# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items have may been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2MeOH@2_2
_database_code_depnum_ccdc_archive 'CCDC 1021703'
_audit_update_record             
;
2014-11-07 deposited with the CCDC.
2014-12-03 downloaded from the CCDC.
;

_vrf_PLAT420_2MeOH@2_2           
;
PROBLEM: D-H Without Acceptor O9 - H9 ... Please Check
RESPONSE: The H9 atom is involved in the O-H...pi interaction.
;

_audit_creation_date             2014-04-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C40 H48 O8, 2(C H4 O)'
_chemical_formula_sum            'C42 H56 O10'
_chemical_formula_weight         720.86
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C40 H40 F5 Br4'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.1523(17)
_cell_length_b                   12.5597(19)
_cell_length_c                   14.3332(14)
_cell_angle_alpha                104.789(11)
_cell_angle_beta                 102.134(10)
_cell_angle_gamma                107.641(13)
_cell_volume                     1915.0(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2773
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.5410
_cell_measurement_theta_min      2.5270
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       pillar
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.2107
_exptl_crystal_size_mid          0.1106
_exptl_crystal_size_min          0.0817
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0809
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10958
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         1.811
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 32.0214
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0040702000
_diffrn_orient_matrix_UB_12      0.0032391000
_diffrn_orient_matrix_UB_13      -0.0492248000
_diffrn_orient_matrix_UB_21      -0.0602671000
_diffrn_orient_matrix_UB_22      -0.0429127000
_diffrn_orient_matrix_UB_23      -0.0188314000
_diffrn_orient_matrix_UB_31      -0.0225256000
_diffrn_orient_matrix_UB_32      0.0461099000
_diffrn_orient_matrix_UB_33      0.0111602000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4682
_reflns_number_total             6909
_reflns_odcompleteness_completeness 99.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         6909
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0631
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0631P)²+0.2276P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1768
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C8(H8A), C18(H18), C28(H28), C38(H38)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C19(H19A,H19B), C29(H29A,H29B), C39(H39A,H39B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6A), C16(H16), C26(H26), C36(H36)
2.d 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), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C)
2.e Idealised tetrahedral OH refined as rotating group:
 O2(H2), O3(H3), O5(H5), O6(H6), O7(H7), O8(H8)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 -0.20687(18) -0.10310(18) 0.77643(16) 0.0355(5) Uani 1 1 d . . . . .
H1 H -0.262(3) -0.164(3) 0.733(3) 0.062(12) Uiso 1 1 d . . . . .
O2 O 0.08338(18) -0.21423(15) 0.63713(15) 0.0342(5) Uani 1 1 d . . . . .
H2 H 0.1392 -0.1791 0.6169 0.051 Uiso 1 1 calc GR . . . .
O3 O 0.24813(19) -0.08818(15) 0.56696(15) 0.0395(5) Uani 1 1 d . . . . .
H3 H 0.1892 -0.1071 0.5150 0.059 Uiso 1 1 calc GR . . . .
O4 O 0.43038(18) 0.30046(17) 0.54560(15) 0.0356(5) Uani 1 1 d . . . . .
H4 H 0.432(3) 0.260(3) 0.486(3) 0.071(12) Uiso 1 1 d . . . . .
O5 O 0.39387(17) 0.50982(16) 0.58128(14) 0.0321(5) Uani 1 1 d . . . . .
H5 H 0.4165 0.4521 0.5728 0.048 Uiso 1 1 calc GR . . . .
O6 O 0.07079(17) 0.58917(17) 0.68760(15) 0.0361(5) Uani 1 1 d . . . . .
H6 H 0.0866 0.6448 0.6640 0.054 Uiso 1 1 calc GR . . . .
O7 O -0.13093(17) 0.45292(17) 0.72767(15) 0.0364(5) Uani 1 1 d . . . . .
H7 H -0.0683 0.4957 0.7194 0.055 Uiso 1 1 calc GR . . . .
O8 O -0.27658(16) 0.09378(16) 0.79036(15) 0.0339(5) Uani 1 1 d . . . . .
H8 H -0.2550 0.0364 0.7909 0.051 Uiso 1 1 calc GR . . . .
O9 O -0.0660(3) 0.1607(3) 0.6015(2) 0.0787(10) Uani 1 1 d . . . . .
H9 H -0.079(4) 0.186(4) 0.651(3) 0.093(16) Uiso 1 1 d . . . . .
O10 O 0.56007(19) 0.74267(19) 0.65288(16) 0.0436(5) Uani 1 1 d . . . . .
H10 H 0.509(3) 0.659(3) 0.631(3) 0.079(12) Uiso 1 1 d . . . . .
C1 C -0.0028(2) 0.0311(2) 0.83532(19) 0.0281(6) Uani 1 1 d . . . . .
C2 C -0.0907(2) -0.0795(2) 0.76973(19) 0.0284(6) Uani 1 1 d . . . . .
C3 C -0.0633(2) -0.1610(2) 0.7019(2) 0.0283(6) Uani 1 1 d . . . . .
C4 C 0.0574(3) -0.1310(2) 0.70384(19) 0.0280(6) Uani 1 1 d . . . . .
C5 C 0.1494(2) -0.0233(2) 0.76925(19) 0.0284(6) Uani 1 1 d . . . . .
C6 C 0.1148(2) 0.0565(2) 0.83199(19) 0.0284(6) Uani 1 1 d . . . . .
H6A H 0.1750 0.1320 0.8744 0.034 Uiso 1 1 calc R . . . .
C7 C -0.1586(3) -0.2788(2) 0.6311(2) 0.0400(7) Uani 1 1 d . . . . .
H7A H -0.1817 -0.3311 0.6699 0.060 Uiso 1 1 calc GR . . . .
H7B H -0.1261 -0.3155 0.5803 0.060 Uiso 1 1 calc GR . . . .
H7C H -0.2302 -0.2666 0.5970 0.060 Uiso 1 1 calc GR . . . .
C8 C 0.2819(2) 0.0074(2) 0.7761(2) 0.0299(6) Uani 1 1 d . . . . .
H8A H 0.2900 -0.0692 0.7436 0.036 Uiso 1 1 calc R . . . .
C9 C 0.3673(3) 0.0583(3) 0.8862(2) 0.0369(7) Uani 1 1 d . . . . .
H9A H 0.4523 0.0773 0.8856 0.044 Uiso 1 1 calc R . . . .
H9B H 0.3600 0.1331 0.9223 0.044 Uiso 1 1 calc R . . . .
C10 C 0.3377(3) -0.0293(3) 0.9432(3) 0.0576(10) Uani 1 1 d . . . . .
H10A H 0.3956 0.0051 1.0120 0.086 Uiso 1 1 calc GR . . . .
H10B H 0.3437 -0.1039 0.9071 0.086 Uiso 1 1 calc GR . . . .
