#------------------------------------------------------------------------------
#$Date: 2020-04-01 02:36:09 +0300 (Wed, 01 Apr 2020) $
#$Revision: 249887 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/03/81/4038157.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_4038157
loop_
_publ_author_name
'Taimoory, S. Maryamdokht'
'Twum, Kwaku'
'Dashti, Mohadeseh'
'Pan, FangFang'
'Lahtinen, Manu'
'Rissanen, Kari'
'Puttreddy, Rakesh'
'Trant, John F.'
'Beyeh, Ngong Kodiah'
_publ_section_title
;
 Bringing a Molecular Plus One: Synergistic Binding Creates Guest-Mediated
 Three Component Complexes.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c00220
_journal_year                    2020
_chemical_formula_moiety         'C40 H48 O8, C5 H6 N, C7 H11 O2'
_chemical_formula_sum            'C52 H65 N O10'
_chemical_formula_weight         864.05
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-07-06
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   50.2896(7)
_cell_length_b                   16.4078(3)
_cell_length_c                   16.6971(4)
_cell_measurement_reflns_used    6776
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.4120
_cell_measurement_theta_min      3.8660
_cell_volume                     13777.5(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω      8.00 116.00   1.00   20.00    --   38.35  57.00  60.00  108
  2  ω    -38.00  70.00   1.00   20.00    --   38.35 -37.00 120.00  108
  3  ω     78.00 107.00   1.00   65.00    --  116.00  30.00-120.00   29
  4  ω     46.00 112.00   1.00   65.00    --  116.00 -61.00 150.00   66
  5  ω     43.00 136.00   1.00   65.00    --  116.00 -61.00 -60.00   93
  6  ω    119.00 178.00   1.00   65.00    --  116.00  30.00-120.00   59
  7  ω     29.00 109.00   1.00   65.00    --  116.00 -94.00 120.00   80
  8  ω     33.00 151.00   1.00   65.00    --  116.00 -15.00-120.00  118
  9  ω    153.00 178.00   1.00   65.00    --  116.00  61.00  60.00   25
 10  ω      6.00  82.00   1.00   20.00    --   38.38  57.00-150.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0191608000
_diffrn_orient_matrix_UB_12      0.0666935000
_diffrn_orient_matrix_UB_13      0.0298113000
_diffrn_orient_matrix_UB_21      -0.0144948000
_diffrn_orient_matrix_UB_22      -0.0633074000
_diffrn_orient_matrix_UB_23      0.0523368000
_diffrn_orient_matrix_UB_31      0.0190040000
_diffrn_orient_matrix_UB_32      0.0189293000
_diffrn_orient_matrix_UB_33      0.0699072000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       63
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            51037
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.432
_diffrn_reflns_theta_min         3.515
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       block
_exptl_crystal_F_000             5568
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     895
_refine_ls_number_reflns         14345
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0672
_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)+(0.0826P)²+9.9015P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1665
_refine_ls_wR_factor_ref         0.1917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9450
_reflns_number_total             14345
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jo0c00220_si_002.cif
_cod_data_source_block           ABC10
_cod_database_code               4038157
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H30 N1 O9'
_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   0.965
_shelx_estimated_absorpt_t_min   0.929
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O15-C78
 1.23 with sigma of 0.01
 O16-C78
 1.23 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C70) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C80) = Uanis(O16) = Uanis(C78) = Uanis(C79) = Uanis(O15) = Uanis(C84) =
Uanis(C83) = Uanis(C81) = Uanis(C82)
4. Others
 Fixed Sof: C66(0.5) H66(0.5) C67(0.5) H67(0.5) C68(0.5) H68(0.5) C69(0.5)
 H69(0.5) C70(0.5) H70(0.5) N2(0.5) H2A(0.5) C78(0.5) C79(0.5) H79(0.5)
 C80(0.5) H80A(0.5) H80B(0.5) C81(0.5) H81A(0.5) H81B(0.5) C82(0.5) H82A(0.5)
 H82B(0.5) C83(0.5) H83A(0.5) H83B(0.5) C84(0.5) H84A(0.5) H84B(0.5) O15(0.5)
 O16(0.5)
5.a Riding coordinates:
 N1(H1A)
5.b Ternary CH refined with riding coordinates:
 C8(H8), C18(H18), C28(H28), C38(H38), C48(H48), C58(H58), C72(H72), C79(H79)
5.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C19(H19A,H19B), C29(H29A,H29B), C39(H39A,H39B), C49(H49A,H49B),
 C59(H59A,H59B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B),
  C77(H77A,H77B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,
 H83B), C84(H84A,H84B)
5.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C14(H14), C24(H24), C34(H34), C44(H44), C54(H54), C61(H61), C62(H62),
 C63(H63), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70),
  N2(H2A)
5.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C17(H17A,H17B,H17C), C20(H20A,H20B,
 H20C), C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C37(H37A,H37B,H37C), C40(H40A,
 H40B,H40C), C47(H47A,H47B,H47C), C50(H50A,H50B,H50C), C57(H57A,H57B,H57C),
 C60(H60A,H60B,H60C)
5.f Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O3(H3), O4(H4A), O5(H5), O6(H6), O7(H7), O8(H8A), O9(H9),
 O10(H10), O11(H11), O12(H12)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.202
_oxdiff_exptl_absorpt_empirical_full_min 0.893
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, 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
C1 C 0.86194(5) 0.85834(17) 0.48987(19) 0.0349(6) Uani 1 1 d . . . . .
C2 C 0.88142(5) 0.83079(17) 0.43729(19) 0.0334(6) Uani 1 1 d . . . . .
C3 C 0.87933(5) 0.75700(17) 0.39582(17) 0.0303(6) Uani 1 1 d . . . . .
C4 C 0.85654(5) 0.71070(16) 0.41025(16) 0.0280(5) Uani 1 1 d . . . . .
H4 H 0.854539 0.661716 0.382878 0.034 Uiso 1 1 calc R . . . .
C5 C 0.83668(5) 0.73409(16) 0.46351(17) 0.0293(5) Uani 1 1 d . . . . .
C6 C 0.83958(5) 0.80914(17) 0.50230(18) 0.0326(6) Uani 1 1 d . . . . .
C7 C 0.86437(6) 0.93939(19) 0.5316(2) 0.0461(8) Uani 1 1 d . . . . .
H7A H 0.870941 0.931180 0.584957 0.069 Uiso 1 1 calc GR . . . .
H7B H 0.847237 0.965078 0.533885 0.069 Uiso 1 1 calc GR . . . .
