75(13) . . . . ?
C35 C34 C43 C42 -0.4(2) . . . . ?
N41 C42 C43 N30 -0.3(2) . . . . ?
C37 C42 C43 N30 -179.68(13) . . . . ?
N41 C42 C43 C34 179.51(13) . . . . ?
C37 C42 C43 C34 0.1(2) . . . . ?
O44 C45 N46 C47 -178.43(18) . . . . ?
O44 C45 N46 C48 -1.0(3) . . . . ?