H10C H 0.2550 -0.0450 0.9471 0.086 Uiso 1 1 calc GR . . . .
C11 C 0.3192(2) 0.0863(2) 0.7143(2) 0.0272(6) Uani 1 1 d . . . . .
C12 C 0.3017(2) 0.0350(2) 0.6107(2) 0.0300(6) Uani 1 1 d . . . . .
C13 C 0.3408(2) 0.1035(2) 0.5526(2) 0.0315(6) Uani 1 1 d . . . . .
C14 C 0.3903(2) 0.2271(2) 0.5991(2) 0.0286(6) Uani 1 1 d . . . . .
C15 C 0.4035(2) 0.2825(2) 0.69981(19) 0.0261(6) Uani 1 1 d . . . . .
C16 C 0.3701(2) 0.2102(2) 0.7562(2) 0.0272(6) Uani 1 1 d . . . . .
H16 H 0.3825 0.2467 0.8263 0.033 Uiso 1 1 calc R . . . .
C17 C 0.3335(3) 0.0468(3) 0.4446(2) 0.0484(8) Uani 1 1 d . . . . .
H17A H 0.2644 0.0515 0.3986 0.073 Uiso 1 1 calc GR . . . .
H17B H 0.3227 -0.0367 0.4319 0.073 Uiso 1 1 calc GR . . . .
H17C H 0.4088 0.0887 0.4328 0.073 Uiso 1 1 calc GR . . . .
C18 C 0.4546(2) 0.4183(2) 0.74617(19) 0.0268(6) Uani 1 1 d . . . . .
H18 H 0.5093 0.4486 0.7076 0.032 Uiso 1 1 calc R . . . .
C19 C 0.5332(2) 0.4669(2) 0.8581(2) 0.0343(7) Uani 1 1 d . . . . .
H19A H 0.4814 0.4422 0.8996 0.041 Uiso 1 1 calc R . . . .
H19B H 0.5959 0.4317 0.8653 0.041 Uiso 1 1 calc R . . . .
C20 C 0.5955(3) 0.6021(2) 0.8985(2) 0.0463(8) Uani 1 1 d . . . . .
H20A H 0.6457 0.6286 0.9694 0.069 Uiso 1 1 calc GR . . . .
H20B H 0.5338 0.6376 0.8943 0.069 Uiso 1 1 calc GR . . . .
H20C H 0.6469 0.6271 0.8577 0.069 Uiso 1 1 calc GR . . . .
C21 C 0.3525(2) 0.4651(2) 0.72823(19) 0.0268(6) Uani 1 1 d . . . . .
C22 C 0.3253(2) 0.5058(2) 0.6473(2) 0.0278(6) Uani 1 1 d . . . . .
C23 C 0.2313(2) 0.5472(2) 0.63077(19) 0.0281(6) Uani 1 1 d . . . . .
C24 C 0.1668(2) 0.5513(2) 0.7003(2) 0.0279(6) Uani 1 1 d . . . . .
C25 C 0.1900(2) 0.5120(2) 0.78212(19) 0.0269(6) Uani 1 1 d . . . . .
C26 C 0.2822(2) 0.4674(2) 0.79255(19) 0.0273(6) Uani 1 1 d . . . . .
H26 H 0.2974 0.4372 0.8463 0.033 Uiso 1 1 calc R . . . .
C27 C 0.2015(3) 0.5870(3) 0.5405(2) 0.0351(7) Uani 1 1 d . . . . .
H27A H 0.2382 0.5563 0.4904 0.053 Uiso 1 1 calc GR . . . .
H27B H 0.2339 0.6741 0.5632 0.053 Uiso 1 1 calc GR . . . .
H27C H 0.1131 0.5564 0.5095 0.053 Uiso 1 1 calc GR . . . .
C28 C 0.1197(2) 0.5194(2) 0.85765(19) 0.0269(6) Uani 1 1 d . . . . .
H28 H 0.0814 0.5779 0.8492 0.032 Uiso 1 1 calc R . . . .
C29 C 0.2002(2) 0.5683(2) 0.9691(2) 0.0310(6) Uani 1 1 d . . . . .
H29A H 0.1478 0.5684 1.0135 0.037 Uiso 1 1 calc R . . . .
H29B H 0.2430 0.5147 0.9803 0.037 Uiso 1 1 calc R . . . .
C30 C 0.2936(3) 0.6936(2) 0.9994(2) 0.0418(8) Uani 1 1 d . . . . .
H30A H 0.3412 0.7208 1.0712 0.063 Uiso 1 1 calc GR . . . .
H30B H 0.2519 0.7472 0.9889 0.063 Uiso 1 1 calc GR . . . .
H30C H 0.3480 0.6935 0.9576 0.063 Uiso 1 1 calc GR . . . .
C31 C 0.0149(2) 0.4012(2) 0.83373(19) 0.0275(6) Uani 1 1 d . . . . .
C32 C -0.1027(2) 0.3772(2) 0.7746(2) 0.0292(6) Uani 1 1 d . . . . .
C33 C -0.2003(2) 0.2742(2) 0.7600(2) 0.0282(6) Uani 1 1 d . . . . .
C34 C -0.1772(2) 0.1921(2) 0.80446(19) 0.0276(6) Uani 1 1 d . . . . .
C35 C -0.0609(2) 0.2102(2) 0.86079(19) 0.0260(6) Uani 1 1 d . . . . .
C36 C 0.0327(2) 0.3150(2) 0.87336(19) 0.0283(6) Uani 1 1 d . . . . .
H36 H 0.1129 0.3284 0.9109 0.034 Uiso 1 1 calc R . . . .
C37 C -0.3249(2) 0.2548(3) 0.6992(2) 0.0399(7) Uani 1 1 d . . . . .
H37A H -0.3296 0.2384 0.6276 0.060 Uiso 1 1 calc GR . . . .
H37B H -0.3425 0.3262 0.7238 0.060 Uiso 1 1 calc GR . . . .
H37C H -0.3844 0.1870 0.7063 0.060 Uiso 1 1 calc GR . . . .
C38 C -0.0352(2) 0.1205(2) 0.90762(19) 0.0276(6) Uani 1 1 d . . . . .
H38 H -0.1126 0.0745 0.9171 0.033 Uiso 1 1 calc R . . . .
C39 C 0.0617(2) 0.1792(2) 1.01330(19) 0.0300(6) Uani 1 1 d . . . . .
H39A H 0.0732 0.1161 1.0392 0.036 Uiso 1 1 calc R . . . .
H39B H 0.1399 0.2249 1.0064 0.036 Uiso 1 1 calc R . . . .
C40 C 0.0288(3) 0.2617(3) 1.0900(2) 0.0430(8) Uani 1 1 d . . . . .
H40A H 0.0942 0.2971 1.1550 0.064 Uiso 1 1 calc GR . . . .