H7C H 0.876484 0.973569 0.502487 0.069 Uiso 1 1 calc GR . . . .
C8 C 0.90102(5) 0.73043(17) 0.33851(18) 0.0318(6) Uani 1 1 d . . . . .
H8 H 0.917613 0.754354 0.358357 0.038 Uiso 1 1 calc R . . . .
C9 C 0.90529(5) 0.63759(18) 0.33666(19) 0.0370(6) Uani 1 1 d . . . . .
H9A H 0.888684 0.611025 0.322830 0.044 Uiso 1 1 calc R . . . .
H9B H 0.918210 0.624361 0.295520 0.044 Uiso 1 1 calc R . . . .
C10 C 0.91504(7) 0.6051(2) 0.4169(2) 0.0537(9) Uani 1 1 d . . . . .
H10A H 0.918332 0.547656 0.412605 0.081 Uiso 1 1 calc GR . . . .
H10B H 0.901741 0.614702 0.457073 0.081 Uiso 1 1 calc GR . . . .
H10C H 0.931177 0.632534 0.431619 0.081 Uiso 1 1 calc GR . . . .
C11 C 0.90691(5) 0.86438(17) 0.15004(19) 0.0329(6) Uani 1 1 d . . . . .
C12 C 0.88976(5) 0.82352(17) 0.09926(18) 0.0325(6) Uani 1 1 d . . . . .
C13 C 0.87513(5) 0.75574(16) 0.12385(17) 0.0298(5) Uani 1 1 d . . . . .
C14 C 0.87887(5) 0.72844(16) 0.20149(17) 0.0298(5) Uani 1 1 d . . . . .
H14 H 0.869178 0.683519 0.218847 0.036 Uiso 1 1 calc R . . . .
C15 C 0.89656(5) 0.76531(17) 0.25501(18) 0.0311(6) Uani 1 1 d . . . . .
C16 C 0.91001(5) 0.83487(18) 0.22829(19) 0.0337(6) Uani 1 1 d . . . . .
C17 C 0.92194(6) 0.93978(18) 0.1242(2) 0.0400(7) Uani 1 1 d . . . . .
H17A H 0.940591 0.927696 0.121414 0.060 Uiso 1 1 calc GR . . . .
H17B H 0.919017 0.982612 0.162410 0.060 Uiso 1 1 calc GR . . . .
H17C H 0.915741 0.956894 0.072526 0.060 Uiso 1 1 calc GR . . . .
C18 C 0.85572(5) 0.71359(16) 0.06694(17) 0.0306(6) Uani 1 1 d . . . . .
H18 H 0.859820 0.733707 0.013073 0.037 Uiso 1 1 calc R . . . .
C19 C 0.85985(6) 0.62073(17) 0.06481(19) 0.0358(6) Uani 1 1 d . . . . .
H19A H 0.857421 0.598687 0.118210 0.043 Uiso 1 1 calc R . . . .
H19B H 0.846609 0.596263 0.030082 0.043 Uiso 1 1 calc R . . . .
C20 C 0.88765(6) 0.5986(2) 0.0345(2) 0.0480(8) Uani 1 1 d . . . . .
H20A H 0.890056 0.620082 -0.018525 0.072 Uiso 1 1 calc GR . . . .
H20B H 0.889534 0.540395 0.033250 0.072 Uiso 1 1 calc GR . . . .
H20C H 0.900781 0.621453 0.069622 0.072 Uiso 1 1 calc GR . . . .
C21 C 0.79142(5) 0.83904(17) 0.07011(17) 0.0321(6) Uani 1 1 d . . . . .
C22 C 0.77578(5) 0.79148(17) 0.12071(16) 0.0295(5) Uani 1 1 d . . . . .
C23 C 0.78468(5) 0.71831(16) 0.15368(15) 0.0266(5) Uani 1 1 d . . . . .
C24 C 0.81071(5) 0.69447(16) 0.13500(16) 0.0278(5) Uani 1 1 d . . . . .
H24 H 0.817243 0.646437 0.157076 0.033 Uiso 1 1 calc R . . . .
C25 C 0.82721(5) 0.73953(16) 0.08488(16) 0.0282(5) Uani 1 1 d . . . . .
C26 C 0.81714(5) 0.81206(17) 0.05293(17) 0.0316(6) Uani 1 1 d . . . . .
C27 C 0.78111(6) 0.9174(2) 0.0348(2) 0.0471(8) Uani 1 1 d . . . . .
H27A H 0.775522 0.908111 -0.019393 0.071 Uiso 1 1 calc GR . . . .
H27B H 0.794962 0.957709 0.035487 0.071 Uiso 1 1 calc GR . . . .
H27C H 0.766290 0.936457 0.065849 0.071 Uiso 1 1 calc GR . . . .
C28 C 0.76641(5) 0.66748(16) 0.20719(16) 0.0275(5) Uani 1 1 d . . . . .
H28 H 0.748240 0.677514 0.188402 0.033 Uiso 1 1 calc R . . . .
C29 C 0.77103(5) 0.57525(16) 0.19996(18) 0.0335(6) Uani 1 1 d . . . . .
H29A H 0.770930 0.560098 0.143807 0.040 Uiso 1 1 calc R . . . .
H29B H 0.788406 0.562009 0.221562 0.040 Uiso 1 1 calc R . . . .
C30 C 0.74988(7) 0.52571(19) 0.2443(2) 0.0469(8) Uani 1 1 d . . . . .
H30A H 0.732590 0.539758 0.224171 0.070 Uiso 1 1 calc GR . . . .
H30B H 0.750737 0.537647 0.300485 0.070 Uiso 1 1 calc GR . . . .
H30C H 0.753037 0.468635 0.235924 0.070 Uiso 1 1 calc GR . . . .
C31 C 0.74887(5) 0.78142(17) 0.40100(17) 0.0310(6) Uani 1 1 d . . . . .
C32 C 0.76971(5) 0.75583(16) 0.45043(16) 0.0294(5) Uani 1 1 d . . . . .
C33 C 0.78945(5) 0.70236(15) 0.42400(16) 0.0264(5) Uani 1 1 d . . . . .
C34 C 0.78789(5) 0.67472(14) 0.34525(16) 0.0253(5) Uani 1 1 d . . . . .
H34 H 0.801004 0.639624 0.326472 0.030 Uiso 1 1 calc R . . . .
C35 C 0.76749(5) 0.69754(15) 0.29351(16) 0.0261(5) Uani 1 1 d . . . . .