H40B H -0.0469 0.2165 1.0995 0.064 Uiso 1 1 calc GR . . . .
H40C H 0.0177 0.3248 1.0653 0.064 Uiso 1 1 calc GR . . . .
C41 C 0.0499(4) 0.1737(4) 0.5976(3) 0.0744(12) Uani 1 1 d . . . . .
H41A H 0.0897 0.1477 0.6494 0.112 Uiso 1 1 calc GR . . . .
H41B H 0.0971 0.2575 0.6104 0.112 Uiso 1 1 calc GR . . . .
H41C H 0.0452 0.1253 0.5303 0.112 Uiso 1 1 calc GR . . . .
C42 C 0.5049(3) 0.8094(3) 0.7118(3) 0.0619(10) Uani 1 1 d . . . . .
H42A H 0.4957 0.7819 0.7689 0.093 Uiso 1 1 calc GR . . . .
H42B H 0.4249 0.7974 0.6688 0.093 Uiso 1 1 calc GR . . . .
H42C H 0.5567 0.8941 0.7378 0.093 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 C2 1.381(3) . ?
O2 C4 1.387(3) . ?
O3 C12 1.390(3) . ?
O4 C14 1.386(3) . ?
O5 C22 1.387(3) . ?
O6 C24 1.382(3) . ?
O7 C32 1.380(3) . ?
O8 C34 1.375(3) . ?
O9 C41 1.382(5) . ?
O10 C42 1.443(4) . ?
C1 C2 1.402(4) . ?
C1 C6 1.380(4) . ?
C1 C38 1.529(4) . ?
C2 C3 1.391(4) . ?
C3 C4 1.392(4) . ?
C3 C7 1.504(4) . ?
C4 C5 1.398(4) . ?
C5 C6 1.396(4) . ?
C5 C8 1.512(4) . ?
C8 C9 1.539(4) . ?
C8 C11 1.522(3) . ?
C9 C10 1.534(4) . ?
C11 C12 1.401(4) . ?
C11 C16 1.395(4) . ?
C12 C13 1.395(4) . ?
C13 C14 1.397(4) . ?
C13 C17 1.502(4) . ?
C14 C15 1.385(4) . ?
C15 C16 1.390(3) . ?
C15 C18 1.530(3) . ?
C18 C19 1.536(3) . ?
C18 C21 1.529(3) . ?
C19 C20 1.525(4) . ?
C21 C22 1.399(3) . ?
C21 C26 1.383(3) . ?
C22 C23 1.394(4) . ?
C23 C24 1.392(4) . ?
C23 C27 1.516(3) . ?
C24 C25 1.393(3) . ?
C25 C26 1.394(3) . ?
C25 C28 1.515(3) . ?
C28 C29 1.538(4) . ?
C28 C31 1.535(4) . ?
C29 C30 1.522(4) . ?
C31 C32 1.396(4) . ?
C31 C36 1.396(3) . ?
C32 C33 1.397(4) . ?
C33 C34 1.408(3) . ?
C33 C37 1.491(4) . ?
C34 C35 1.390(4) . ?
C35 C36 1.394(3) . ?
C35 C38 1.526(3) . ?
C38 C39 1.542(3) . ?
C39 C40 1.515(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
C2 C1 C38 121.6(2) . . ?
C6 C1 C2 117.4(2) . . ?
C6 C1 C38 121.0(2) . . ?
O1 C2 C1 115.9(2) . . ?
O1 C2 C3 121.7(2) . . ?
C3 C2 C1 122.4(2) . . ?
C2 C3 C4 117.4(2) . . ?
C2 C3 C7 122.0(2) . . ?
C4 C3 C7 120.6(2) . . ?
O2 C4 C3 116.6(2) . . ?
O2 C4 C5 120.7(2) . . ?
C3 C4 C5 122.7(2) . . ?
C4 C5 C8 123.2(2) . . ?
C6 C5 C4 116.9(2) . . ?
C6 C5 C8 119.9(2) . . ?
C1 C6 C5 123.1(2) . . ?
C5 C8 C9 113.1(2) . . ?
C5 C8 C11 111.4(2) . . ?
C11 C8 C9 112.7(2) . . ?
C10 C9 C8 111.9(2) . . ?
C12 C11 C8 120.0(2) . . ?
C16 C11 C8 122.8(2) . . ?
C16 C11 C12 117.3(2) . . ?
O3 C12 C11 118.2(2) . . ?
O3 C12 C13 120.0(2) . . ?
C13 C12 C11 121.8(2) . . ?
C12 C13 C14 117.8(2) . . ?
C12 C13 C17 121.3(2) . . ?
C14 C13 C17 120.8(2) . . ?
O4 C14 C13 120.8(2) . . ?
C15 C14 O4 116.6(2) . . ?
C15 C14 C13 122.6(2) . . ?
C14 C15 C16 117.4(2) . . ?
C14 C15 C18 120.5(2) . . ?
C16 C15 C18 122.1(2) . . ?
C15 C16 C11 122.9(2) . . ?
C15 C18 C19 113.8(2) . . ?
C21 C18 C15 110.3(2) . . ?
C21 C18 C19 112.8(2) . . ?
C20 C19 C18 112.6(2) . . ?
C22 C21 C18 122.4(2) . . ?
C26 C21 C18 120.1(2) . . ?
C26 C21 C22 117.5(2) . . ?
O5 C22 C21 121.1(2) . . ?
O5 C22 C23 116.8(2) . . ?
C23 C22 C21 122.1(2) . . ?
C22 C23 C27 120.9(2) . . ?
C24 C23 C22 117.6(2) . . ?
C24 C23 C27 121.5(2) . . ?
O6 C24 C23 120.8(2) . . ?
O6 C24 C25 116.5(2) . . ?
C23 C24 C25 122.6(2) . . ?
C24 C25 C26 117.1(2) . . ?
C24 C25 C28 121.4(2) . . ?
C26 C25 C28 121.4(2) . . ?
C21 C26 C25 123.0(2) . . ?
C25 C28 C29 113.8(2) . . ?
C25 C28 C31 112.1(2) . . ?
C31 C28 C29 111.6(2) . . ?
C30 C29 C28 112.9(2) . . ?
C32 C31 C28 121.6(2) . . ?
C36 C31 C28 121.0(2) . . ?
C36 C31 C32 117.3(2) . . ?
O7 C32 C31 122.8(2) . . ?
O7 C32 C33 115.5(2) . . ?
C31 C32 C33 121.7(2) . . ?
C32 C33 C34 118.3(2) . . ?
C32 C33 C37 119.6(2) . . ?
C34 C33 C37 122.1(2) . . ?
O8 C34 C33 116.2(2) . . ?
O8 C34 C35 121.8(2) . . ?
C35 C34 C33 122.0(2) . . ?
C34 C35 C36 117.1(2) . . ?
C34 C35 C38 122.1(2) . . ?
C36 C35 C38 120.8(2) . . ?
C35 C36 C31 123.5(2) . . ?
C1 C38 C39 111.4(2) . . ?
C35 C38 C1 111.1(2) . . ?
C35 C38 C39 113.3(2) . . ?
C40 C39 C38 113.4(2) . . ?

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 C2 C3 C4 -177.4(2) . . . . ?
O1 C2 C3 C7 0.8(4) . . . . ?
O2 C4 C5 C6 178.4(2) . . . . ?
O2 C4 C5 C8 -3.2(4) . . . . ?
O3 C12 C13 C14 177.9(2) . . . . ?
O3 C12 C13 C17 -3.9(4) . . . . ?
O4 C14 C15 C16 -176.5(2) . . . . ?
O4 C14 C15 C18 2.8(4) . . . . ?
O5 C22 C23 C24 -175.8(2) . . . . ?
O5 C22 C23 C27 3.8(4) . . . . ?
O6 C24 C25 C26 176.5(2) . . . . ?
O6 C24 C25 C28 -4.6(4) . . . . ?
O7 C32 C33 C34 178.9(2) . . . . ?
O7 C32 C33 C37 -1.5(4) . . . . ?
O8 C34 C35 C36 -177.8(2) . . . . ?
O8 C34 C35 C38 2.1(4) . . . . ?
C1 C2 C3 C4 2.5(4) . . . . ?
C1 C2 C3 C7 -179.3(2) . . . . ?
C1 C38 C39 C40 -175.6(2) . . . . ?
C2 C1 C6 C5 -1.9(4) . . . . ?
C2 C1 C38 C35 -94.8(3) . . . . ?
C2 C1 C38 C39 137.9(2) . . . . ?
C2 C3 C4 O2 178.8(2) . . . . ?
C2 C3 C4 C5 -0.9(4) . . . . ?
C3 C4 C5 C6 -1.9(4) . . . . ?
C3 C4 C5 C8 176.5(2) . . . . ?
C4 C5 C6 C1 3.4(4) . . . . ?
C4 C5 C8 C9 -132.9(3) . . . . ?
C4 C5 C8 C11 98.9(3) . . . . ?
C5 C8 C9 C10 59.5(3) . . . . ?
C5 C8 C11 C12 -86.1(3) . . . . ?
C5 C8 C11 C16 93.2(3) . . . . ?
C6 C1 C2 O1 178.7(2) . . . . ?
C6 C1 C2 C3 -1.2(4) . . . . ?
C6 C1 C38 C35 85.0(3) . . . . ?
C6 C1 C38 C39 -42.3(3) . . . . ?
C6 C5 C8 C9 45.4(3) . . . . ?
C6 C5 C8 C11 -82.7(3) . . . . ?
C7 C3 C4 O2 0.6(3) . . . . ?
C7 C3 C4 C5 -179.1(2) . . . . ?
C8 C5 C6 C1 -175.1(2) . . . . ?
C8 C11 C12 O3 1.0(4) . . . . ?
C8 C11 C12 C13 -176.4(2) . . . . ?
C8 C11 C16 C15 -179.5(2) . . . . ?
C9 C8 C11 C12 145.5(3) . . . . ?
C9 C8 C11 C16 -35.2(3) . . . . ?
C11 C8 C9 C10 -173.0(2) . . . . ?
C11 C12 C13 C14 -4.8(4) . . . . ?
C11 C12 C13 C17 173.4(3) . . . . ?
C12 C11 C16 C15 -0.2(4) . . . . ?
C12 C13 C14 O4 -179.7(2) . . . . ?
C12 C13 C14 C15 1.2(4) . . . . ?
C13 C14 C15 C16 2.7(4) . . . . ?
C13 C14 C15 C18 -178.0(2) . . . . ?
C14 C15 C16 C11 -3.2(4) . . . . ?
C14 C15 C18 C19 -145.0(3) . . . . ?
C14 C15 C18 C21 87.1(3) . . . . ?
C15 C18 C19 C20 172.9(2) . . . . ?
C15 C18 C21 C22 -96.4(3) . . . . ?
C15 C18 C21 C26 83.0(3) . . . . ?
C16 C11 C12 O3 -178.3(2) . . . . ?
C16 C11 C12 C13 4.3(4) . . . . ?
C16 C15 C18 C19 34.2(3) . . . . ?
C16 C15 C18 C21 -93.7(3) . . . . ?
C17 C13 C14 O4 2.1(4) . . . . ?
C17 C13 C14 C15 -177.0(3) . . . . ?
C18 C15 C16 C11 177.6(2) . . . . ?
C18 C21 C22 O5 -2.6(4) . . . . ?
C18 C21 C22 C23 179.3(2) . . . . ?
C18 C21 C26 C25 178.2(2) . . . . ?
C19 C18 C21 C22 135.2(3) . . . . ?
C19 C18 C21 C26 -45.4(3) . . . . ?
C21 C18 C19 C20 -60.5(3) . . . . ?
C21 C22 C23 C24 2.4(4) . . . . ?
C21 C22 C23 C27 -178.0(2) . . . . ?
C22 C21 C26 C25 -2.4(4) . . . . ?
C22 C23 C24 O6 -178.7(2) . . . . ?
C22 C23 C24 C25 -2.4(4) . . . . ?
C23 C24 C25 C26 0.1(4) . . . . ?
C23 C24 C25 C28 178.9(2) . . . . ?
C24 C25 C26 C21 2.4(4) . . . . ?
C24 C25 C28 C29 -134.5(2) . . . . ?
C24 C25 C28 C31 97.6(3) . . . . ?
C25 C28 C29 C30 60.2(3) . . . . ?
C25 C28 C31 C32 -93.3(3) . . . . ?
C25 C28 C31 C36 89.0(3) . . . . ?
C26 C21 C22 O5 178.0(2) . . . . ?
C26 C21 C22 C23 -0.1(4) . . . . ?
C26 C25 C28 C29 44.3(3) . . . . ?
C26 C25 C28 C31 -83.6(3) . . . . ?
C27 C23 C24 O6 1.7(4) . . . . ?
C27 C23 C24 C25 178.0(2) . . . . ?
C28 C25 C26 C21 -176.5(2) . . . . ?
C28 C31 C32 O7 5.0(4) . . . . ?
C28 C31 C32 C33 -174.3(2) . . . . ?
C28 C31 C36 C35 174.8(2) . . . . ?
C29 C28 C31 C32 137.7(3) . . . . ?
C29 C28 C31 C36 -40.1(3) . . . . ?
C31 C28 C29 C30 -171.6(2) . . . . ?
C31 C32 C33 C34 -1.7(4) . . . . ?