C36 C 0.74821(5) 0.75137(16) 0.32327(16) 0.0275(5) Uani 1 1 d . . . . .
C37 C 0.72839(6) 0.8408(2) 0.43114(19) 0.0424(7) Uani 1 1 d . . . . .
H37A H 0.723929 0.878481 0.389235 0.064 Uiso 1 1 calc GR . . . .
H37B H 0.735454 0.870185 0.476089 0.064 Uiso 1 1 calc GR . . . .
H37C H 0.712728 0.811712 0.447305 0.064 Uiso 1 1 calc GR . . . .
C38 C 0.81258(5) 0.68003(15) 0.47899(16) 0.0257(5) Uani 1 1 d . . . . .
H38 H 0.806687 0.691866 0.533712 0.031 Uiso 1 1 calc R . . . .
C39 C 0.81921(5) 0.58847(15) 0.47658(17) 0.0291(5) Uani 1 1 d . . . . .
H39A H 0.823993 0.573260 0.422327 0.035 Uiso 1 1 calc R . . . .
H39B H 0.834426 0.577954 0.510741 0.035 Uiso 1 1 calc R . . . .
C40 C 0.79597(6) 0.53649(17) 0.50412(19) 0.0366(6) Uani 1 1 d . . . . .
H40A H 0.781510 0.542158 0.467008 0.055 Uiso 1 1 calc GR . . . .
H40B H 0.790348 0.554024 0.556286 0.055 Uiso 1 1 calc GR . . . .
H40C H 0.801369 0.480421 0.506467 0.055 Uiso 1 1 calc GR . . . .
O1 O 0.82130(4) 0.83894(13) 0.55571(15) 0.0434(5) Uani 1 1 d . . . . .
H1 H 0.806406 0.823057 0.543197 0.065 Uiso 1 1 calc GR . . . .
O2 O 0.90380(4) 0.87958(13) 0.42380(14) 0.0405(5) Uani 1 1 d . . . . .
H2 H 0.913538 0.878016 0.463164 0.061 Uiso 1 1 calc GR . . . .
O3 O 0.92689(4) 0.87780(14) 0.27688(14) 0.0432(5) Uani 1 1 d . . . . .
H3 H 0.921318 0.876705 0.323022 0.065 Uiso 1 1 calc GR . . . .
O4 O 0.88561(4) 0.85173(13) 0.02202(13) 0.0373(5) Uani 1 1 d . . . . .
H4A H 0.899928 0.855853 -0.001103 0.056 Uiso 1 1 calc GR . . . .
O5 O 0.83147(4) 0.86169(14) 0.00281(14) 0.0412(5) Uani 1 1 d . . . . .
H5 H 0.847295 0.850086 0.005930 0.062 Uiso 1 1 calc GR . . . .
O6 O 0.74992(4) 0.81837(12) 0.13199(12) 0.0331(4) Uani 1 1 d . . . . .
H6 H 0.744808 0.805109 0.176764 0.050 Uiso 1 1 calc GR . . . .
O7 O 0.72877(3) 0.78021(13) 0.27171(12) 0.0341(4) Uani 1 1 d . . . . .
H7 H 0.714853 0.755397 0.279550 0.051 Uiso 1 1 calc GR . . . .
O8 O 0.77120(4) 0.78851(12) 0.52681(12) 0.0339(4) Uani 1 1 d . . . . .
H8A H 0.766839 0.753863 0.559676 0.051 Uiso 1 1 calc GR . . . .
C01L C 0.93439(6) 0.8030(2) -0.1181(2) 0.0412(7) Uani 1 1 d . . . . .
C42 C 0.91833(6) 0.7937(2) -0.2522(2) 0.0423(7) Uani 1 1 d . . . . .
C43 C 0.93521(5) 0.72780(19) -0.2680(2) 0.0389(7) Uani 1 1 d . . . . .
C44 C 0.95058(5) 0.69932(19) -0.2052(2) 0.0413(7) Uani 1 1 d . . . . .
H44 H 0.961789 0.655203 -0.214325 0.050 Uiso 1 1 calc R . . . .
C45 C 0.95003(5) 0.73363(19) -0.1291(2) 0.0404(7) Uani 1 1 d . . . . .
C46 C 0.91823(6) 0.83389(19) -0.1787(2) 0.0427(7) Uani 1 1 d . . . . .
C47 C 0.90251(7) 0.9110(2) -0.1649(2) 0.0503(8) Uani 1 1 d . . . . .
H47A H 0.886178 0.898021 -0.138045 0.075 Uiso 1 1 calc GR . . . .
H47B H 0.898647 0.936226 -0.215474 0.075 Uiso 1 1 calc GR . . . .
H47C H 0.912721 0.947802 -0.132474 0.075 Uiso 1 1 calc GR . . . .
C48 C 0.96567(6) 0.6969(2) -0.0594(2) 0.0455(8) Uani 1 1 d . . . . .
H48 H 0.956644 0.714595 -0.010342 0.055 Uiso 1 1 calc R . . . .
C49 C 0.96453(7) 0.6029(2) -0.0597(3) 0.0564(10) Uani 1 1 d . . . . .
H49A H 0.946504 0.585461 -0.071156 0.068 Uiso 1 1 calc R . . . .
H49B H 0.975989 0.582210 -0.101723 0.068 Uiso 1 1 calc R . . . .
C50 C 0.97316(9) 0.5679(3) 0.0195(3) 0.0830(15) Uani 1 1 d . . . . .
H50A H 0.973918 0.509592 0.015619 0.125 Uiso 1 1 calc GR . . . .
H50B H 0.960644 0.583183 0.060198 0.125 Uiso 1 1 calc GR . . . .
H50C H 0.990433 0.588658 0.033059 0.125 Uiso 1 1 calc GR . . . .
C51 C 1.02414(6) 0.8377(2) -0.0092(2) 0.0491(8) Uani 1 1 d . . . . .
C52 C 0.99933(6) 0.7992(2) -0.0092(2) 0.0482(8) Uani 1 1 d . . . . .
C53 C 0.99376(6) 0.7319(2) -0.0554(2) 0.0446(8) Uani 1 1 d . . . . .
C54 C 1.01456(6) 0.6992(2) -0.1008(2) 0.0448(7) Uani 1 1 d . . . . .
H54 H 1.011209 0.653625 -0.132284 0.054 Uiso 1 1 calc R . . . .
C55 C 1.04018(6) 0.7322(2) -0.1007(2) 0.0423(7) Uani 1 1 d . . . . .