C31 C32 C33 C37 177.8(3) . . . . ?
C32 C31 C36 C35 -3.1(4) . . . . ?
C32 C33 C34 O8 178.3(2) . . . . ?
C32 C33 C34 C35 -0.7(4) . . . . ?
C33 C34 C35 C36 1.2(4) . . . . ?
C33 C34 C35 C38 -179.0(2) . . . . ?
C34 C35 C36 C31 0.8(4) . . . . ?
C34 C35 C38 C1 91.5(3) . . . . ?
C34 C35 C38 C39 -142.2(3) . . . . ?
C35 C38 C39 C40 58.2(3) . . . . ?
C36 C31 C32 O7 -177.2(2) . . . . ?
C36 C31 C32 C33 3.5(4) . . . . ?
C36 C35 C38 C1 -88.7(3) . . . . ?
C36 C35 C38 C39 37.6(3) . . . . ?
C37 C33 C34 O8 -1.3(4) . . . . ?
C37 C33 C34 C35 179.7(2) . . . . ?
C38 C1 C2 O1 -1.4(3) . . . . ?
C38 C1 C2 C3 178.6(2) . . . . ?
C38 C1 C6 C5 178.3(2) . . . . ?
C38 C35 C36 C31 -179.1(2) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_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
-16 -1 10 0.0579 -15.9999 -1.0000 10.0000 -0.4304 0.8189 0.4259
15 2 -10 0.0478 14.9999 2.0000 -10.0000 0.4377 -0.8015 -0.3573
0 17 -6 0.0939 0.0003 17.0001 -6.0001 0.3504 -0.6165 0.7169
4 -18 4 0.0832 3.9997 -18.0001 4.0001 -0.2715 0.4561 -0.8754
-3 0 -17 0.0496 -3.0001 0.0000 -17.0000 0.8490 0.5009 -0.1221
2 1 17 0.0251 2.0001 1.0000 17.0000 -0.8417 -0.4836 0.1908
-12 13 -9 0.0882 -11.9997 13.0001 -9.0001 0.5340 0.3348 0.7693
-15 -1 -1 0.0561 -14.9999 -1.0000 -1.0000 0.1070 0.9657 0.2806
0 14 -16 0.0815 0.0002 14.0001 -16.0000 0.8329 -0.2995 0.4670

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items have may been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5a@2
_database_code_depnum_ccdc_archive 'CCDC 1021704'
_audit_update_record             
;
2014-11-07 deposited with the CCDC.
2014-12-03 downloaded from the CCDC.
;

_audit_creation_date             2014-05-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'2(C40 H48 O8), 2(C H4 O), C3 H10 N, 4(H2 O), Cl'
_chemical_formula_sum            'C85 H122 Cl N O22'
_chemical_formula_weight         1545.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H72 N12 O6'
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'
Cl Cl 0.1484 0.1585 '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'

_shelx_space_group_comment       
;
The structure is solved and refined in space group Pnnn with Z=2.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           48
_space_group_name_H-M_alt        'P n n n'
_space_group_name_Hall           '-P 2ab 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x, -y+1/2, -z+1/2'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x, y-1/2, z-1/2'
'x-1/2, -y, z-1/2'

_cell_length_a                   12.6722(4)
_cell_length_b                   15.1699(5)
_cell_length_c                   22.9465(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4411.2(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3695
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.3220
_cell_measurement_theta_min      2.2550
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94309
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.347
_exptl_crystal_size_mid          0.2729
_exptl_crystal_size_min          0.1837
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12721
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         25.247
_diffrn_reflns_theta_min         1.836
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 32.0214
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -93.00  -68.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8607 -178.0000  120.0000 25

#__ type_ start__ end____ width___ exp.time_
  2 omega   -7.00   86.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6419   77.0000 -150.0000 93

#__ type_ start__ end____ width___ exp.time_
  3 omega   12.00   62.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6419   37.0000    0.0000 50
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0050857000
_diffrn_orient_matrix_UB_12      -0.0362233000
_diffrn_orient_matrix_UB_13      0.0193102000
_diffrn_orient_matrix_UB_21      0.0020723000
_diffrn_orient_matrix_UB_22      0.0291932000
_diffrn_orient_matrix_UB_23      0.0241378000
_diffrn_orient_matrix_UB_31      -0.0557122000
_diffrn_orient_matrix_UB_32      0.0044102000
_diffrn_orient_matrix_UB_33      -0.0008374000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3009
_reflns_number_total             4003
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4003
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0626
_refine_ls_restrained_S_all      1.053
_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)+(0.1142P)²+2.2983P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1836
_refine_ls_wR_factor_ref         0.2050
_refine_special_details          
;
 ?
;
_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, All O(H,H) groups
2. Restrained distances
 C22A-C23A = C22A-C24A = C23A-C24A = C22B-C23B = C22B-C24B = C23B-C24B
 2.4 with sigma of 0.04
 N1A-C22A = N1A-C23A = N1A-C24A = N1B-C22B = N1B-C23B = N1B-C24B
 1.5 with sigma of 0.02
 H4B-H15 = H3B-H15
 2.1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl2) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Uiso(N1B)=Uiso(N1A)=0.8*FVAR(2)
 Uiso(C22B)=Uiso(C23B)=Uiso(C24B)=Uiso(C22A)=Uiso(C23A)=Uiso(C24A)=FVAR(1)
 Fixed Sof: H2A(0.5) H2B(0.5) H3A(0.5) H3B(0.5) H4B(0.5) H4A(0.5) O9(0.5)
 H9(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) N1B(0.125) H1BA(0.125)
 C22B(0.125) H22A(0.125) H22B(0.125) H22C(0.125) C23B(0.125) H23A(0.125)
 H23B(0.125) H23C(0.125) C24B(0.125) H24A(0.125) H24B(0.125) H24C(0.125)
 N1A(0.125) H1AB(0.125) C22A(0.125) H22D(0.125) H22E(0.125) H22F(0.125)
 C23A(0.125) H23D(0.125) H23E(0.125) H23F(0.125) C24A(0.125) H24D(0.125)
 H24E(0.125) H24F(0.125) O8(0.5) H8A(0.5) H8B(0.5) Cl3(0.05) O5(0.5) H5A(0.5)
 H5B(0.5) Cl2(0.1) Cl1(0.1) H1BB(0.5) H1AA(0.5)
5.a Riding coordinates:
 O2(H2B), O4(H4A), C22B(H22A,H22B,H22C), C22A(H22D,H22E,H22F), C23A(H23D,H23E,
 H23F)
5.b Free rotating group:
 O8(H8A,H8B), O5(H5A,H5B)
5.c Ternary CH refined with riding coordinates:
 C5(H5), C15(H15), N1B(H1BA), N1A(H1AB)
5.d Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C16(H16A,H16B)
5.e Aromatic/amide H refined with riding coordinates:
 C14(H14), C20(H20)
5.f Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C17(H17A,H17B,H17C),
 C21(H21A,H21B,H21C), C23B(H23A,H23B,H23C), C24B(H24A,H24B,H24C), C24A(H24D,
 H24E,H24F)
5.g Idealised tetrahedral OH refined as rotating group:
 O2(H2A), O3(H3A), O3(H3B), O4(H4B), O9(H9), O1(H1BB), O1(H1AA)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
O2 O 0.52080(15) -0.00340(12) 0.34983(9) 0.0502(5) Uani 1 1 d . . . . .
H2A H 0.5847 -0.0182 0.3498 0.075 Uiso 0.5 1 calc GR . P A 1
H2B H 0.4640 -0.0321 0.3398 0.061(19) Uiso 0.5 1 d R . P B 2
O3 O 0.35511(13) 0.27897(11) 0.35350(9) 0.0433(5) Uani 1 1 d . . . . .
H3A H 0.2953 0.2551 0.3529 0.065 Uiso 0.5 1 calc GR . P C -2
H3B H 0.3821 0.3294 0.3513 0.065 Uiso 0.5 1 calc DGR . P D 1
O4 O 0.43891(14) 0.44723(12) 0.35054(9) 0.0487(5) Uani 1 1 d . . . . .
H4B H 0.4186 0.3945 0.3506 0.073 Uiso 0.5 1 calc DGR . P E 2
H4A H 0.4164 0.4958 0.3334 0.073 Uiso 0.5 1 d R . P F 1
C1 C 0.5853(2) 0.5646(2) 0.29752(14) 0.0584(8) Uani 1 1 d . . . . .
H1A H 0.5543 0.6209 0.3097 0.088 Uiso 1 1 calc GR . . . .
H1B H 0.5347 0.5325 0.2732 0.088 Uiso 1 1 calc GR . . . .
H1C H 0.6498 0.5758 0.2751 0.088 Uiso 1 1 calc GR . . . .
C2 C 0.61162(19) 0.51047(15) 0.35065(11) 0.0371(6) Uani 1 1 d . . . . .
C3 C 0.71205(18) 0.51464(15) 0.37572(11) 0.0337(6) Uani 1 1 d . . . . .
C4 C 0.74149(17) 0.46142(14) 0.42253(10) 0.0295(5) Uani 1 1 d . . . . .
C5 C 0.64864(17) 0.03344(14) 0.44954(11) 0.0308(5) Uani 1 1 d . . . . .
H5 H 0.6201 -0.0262 0.4397 0.037 Uiso 1 1 calc R . . . .
C6 C 0.65129(18) 0.03899(16) 0.51626(11) 0.0359(6) Uani 1 1 d . . . . .
H6A H 0.6807 0.0969 0.5279 0.043 Uiso 1 1 calc R . . . .
H6B H 0.5782 0.0355 0.5314 0.043 Uiso 1 1 calc R . . . .
C7 C 0.7166(2) -0.0335(2) 0.54383(14) 0.0520(7) Uani 1 1 d . . . . .
H7A H 0.7897 -0.0292 0.5301 0.078 Uiso 1 1 calc GR . . . .
H7B H 0.6875 -0.0910 0.5329 0.078 Uiso 1 1 calc GR . . . .
H7C H 0.7150 -0.0272 0.5863 0.078 Uiso 1 1 calc GR . . . .
C8 C 0.57334(17) 0.10041(14) 0.42257(10) 0.0293(5) Uani 1 1 d . . . . .
C9 C 0.51062(18) 0.07907(15) 0.37474(11) 0.0337(6) Uani 1 1 d . . . . .
C10 C 0.43781(18) 0.13800(16) 0.35057(11) 0.0349(6) Uani 1 1 d . . . . .
C11 C 0.3717(2) 0.11364(19) 0.29816(13) 0.0491(7) Uani 1 1 d . . . . .
H11A H 0.4121 0.0740 0.2728 0.074 Uiso 1 1 calc GR . . . .
H11B H 0.3531 0.1672 0.2765 0.074 Uiso 1 1 calc GR . . . .
H11C H 0.3072 0.0840 0.3111 0.074 Uiso 1 1 calc GR . . . .
C12 C 0.42813(17) 0.22052(15) 0.37655(11) 0.0324(5) Uani 1 1 d . . . . .
C13 C 0.49012(16) 0.24607(14) 0.42393(10) 0.0288(5) Uani 1 1 d . . . . .
C14 C 0.56210(17) 0.18481(14) 0.44532(10) 0.0298(5) Uani 1 1 d . . . . .
H14 H 0.6058 0.2015 0.4771 0.036 Uiso 1 1 calc R . . . .
C15 C 0.48136(17) 0.33818(14) 0.45002(11) 0.0311(5) Uani 1 1 d . . . . .
H15 H 0.4105 0.3615 0.4385 0.037 Uiso 1 1 calc DR . . . .
C16 C 0.48466(19) 0.33917(16) 0.51707(11) 0.0381(6) Uani 1 1 d . . . . .
H16A H 0.5528 0.3143 0.5302 0.046 Uiso 1 1 calc R . . . .
H16B H 0.4810 0.4010 0.5308 0.046 Uiso 1 1 calc R . . . .
C17 C 0.3949(2) 0.2869(2) 0.54473(14) 0.0547(8) Uani 1 1 d . . . . .
H17A H 0.3272 0.3086 0.5299 0.082 Uiso 1 1 calc GR . . . .
H17B H 0.3973 0.2940 0.5872 0.082 Uiso 1 1 calc GR . . . .
H17C H 0.4026 0.2243 0.5349 0.082 Uiso 1 1 calc GR . . . .
C18 C 0.56287(17) 0.39948(14) 0.42287(10) 0.0295(5) Uani 1 1 d . . . . .
C19 C 0.53837(18) 0.45260(15) 0.37531(11) 0.0346(6) Uani 1 1 d . . . . .
C20 C 0.66524(17) 0.40407(14) 0.44422(10) 0.0301(5) Uani 1 1 d . . . . .
H20 H 0.6843 0.3660 0.4753 0.036 Uiso 1 1 calc R . . . .