C56 C 1.04422(6) 0.8027(2) -0.0566(2) 0.0455(8) Uani 1 1 d . . . . .
C57 C 1.02910(7) 0.9145(3) 0.0380(3) 0.0640(11) Uani 1 1 d . . . . .
H57A H 1.012615 0.942935 0.045656 0.096 Uiso 1 1 calc GR . . . .
H57B H 1.041291 0.948718 0.009280 0.096 Uiso 1 1 calc GR . . . .
H57C H 1.036551 0.900683 0.089175 0.096 Uiso 1 1 calc GR . . . .
C58 C 1.06274(6) 0.6914(2) -0.1480(2) 0.0439(7) Uani 1 1 d . . . . .
H58 H 1.079318 0.705367 -0.120365 0.053 Uiso 1 1 calc R . . . .
C59 C 1.06062(6) 0.5984(2) -0.1465(2) 0.0494(8) Uani 1 1 d . . . . .
H59A H 1.058995 0.580297 -0.091394 0.059 Uiso 1 1 calc R . . . .
H59B H 1.044645 0.581944 -0.174744 0.059 Uiso 1 1 calc R . . . .
C60 C 1.08447(7) 0.5572(3) -0.1845(3) 0.0681(12) Uani 1 1 d . . . . .
H60A H 1.085716 0.573060 -0.239729 0.102 Uiso 1 1 calc GR . . . .
H60B H 1.082437 0.499139 -0.181068 0.102 Uiso 1 1 calc GR . . . .
H60C H 1.100345 0.573352 -0.156821 0.102 Uiso 1 1 calc GR . . . .
O9 O 0.90279(4) 0.82215(15) -0.31431(15) 0.0485(6) Uani 1 1 d . . . . .
H9 H 0.887420 0.827634 -0.298797 0.073 Uiso 1 1 calc GR . . . .
O10 O 0.93374(4) 0.84500(16) -0.04644(15) 0.0479(6) Uani 1 1 d . . . . .
H10 H 0.947078 0.834166 -0.020299 0.072 Uiso 1 1 calc GR . . . .
O11 O 0.97887(4) 0.83179(18) 0.03663(18) 0.0588(7) Uani 1 1 d . . . . .
H11 H 0.984774 0.846723 0.079998 0.088 Uiso 1 1 calc GR . . . .
O12 O 1.06839(4) 0.84332(17) -0.05557(16) 0.0523(6) Uani 1 1 d . . . . .
H12 H 1.076318 0.834756 -0.097655 0.078 Uiso 1 1 calc GR . . . .
C61 C 0.81975(7) 1.0181(2) 0.3396(2) 0.0489(8) Uani 1 1 d . . . . .
H61 H 0.817260 1.065730 0.368925 0.059 Uiso 1 1 calc R . . . .
C62 C 0.80869(8) 0.9465(2) 0.3653(2) 0.0558(9) Uani 1 1 d . . . . .
H62 H 0.798649 0.944690 0.412035 0.067 Uiso 1 1 calc R . . . .
C63 C 0.81275(7) 0.87701(19) 0.3203(2) 0.0467(8) Uani 1 1 d . . . . .
H63 H 0.805195 0.827966 0.336508 0.056 Uiso 1 1 calc R . . . .
C64 C 0.82757(8) 0.8797(2) 0.2533(2) 0.0507(8) Uani 1 1 d . . . . .
H64 H 0.830458 0.832864 0.223201 0.061 Uiso 1 1 calc R . . . .
C65 C 0.83836(7) 0.9530(2) 0.2302(2) 0.0543(9) Uani 1 1 d . . . . .
H65 H 0.848772 0.955964 0.184239 0.065 Uiso 1 1 calc R . . . .
N1 N 0.83395(5) 1.01949(15) 0.27321(18) 0.0448(6) Uani 1 1 d . . . . .
H1A H 0.839955 1.065958 0.255531 0.054 Uiso 1 1 d R . . . .
C66 C 1.02182(17) 1.0058(8) 0.2445(8) 0.086(5) Uani 0.5 1 d . . P A -1
H66 H 1.035638 0.968838 0.237125 0.103 Uiso 0.5 1 calc R . P A -1
C67 C 1.0270(2) 1.0802(8) 0.2752(10) 0.087(4) Uani 0.5 1 d . . P A -1
H67 H 1.043906 1.092618 0.294502 0.105 Uiso 0.5 1 calc R . P A -1
C68 C 1.0071(2) 1.1369(6) 0.2777(7) 0.065(3) Uani 0.5 1 d . . P A -1
H68 H 1.010736 1.189882 0.294132 0.078 Uiso 0.5 1 calc R . P A -1
C69 C 0.9835(2) 1.1164(7) 0.2570(8) 0.071(3) Uani 0.5 1 d . . P A -1
H69 H 0.969789 1.154452 0.260356 0.085 Uiso 0.5 1 calc R . P A -1
C70 C 0.9779(3) 1.0362(11) 0.2292(9) 0.085(4) Uani 0.5 1 d . U P A -1
H70 H 0.960732 1.021136 0.214568 0.103 Uiso 0.5 1 calc R . P A -1
N2 N 0.99735(15) 0.9848(3) 0.2247(4) 0.0567(17) Uani 0.5 1 d . . P A -1
H2A H 0.994270 0.935971 0.208451 0.068 Uiso 0.5 1 calc R . P A -1
C71 C 0.83801(6) 1.21652(18) 0.2532(2) 0.0405(7) Uani 1 1 d . . . . .
C72 C 0.84750(6) 1.30533(18) 0.2504(2) 0.0384(6) Uani 1 1 d . . . . .
H72 H 0.865677 1.306416 0.229299 0.046 Uiso 1 1 calc R . . . .
C73 C 0.82982(6) 1.35528(18) 0.1954(2) 0.0402(7) Uani 1 1 d . . . . .
H73A H 0.811482 1.350239 0.212687 0.048 Uiso 1 1 calc R . . . .
H73B H 0.831065 1.333893 0.141335 0.048 Uiso 1 1 calc R . . . .
C74 C 0.83769(6) 1.44514(18) 0.19508(19) 0.0384(6) Uani 1 1 d . . . . .
H74A H 0.855308 1.450967 0.172125 0.046 Uiso 1 1 calc R . . . .
H74B H 0.825328 1.475610 0.162039 0.046 Uiso 1 1 calc R . . . .
C75 C 0.83758(6) 1.47955(18) 0.2791(2) 0.0425(7) Uani 1 1 d . . . . .
H75A H 0.843449 1.535845 0.277655 0.051 Uiso 1 1 calc R . . . .
H75B H 0.819586 1.478591 0.300005 0.051 Uiso 1 1 calc R . . . .
C76 C 0.85554(7) 1.4315(2) 0.3342(2) 0.0459(7) Uani 1 1 d . . . . .
H76A H 0.854292 1.453396 0.388085 0.055 Uiso 1 1 calc R . . . .
H76B H 0.873822 1.436966 0.316536 0.055 Uiso 1 1 calc R . . . .
C77 C 0.84776(7) 1.3409(2) 0.3351(2) 0.0456(7) Uani 1 1 d . . . . .
H77A H 0.860313 1.310779 0.367792 0.055 Uiso 1 1 calc R . . . .
H77B H 0.830262 1.334921 0.358827 0.055 Uiso 1 1 calc R . . . .
O13 O 0.85449(4) 1.16158(13) 0.23469(16) 0.0483(6) Uani 1 1 d . . . . .
O14 O 0.81487(5) 1.19953(14) 0.27526(18) 0.0564(7) Uani 1 1 d . . . . .
C78 C 1.0014(2) 0.7914(4) 0.2650(4) 0.0570(7) Uani 0.5 1 d D . P B -1
C79 C 1.00440(15) 0.7009(5) 0.2832(5) 0.0570(7) Uani 0.5 1 d . . P B -1
H79 H 1.012132 0.698047 0.336983 0.068 Uiso 0.5 1 calc R . P B -1
C80 C 0.9784(3) 0.6627(7) 0.2897(7) 0.0570(7) Uani 0.5 1 d . . P B -1
H80A H 0.968308 0.674076 0.241506 0.068 Uiso 0.5 1 calc R . P B -1
H80B H 0.968947 0.686429 0.334584 0.068 Uiso 0.5 1 calc R . P B -1
C81 C 0.98015(16) 0.5694(5) 0.3015(5) 0.0570(7) Uani 0.5 1 d . . P B -1
H81A H 0.962499 0.546008 0.297001 0.068 Uiso 0.5 1 calc R . P B -1
H81B H 0.986779 0.557832 0.354879 0.068 Uiso 0.5 1 calc R . P B -1
C82 C 0.9992(3) 0.5284(4) 0.2372(6) 0.0570(7) Uani 0.5 1 d . . P B -1
H82A H 1.001283 0.470873 0.248779 0.068 Uiso 0.5 1 calc R . P B -1
H82B H 0.991587 0.533874 0.184030 0.068 Uiso 0.5 1 calc R . P B -1
C83 C 1.02542(16) 0.5700(5) 0.2405(6) 0.0570(7) Uani 0.5 1 d . . P B -1
H83A H 1.033708 0.558406 0.291747 0.068 Uiso 0.5 1 calc R . P B -1
H83B H 1.036792 0.547916 0.198911 0.068 Uiso 0.5 1 calc R . P B -1
C84 C 1.0235(3) 0.6582(7) 0.2303(6) 0.0570(7) Uani 0.5 1 d . . P B -1
H84A H 1.018549 0.669197 0.175198 0.068 Uiso 0.5 1 calc R . P B -1
H84B H 1.040960 0.681497 0.238925 0.068 Uiso 0.5 1 calc R . P B -1
O15 O 0.99225(13) 0.8169(3) 0.1992(4) 0.0570(7) Uani 0.5 1 d D . P B -1
O16 O 1.00848(13) 0.8415(3) 0.3197(4) 0.0570(7) Uani 0.5 1 d D . P B -1
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'
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
25 6 -4 0.0207
-24 -6 4 0.0322
-2 -3 10 0.0302
-1 2 -11 0.0267
32 -3 -1 0.0301
-30 3 3 0.0171
-20 -2 -8 0.0262
20 2 8 0.0459
24 -5 5 0.0267
2 -9 -5 0.0411
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
C2 C1 C6 118.2(3) . . ?
C2 C1 C7 121.4(3) . . ?
C6 C1 C7 120.4(3) . . ?
C1 C2 C3 122.7(2) . . ?
C1 C2 O2 118.8(3) . . ?
C3 C2 O2 118.4(3) . . ?
C2 C3 C8 120.5(2) . . ?
C4 C3 C2 116.6(2) . . ?
C4 C3 C8 122.9(2) . . ?
C3 C4 H4 118.3 . . ?
C5 C4 C3 123.3(3) . . ?
C5 C4 H4 118.3 . . ?
C4 C5 C6 117.6(2) . . ?
C4 C5 C38 121.3(2) . . ?
C6 C5 C38 121.1(2) . . ?
C5 C6 C1 121.5(3) . . ?
O1 C6 C1 115.4(2) . . ?
O1 C6 C5 123.0(2) . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C3 C8 H8 106.5 . . ?
C3 C8 C9 113.5(2) . . ?
C3 C8 C15 111.3(2) . . ?
C9 C8 H8 106.5 . . ?
C15 C8 H8 106.5 . . ?
C15 C8 C9 112.0(2) . . ?
C8 C9 H9A 109.2 . . ?
C8 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C10 C9 C8 111.9(3) . . ?
C10 C9 H9A 109.2 . . ?
C10 C9 H9B 109.2 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C16 118.2(3) . . ?
C12 C11 C17 122.2(3) . . ?
C16 C11 C17 119.5(3) . . ?
C11 C12 C13 122.3(3) . . ?
C11 C12 O4 120.2(2) . . ?
O4 C12 C13 117.4(3) . . ?
C12 C13 C18 121.0(3) . . ?
C14 C13 C12 117.5(3) . . ?
C14 C13 C18 121.5(2) . . ?
C13 C14 H14 118.5 . . ?
C13 C14 C15 123.0(3) . . ?
C15 C14 H14 118.5 . . ?
C14 C15 C8 121.1(2) . . ?
C14 C15 C16 117.2(3) . . ?
C16 C15 C8 121.8(2) . . ?
C15 C16 C11 121.7(3) . . ?
O3 C16 C11 116.3(2) . . ?
O3 C16 C15 122.0(3) . . ?
C11 C17 H17A 109.5 . . ?
C11 C17 H17B 109.5 . . ?
C11 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C13 C18 H18 106.5 . . ?
C13 C18 C19 112.1(2) . . ?
C19 C18 H18 106.5 . . ?
C25 C18 C13 110.6(2) . . ?
C25 C18 H18 106.5 . . ?
C25 C18 C19 114.1(2) . . ?