O9 O 0.6177(6) 0.1172(5) 0.6933(3) 0.0613(17) Uani 0.5 1 d . . P G 1
H9 H 0.5847 0.0736 0.6800 0.092 Uiso 0.5 1 calc GR . P G 1
C21 C 0.5735(7) 0.1928(4) 0.6729(4) 0.092(3) Uani 0.5 1 d . . P G 1
H21A H 0.6147 0.2147 0.6398 0.138 Uiso 0.5 1 calc GR . P G 1
H21B H 0.5729 0.2373 0.7039 0.138 Uiso 0.5 1 calc GR . P G 1
H21C H 0.5010 0.1810 0.6603 0.138 Uiso 0.5 1 calc GR . P G 1
N1B N 0.779(2) 0.258(2) 0.2689(11) 0.086(4) Uiso 0.125 1 d D . P H -2
H1BA H 0.7180 0.2437 0.2429 0.103 Uiso 0.125 1 calc R . P H -2
C22B C 0.758(6) 0.257(4) 0.3352(13) 0.107(5) Uiso 0.125 1 d D . P H -2
H22A H 0.7046 0.3017 0.3436 0.160 Uiso 0.125 1 d R . P H -2
H22B H 0.7351 0.1998 0.3503 0.160 Uiso 0.125 1 d R . P H -2
H22C H 0.8249 0.2737 0.3539 0.160 Uiso 0.125 1 d R . P H -2
C23B C 0.877(3) 0.196(2) 0.266(2) 0.107(5) Uiso 0.125 1 d D . P H -2
H23A H 0.9347 0.2214 0.2888 0.160 Uiso 0.125 1 calc GR . P H -2
H23B H 0.8987 0.1883 0.2256 0.160 Uiso 0.125 1 calc GR . P H -2
H23C H 0.8578 0.1382 0.2827 0.160 Uiso 0.125 1 calc GR . P H -2
C24B C 0.836(3) 0.3453(19) 0.257(2) 0.107(5) Uiso 0.125 1 d D . P H -2
H24A H 0.8111 0.3900 0.2849 0.160 Uiso 0.125 1 calc GR . P H -2
H24B H 0.8214 0.3648 0.2174 0.160 Uiso 0.125 1 calc GR . P H -2
H24C H 0.9121 0.3368 0.2623 0.160 Uiso 0.125 1 calc GR . P H -2
N1A N 0.729(2) 0.2719(14) 0.2559(15) 0.086(4) Uiso 0.125 1 d D . P I -1
H1AB H 0.7922 0.2411 0.2398 0.103 Uiso 0.125 1 calc R . P I -1
C22A C 0.706(3) 0.264(3) 0.3219(14) 0.107(5) Uiso 0.125 1 d D . P I -1
H22D H 0.6897 0.2031 0.3337 0.160 Uiso 0.125 1 d R . P I -1
H22E H 0.7616 0.2873 0.3474 0.160 Uiso 0.125 1 d R . P I -1
H22F H 0.6430 0.3002 0.3250 0.160 Uiso 0.125 1 d R . P I -1
C23A C 0.618(2) 0.246(3) 0.2314(15) 0.107(5) Uiso 0.125 1 d D . P I -1
H23D H 0.5885 0.1965 0.2535 0.160 Uiso 0.125 1 d R . P I -1
H23E H 0.6250 0.2293 0.1903 0.160 Uiso 0.125 1 d R . P I -1
H23F H 0.5699 0.2968 0.2345 0.160 Uiso 0.125 1 d R . P I -1
C24A C 0.719(3) 0.3715(17) 0.246(2) 0.107(5) Uiso 0.125 1 d D . P I -1
H24D H 0.6518 0.3924 0.2623 0.160 Uiso 0.125 1 calc GR . P I -1
H24E H 0.7200 0.3837 0.2039 0.160 Uiso 0.125 1 calc GR . P I -1
H24F H 0.7775 0.4020 0.2648 0.160 Uiso 0.125 1 calc GR . P I -1
O8 O 0.761(2) 0.7581(15) 0.31168(19) 0.059(3) Uani 0.5 1 d . . P J -1
H8A H 0.7463 0.7094 0.3301 0.088 Uiso 0.5 1 d G . P J -1
H8B H 0.7301 0.7580 0.2778 0.088 Uiso 0.5 1 d G . P J -1
Cl3 Cl 0.7500 0.2500 0.5819(7) 0.072(4) Uani 0.1 2 d S T P K 3
O5 O 0.6681(7) 0.4109(5) 0.6885(4) 0.076(2) Uani 0.5 1 d . U P L 2
H5A H 0.6749 0.4060 0.7261 0.114 Uiso 0.5 1 d G . P L 2
H5B H 0.7287 0.4015 0.6719 0.114 Uiso 0.5 1 d G . P L 2
Cl2 Cl 0.6698(15) 0.3872(12) 0.6599(9) 0.098(5) Uani 0.1 1 d . U P M 1
Cl1 Cl 0.6324(15) 0.1229(15) 0.6635(9) 0.101(7) Uani 0.1 1 d . . P N 2
O1 O 0.78371(14) 0.57359(12) 0.35219(9) 0.0475(5) Uani 1 1 d . . . . .
H1BB H 0.8447 0.5521 0.3541 0.071 Uiso 0.5 1 calc GR . P O 2
H1AA H 0.7515 0.6184 0.3400 0.08(2) Uiso 0.5 1 calc GR . P P 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
O2 C9 1.381(3) . ?
O3 C12 1.386(3) . ?
O4 C19 1.385(3) . ?
C1 C2 1.507(4) . ?
C2 C3 1.398(3) . ?
C2 C19 1.397(3) . ?
C3 C4 1.395(3) . ?
C3 O1 1.384(3) . ?
C4 C5 1.526(3) 2_655 ?
C4 C20 1.392(3) . ?
C5 C4 1.526(3) 2_655 ?
C5 C6 1.534(3) . ?
C5 C8 1.525(3) . ?
C6 C7 1.515(4) . ?
C8 C9 1.393(3) . ?
C8 C14 1.390(3) . ?
C9 C10 1.399(3) . ?
C10 C11 1.511(3) . ?
C10 C12 1.392(3) . ?
C12 C13 1.396(3) . ?
C13 C14 1.392(3) . ?
C13 C15 1.524(3) . ?
C15 C16 1.539(3) . ?
C15 C18 1.523(3) . ?
C16 C17 1.525(4) . ?
C18 C19 1.392(3) . ?
C18 C20 1.388(3) . ?
O9 C21 1.360(11) . ?
N1B C22B 1.544(18) . ?
N1B C23B 1.562(19) . ?
N1B C24B 1.527(19) . ?
N1A C22A 1.545(19) . ?
N1A C23A 1.568(19) . ?
N1A C24A 1.535(18) . ?

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 C2 C1 120.6(2) . . ?
C19 C2 C1 121.5(2) . . ?
C19 C2 C3 117.8(2) . . ?
C4 C3 C2 122.3(2) . . ?
O1 C3 C2 117.8(2) . . ?
O1 C3 C4 119.9(2) . . ?
C3 C4 C5 121.8(2) . 2_655 ?
C20 C4 C3 116.8(2) . . ?
C20 C4 C5 121.3(2) . 2_655 ?
C4 C5 C6 112.50(19) 2_655 . ?
C8 C5 C4 111.84(18) . 2_655 ?
C8 C5 C6 112.47(19) . . ?