C18 C19 H19A 109.3 . . ?
C18 C19 H19B 109.3 . . ?
H19A C19 H19B 108.0 . . ?
C20 C19 C18 111.5(2) . . ?
C20 C19 H19A 109.3 . . ?
C20 C19 H19B 109.3 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C26 118.0(3) . . ?
C22 C21 C27 121.4(2) . . ?
C26 C21 C27 120.6(2) . . ?
C21 C22 C23 122.7(2) . . ?
O6 C22 C21 115.7(2) . . ?
O6 C22 C23 121.4(2) . . ?
C22 C23 C24 116.9(2) . . ?
C22 C23 C28 120.5(2) . . ?
C24 C23 C28 122.6(2) . . ?
C23 C24 H24 118.6 . . ?
C25 C24 C23 122.9(2) . . ?
C25 C24 H24 118.6 . . ?
C24 C25 C18 122.0(2) . . ?
C24 C25 C26 117.7(2) . . ?
C26 C25 C18 120.2(2) . . ?
C21 C26 C25 121.8(2) . . ?
O5 C26 C21 115.1(2) . . ?
O5 C26 C25 123.2(2) . . ?
C21 C27 H27A 109.5 . . ?
C21 C27 H27B 109.5 . . ?
C21 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C23 C28 H28 106.3 . . ?
C23 C28 C29 113.6(2) . . ?
C29 C28 H28 106.3 . . ?
C35 C28 C23 110.8(2) . . ?
C35 C28 H28 106.3 . . ?
C35 C28 C29 112.8(2) . . ?
C28 C29 H29A 109.1 . . ?
C28 C29 H29B 109.1 . . ?
H29A C29 H29B 107.9 . . ?
C30 C29 C28 112.4(2) . . ?
C30 C29 H29A 109.1 . . ?
C30 C29 H29B 109.1 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C37 120.7(3) . . ?
C36 C31 C32 117.6(2) . . ?
C36 C31 C37 121.7(3) . . ?
C33 C32 C31 122.3(3) . . ?
O8 C32 C31 117.9(2) . . ?
O8 C32 C33 119.7(2) . . ?
C32 C33 C38 120.2(2) . . ?
C34 C33 C32 117.6(2) . . ?
C34 C33 C38 122.2(2) . . ?
C33 C34 H34 118.7 . . ?
C35 C34 C33 122.7(2) . . ?
C35 C34 H34 118.7 . . ?
C34 C35 C28 121.7(2) . . ?
C34 C35 C36 117.3(2) . . ?
C36 C35 C28 120.9(2) . . ?
C31 C36 C35 122.6(2) . . ?
O7 C36 C31 118.4(2) . . ?
O7 C36 C35 118.9(2) . . ?
C31 C37 H37A 109.5 . . ?
C31 C37 H37B 109.5 . . ?
C31 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C5 C38 C33 111.4(2) . . ?
C5 C38 H38 106.4 . . ?
C5 C38 C39 113.0(2) . . ?
C33 C38 H38 106.4 . . ?
C33 C38 C39 112.6(2) . . ?
C39 C38 H38 106.4 . . ?
C38 C39 H39A 109.2 . . ?
C38 C39 H39B 109.2 . . ?
H39A C39 H39B 107.9 . . ?
C40 C39 C38 111.9(2) . . ?
C40 C39 H39A 109.2 . . ?
C40 C39 H39B 109.2 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C6 O1 H1 109.5 . . ?
C2 O2 H2 109.5 . . ?
C16 O3 H3 109.5 . . ?
C12 O4 H4A 109.5 . . ?
C26 O5 H5 109.5 . . ?
C22 O6 H6 109.5 . . ?
C36 O7 H7 109.5 . . ?
C32 O8 H8A 109.5 . . ?
C46 C01L C45 122.0(3) . . ?
O10 C01L C45 122.3(3) . . ?
O10 C01L C46 115.7(3) . . ?
C46 C42 C43 122.3(3) . . ?
O9 C42 C43 117.5(3) . . ?
O9 C42 C46 120.0(3) . . ?
C42 C43 C58 121.1(3) . 3_754 ?
C44 C43 C42 117.1(3) . . ?
C44 C43 C58 121.7(3) . 3_754 ?
C43 C44 H44 118.5 . . ?
C43 C44 C45 123.0(3) . . ?
C45 C44 H44 118.5 . . ?
C01L C45 C48 120.8(3) . . ?
C44 C45 C01L 117.5(3) . . ?
C44 C45 C48 121.8(3) . . ?
C01L C46 C47 120.0(3) . . ?
C42 C46 C01L 117.7(3) . . ?
C42 C46 C47 122.2(3) . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C48 H48 106.3 . . ?
C45 C48 C49 111.9(3) . . ?
C49 C48 H48 106.3 . . ?
C53 C48 C45 111.1(3) . . ?
C53 C48 H48 106.3 . . ?
C53 C48 C49 114.2(3) . . ?
C48 C49 H49A 109.3 . . ?
C48 C49 H49B 109.3 . . ?
H49A C49 H49B 108.0 . . ?
C50 C49 C48 111.6(4) . . ?
C50 C49 H49A 109.3 . . ?
C50 C49 H49B 109.3 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C52 C51 C56 117.2(3) . . ?
C52 C51 C57 121.6(3) . . ?
C56 C51 C57 121.1(3) . . ?
C53 C52 C51 122.9(3) . . ?
C53 C52 O11 117.8(3) . . ?
O11 C52 C51 119.2(3) . . ?
C52 C53 C48 121.0(3) . . ?
C52 C53 C54 117.3(3) . . ?
C54 C53 C48 121.7(3) . . ?
C53 C54 H54 118.6 . . ?
C55 C54 C53 122.7(3) . . ?
C55 C54 H54 118.6 . . ?
C54 C55 C58 120.8(3) . . ?
C56 C55 C54 117.3(3) . . ?
C56 C55 C58 121.9(3) . . ?
C55 C56 C51 122.3(3) . . ?
O12 C56 C51 115.3(3) . . ?
O12 C56 C55 122.4(3) . . ?
C51 C57 H57A 109.5 . . ?
C51 C57 H57B 109.5 . . ?
C51 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C43 C58 C55 110.6(3) 3_754 . ?
C43 C58 H58 106.5 3_754 . ?
C43 C58 C59 114.2(3) 3_754 . ?
C55 C58 H58 106.5 . . ?
C59 C58 C55 112.0(3) . . ?
C59 C58 H58 106.5 . . ?
C58 C59 H59A 109.1 . . ?
C58 C59 H59B 109.1 . . ?
H59A C59 H59B 107.8 . . ?
C60 C59 C58 112.5(3) . . ?
C60 C59 H59A 109.1 . . ?
C60 C59 H59B 109.1 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C42 O9 H9 109.5 . . ?
C01L O10 H10 109.5 . . ?
C52 O11 H11 109.5 . . ?
C56 O12 H12 109.5 . . ?
C62 C61 H61 120.1 . . ?
N1 C61 H61 120.1 . . ?
N1 C61 C62 119.8(3) . . ?
C61 C62 H62 120.7 . . ?
C61 C62 C63 118.6(3) . . ?
C63 C62 H62 120.7 . . ?
C62 C63 H63 119.8 . . ?
C64 C63 C62 120.5(3) . . ?
C64 C63 H63 119.8 . . ?
C63 C64 H64 120.6 . . ?
C63 C64 C65 118.8(3) . . ?
C65 C64 H64 120.6 . . ?
C64 C65 H65 119.9 . . ?
N1 C65 C64 120.1(3) . . ?
N1 C65 H65 119.9 . . ?
C61 N1 C65 122.2(3) . . ?
C61 N1 H1A 119.1 . . ?
C65 N1 H1A 118.6 . . ?
C67 C66 H66 119.6 . . ?
N2 C66 H66 119.6 . . ?
N2 C66 C67 120.8(9) . . ?
C66 C67 H67 120.5 . . ?
C66 C67 C68 119.0(12) . . ?
C68 C67 H67 120.5 . . ?
C67 C68 H68 120.2 . . ?
C69 C68 C67 119.5(11) . . ?
C69 C68 H68 120.2 . . ?
C68 C69 H69 119.6 . . ?
C68 C69 C70 120.8(11) . . ?
C70 C69 H69 119.6 . . ?
C69 C70 H70 120.9 . . ?
N2 C70 C69 118.2(10) . . ?
N2 C70 H70 120.9 . . ?
C66 N2 H2A 119.3 . . ?
C70 N2 C66 121.4(9) . . ?
C70 N2 H2A 119.3 . . ?
O13 C71 C72 117.8(3) . . ?
O14 C71 C72 120.6(3) . . ?
O14 C71 O13 121.5(3) . . ?
C71 C72 H72 108.6 . . ?
C73 C72 C71 110.4(3) . . ?
C73 C72 H72 108.6 . . ?
C73 C72 C77 111.0(3) . . ?
C77 C72 C71 109.7(3) . . ?
C77 C72 H72 108.6 . . ?
C72 C73 H73A 109.3 . . ?
C72 C73 H73B 109.3 . . ?
C72 C73 C74 111.8(3) . . ?
H73A C73 H73B 107.9 . . ?
C74 C73 H73A 109.3 . . ?
C74 C73 H73B 109.3 . . ?
C73 C74 H74A 109.5 . . ?
C73 C74 H74B 109.5 . . ?
H74A C74 H74B 108.0 . . ?
C75 C74 C73 110.9(3) . . ?
C75 C74 H74A 109.5 . . ?
C75 C74 H74B 109.5 . . ?
C74 C75 H75A 109.3 . . ?
C74 C75 H75B 109.3 . . ?
H75A C75 H75B 108.0 . . ?
C76 C75 C74 111.6(3) . . ?
C76 C75 H75A 109.3 . . ?
C76 C75 H75B 109.3 . . ?
C75 C76 H76A 109.4 . . ?
C75 C76 H76B 109.4 . . ?
C75 C76 C77 111.0(3) . . ?
H76A C76 H76B 108.0 . . ?
C77 C76 H76A 109.4 . . ?
C77 C76 H76B 109.4 . . ?
C72 C77 C76 111.3(3) . . ?
C72 C77 H77A 109.4 . . ?
C72 C77 H77B 109.4 . . ?
C76 C77 H77A 109.4 . . ?
C76 C77 H77B 109.4 . . ?
H77A C77 H77B 108.0 . . ?
O15 C78 C79 122.1(6) . . ?
O15 C78 O16 120.6(6) . . ?
O16 C78 C79 117.2(6) . . ?
C78 C79 H79 105.5 . . ?
C80 C79 C78 110.3(8) . . ?
C80 C79 H79 105.5 . . ?
C80 C79 C84 115.0(7) . . ?
C84 C79 C78 114.0(8) . . ?
C84 C79 H79 105.5 . . ?
C79 C80 H80A 109.0 . . ?
C79 C80 H80B 109.0 . . ?
C79 C80 C81 112.7(10) . . ?
H80A C80 H80B 107.8 . . ?
C81 C80 H80A 109.0 . . ?
C81 C80 H80B 109.0 . . ?
C80 C81 H81A 109.3 . . ?
C80 C81 H81B 109.3 . . ?
C80 C81 C82 111.5(7) . . ?
H81A C81 H81B 108.0 . . ?
C82 C81 H81A 109.3 . . ?
C82 C81 H81B 109.3 . . ?
C81 C82 H82A 110.0 . . ?
C81 C82 H82B 110.0 . . ?
H82A C82 H82B 108.4 . . ?
C83 C82 C81 108.4(6) . . ?
C83 C82 H82A 110.0 . . ?
C83 C82 H82B 110.0 . . ?
C82 C83 H83A 109.0 . . ?
C82 C83 H83B 109.0 . . ?
H83A C83 H83B 107.8 . . ?
C84 C83 C82 113.0(8) . . ?
C84 C83 H83A 109.0 . . ?
C84 C83 H83B 109.0 . . ?
C79 C84 H84A 108.2 . . ?
C79 C84 H84B 108.2 . . ?
C83 C84 C79 116.3(9) . . ?
C83 C84 H84A 108.2 . . ?
C83 C84 H84B 108.2 . . ?
H84A C84 H84B 107.4 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.391(4) . ?
C1 C6 1.400(4) . ?
C1 C7 1.506(4) . ?
C2 C3 1.399(4) . ?
C2 O2 1.400(3) . ?
C3 C4 1.396(4) . ?
C3 C8 1.515(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.391(4) . ?
C5 C6 1.399(4) . ?
C5 C38 1.524(3) . ?
C6 O1 1.371(3) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8 0.9800 . ?
C8 C9 1.539(4) . ?
C8 C15 1.524(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.523(5) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.383(4) . ?
C11 C16 1.402(4) . ?
C11 C17 1.512(4) . ?
C12 C13 1.395(4) . ?
C12 O4 1.386(4) . ?
C13 C14 1.384(4) . ?
C13 C18 1.528(4) . ?
C14 H14 0.9300 . ?
C14 C15 1.398(4) . ?
C15 C16 1.400(4) . ?
C16 O3 1.370(3) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18 0.9800 . ?
C18 C19 1.538(4) . ?
C18 C25 1.525(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.530(4) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.393(4) . ?
C21 C26 1.397(4) . ?
C21 C27 1.507(4) . ?
C22 C23 1.394(4) . ?
C22 O6 1.386(3) . ?
C23 C24 1.402(3) . ?
C23 C28 1.529(3) . ?
C24 H24 0.9300 . ?
C24 C25 1.391(4) . ?
C25 C26 1.399(4) . ?
C26 O5 1.372(3) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28 0.9800 . ?
C28 C29 1.536(4) . ?
C28 C35 1.524(4) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.529(4) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32 1.398(4) . ?
C31 C36 1.389(4) . ?
C31 C37 1.505(4) . ?
C32 C33 1.397(4) . ?
C32 O8 1.385(3) . ?
C33 C34 1.393(4) . ?
C33 C38 1.526(3) . ?
C34 H34 0.9300 . ?
C34 C35 1.393(4) . ?
C35 C36 1.402(4) . ?
C36 O7 1.386(3) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 H38 0.9800 . ?
C38 C39 1.539(3) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 C40 1.518(4) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
O1 H1 0.8200 . ?
O2 H2 0.8200 . ?
O3 H3 0.8200 . ?
O4 H4A 0.8200 . ?
O5 H5 0.8200 . ?
O6 H6 0.8200 . ?
O7 H7 0.8200 . ?
O8 H8A 0.8200 . ?
C01L C45 1.395(4) . ?
C01L C46 1.393(5) . ?
C01L O10 1.381(4) . ?
C42 C43 1.400(4) . ?
C42 C46 1.393(5) . ?
C42 O9 1.380(4) . ?
C43 C44 1.384(5) . ?
C43 C58 1.527(5) 3_754 ?
C44 H44 0.9300 . ?
C44 C45 1.390(5) . ?
C45 C48 1.528(5) . ?
C46 C47 1.509(4) . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 H48 0.9800 . ?
C48 C49 1.543(5) . ?
C48 C53 1.527(4) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C49 C50 1.505(6) . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 C52 1.398(5) . ?
C51 C56 1.405(5) . ?
C51 C57 1.507(5) . ?
C52 C53 1.377(5) . ?
C52 O11 1.389(4) . ?
C53 C54 1.398(4) . ?
C54 H54 0.9300 . ?
C54 C55 1.397(4) . ?
C55 C56 1.386(5) . ?
C55 C58 1.537(4) . ?
C56 O12 1.386(4) . ?
C57 H57A 0.9600 . ?
C57 H57B 0.9600 . ?
C57 H57C 0.9600 . ?
C58 H58 0.9800 . ?
C58 C59 1.530(4) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C59 C60 1.516(5) . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
O9 H9 0.8200 . ?
O10 H10 0.8200 . ?
O11 H11 0.8200 . ?
O12 H12 0.8200 . ?
C61 H61 0.9300 . ?
C61 C62 1.370(5) . ?
C61 N1 1.319(5) . ?
C62 H62 0.9300 . ?
C62 C63 1.380(5) . ?
C63 H63 0.9300 . ?
C63 C64 1.345(5) . ?
C64 H64 0.9300 . ?
C64 C65 1.375(5) . ?
C65 H65 0.9300 . ?
C65 N1 1.324(4) . ?
N1 H1A 0.8715 . ?
C66 H66 0.9300 . ?
C66 C67 1.350(16) . ?
C66 N2 1.320(12) . ?
C67 H67 0.9300 . ?
C67 C68 1.367(15) . ?
C68 H68 0.9300 . ?
C68 C69 1.285(15) . ?
C69 H69 0.9300 . ?
C69 C70 1.424(16) . ?
C70 H70 0.9300 . ?
C70 N2 1.294(16) . ?
N2 H2A 0.8600 . ?
C71 C72 1.534(4) . ?
C71 O13 1.263(4) . ?
C71 O14 1.252(4) . ?
C72 H72 0.9800 . ?
C72 C73 1.519(4) . ?
C72 C77 1.529(5) . ?
C73 H73A 0.9700 . ?
C73 H73B 0.9700 . ?
C73 C74 1.527(4) . ?
C74 H74A 0.9700 . ?
C74 H74B 0.9700 . ?
C74 C75 1.513(4) . ?
C75 H75A 0.9700 . ?
C75 H75B 0.9700 . ?
C75 C76 1.511(4) . ?
C76 H76A 0.9700 . ?
C76 H76B 0.9700 . ?
C76 C77 1.538(4) . ?
C77 H77A 0.9700 . ?
C77 H77B 0.9700 . ?
C78 C79 1.523(9) . ?
C78 O15 1.263(7) . ?
C78 O16 1.278(7) . ?
C79 H79 0.9800 . ?
C79 C80 1.453(15) . ?
C79 C84 1.479(15) . ?
C80 H80A 0.9700 . ?
C80 H80B 0.9700 . ?
C80 C81 1.545(14) . ?
C81 H81A 0.9700 . ?
C81 H81B 0.9700 . ?
C81 C82 1.589(14) . ?
C82 H82A 0.9700 . ?
C82 H82B 0.9700 . ?
C82 C83 1.486(15) . ?
C83 H83A 0.9700 . ?
C83 H83B 0.9700 . ?
C83 C84 1.461(14) . ?
C84 H84A 0.9700 . ?
C84 H84B 0.9700 . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
25.0027 5.9978 -3.9986 -0.1983 -0.9514 0.3092
-24.0027 -5.9978 3.9987 0.1791 0.9369 -0.2901
-2.0073 -2.9942 10.0038 0.1370 0.7422 0.6045
-0.9921 1.9938 -11.0045 -0.1761 -0.6878 -0.7504
31.9983 -2.9981 -0.9966 -0.8428 -0.3262 0.4817
-29.9997 2.9993 2.9976 0.8642 0.4018 -0.3038
-19.9939 -2.0047 -8.0056 0.0107 -0.0023 -0.9776
19.9939 2.0047 8.0056 -0.0107 0.0023 0.9776
23.9942 -4.9950 5.0049 -0.6437 0.2304 0.7113
2.0013 -9.0004 -5.0017 -0.7877 0.2790 -0.4820