C7 C6 C5 112.9(2) . . ?
C9 C8 C5 121.5(2) . . ?
C14 C8 C5 121.7(2) . . ?
C14 C8 C9 116.8(2) . . ?
O2 C9 C8 118.9(2) . . ?
O2 C9 C10 118.4(2) . . ?
C8 C9 C10 122.7(2) . . ?
C9 C10 C11 121.6(2) . . ?
C12 C10 C9 117.6(2) . . ?
C12 C10 C11 120.8(2) . . ?
O3 C12 C10 118.1(2) . . ?
O3 C12 C13 119.7(2) . . ?
C10 C12 C13 122.2(2) . . ?
C12 C13 C15 121.3(2) . . ?
C14 C13 C12 117.3(2) . . ?
C14 C13 C15 121.4(2) . . ?
C8 C14 C13 123.4(2) . . ?
C13 C15 C16 113.55(19) . . ?
C18 C15 C13 110.46(18) . . ?
C18 C15 C16 112.61(19) . . ?
C17 C16 C15 113.0(2) . . ?
C19 C18 C15 121.5(2) . . ?
C20 C18 C15 121.3(2) . . ?
C20 C18 C19 117.1(2) . . ?
O4 C19 C2 118.4(2) . . ?
O4 C19 C18 119.4(2) . . ?
C18 C19 C2 122.2(2) . . ?
C18 C20 C4 123.6(2) . . ?
C22B N1B C23B 99(2) . . ?
C24B N1B C22B 105(2) . . ?
C24B N1B C23B 98(2) . . ?
C22A N1A C23A 100(2) . . ?
C24A N1A C22A 102(2) . . ?
C24A N1A C23A 97(2) . . ?

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
O2 C9 C10 C11 -0.5(4) . . . . ?
O2 C9 C10 C12 179.5(2) . . . . ?
O3 C12 C13 C14 180.0(2) . . . . ?
O3 C12 C13 C15 -1.7(3) . . . . ?
C1 C2 C3 C4 -175.8(2) . . . . ?
C1 C2 C3 O1 3.6(4) . . . . ?
C1 C2 C19 O4 -1.5(4) . . . . ?
C1 C2 C19 C18 177.3(2) . . . . ?
C2 C3 C4 C5 180.0(2) . . . 2_655 ?
C2 C3 C4 C20 -1.0(3) . . . . ?
C3 C2 C19 O4 -179.4(2) . . . . ?
C3 C2 C19 C18 -0.7(4) . . . . ?
C3 C4 C20 C18 -1.9(3) . . . . ?
C4 C5 C6 C7 -58.8(3) 2_655 . . . ?
C4 C5 C8 C9 91.3(3) 2_655 . . . ?
C4 C5 C8 C14 -90.2(3) 2_655 . . . ?
C5 C4 C20 C18 177.2(2) 2_655 . . . ?
C5 C8 C9 O2 -2.9(3) . . . . ?
C5 C8 C9 C10 177.4(2) . . . . ?
C5 C8 C14 C13 -176.4(2) . . . . ?
C6 C5 C8 C9 -141.0(2) . . . . ?
C6 C5 C8 C14 37.5(3) . . . . ?
C8 C5 C6 C7 173.8(2) . . . . ?
C8 C9 C10 C11 179.2(2) . . . . ?
C8 C9 C10 C12 -0.8(4) . . . . ?
C9 C8 C14 C13 2.1(3) . . . . ?
C9 C10 C12 O3 -179.1(2) . . . . ?
C9 C10 C12 C13 1.9(4) . . . . ?
C10 C12 C13 C14 -1.0(3) . . . . ?
C10 C12 C13 C15 177.4(2) . . . . ?
C11 C10 C12 O3 1.0(4) . . . . ?
C11 C10 C12 C13 -178.1(2) . . . . ?
C12 C13 C14 C8 -1.1(3) . . . . ?
C12 C13 C15 C16 138.7(2) . . . . ?
C12 C13 C15 C18 -93.7(2) . . . . ?
C13 C15 C16 C17 -60.5(3) . . . . ?
C13 C15 C18 C19 94.0(2) . . . . ?
C13 C15 C18 C20 -85.3(3) . . . . ?
C14 C8 C9 O2 178.5(2) . . . . ?
C14 C8 C9 C10 -1.1(4) . . . . ?
C14 C13 C15 C16 -43.0(3) . . . . ?
C14 C13 C15 C18 84.6(3) . . . . ?
C15 C13 C14 C8 -179.5(2) . . . . ?
C15 C18 C19 O4 -2.6(3) . . . . ?
C15 C18 C19 C2 178.7(2) . . . . ?
C15 C18 C20 C4 -177.3(2) . . . . ?
C16 C15 C18 C19 -137.8(2) . . . . ?
C16 C15 C18 C20 42.8(3) . . . . ?
C18 C15 C16 C17 173.0(2) . . . . ?
C19 C2 C3 C4 2.2(4) . . . . ?
C19 C2 C3 O1 -178.4(2) . . . . ?
C19 C18 C20 C4 3.3(3) . . . . ?
C20 C18 C19 O4 176.8(2) . . . . ?
C20 C18 C19 C2 -1.9(3) . . . . ?
O1 C3 C4 C5 0.6(3) . . . 2_655 ?
O1 C3 C4 C20 179.6(2) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_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
0 -5 -31 0.1229 -0.0232 -5.0489 -31.0219 -0.4160 -0.8962 0.0050
0 5 31 0.1499 0.0232 5.0489 31.0219 0.4160 0.8962 -0.0050
-18 2 -1 0.1770 -17.9699 2.0124 -0.9968 -0.0008 -0.0025 1.0109
18 -2 1 0.1701 17.9699 -2.0124 0.9968 0.0008 0.0025 -1.0109
-2 -21 7 0.0983 -2.0180 -21.0033 7.0193 0.9066 -0.4479 0.0139
2 21 -7 0.0853 2.0180 21.0033 -7.0193 -0.9066 0.4479 -0.0139
14 13 -4 0.1160 13.9913 12.9937 -4.0154 -0.6194 0.3114 -0.7188
-11 16 -6 0.1252 -10.9669 16.0102 -6.0116 -0.6403 0.2996 0.6866
9 -18 6 0.1042 8.9677 -18.0103 6.0134 0.7229 -0.3620 -0.5841
-11 -16 6 0.1460 -10.9985 -15.9950 6.0180 0.7515 -0.3445 0.5372


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items have may been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5b@2
_database_code_depnum_ccdc_archive 'CCDC 1021705'
_audit_update_record             
;
2014-11-07 deposited with the CCDC.
2014-12-03 downloaded from the CCDC.
;

_audit_creation_date             2014-05-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'2(C40 H48 O8), 4(C H4 O), 6(H2 O), Cl, C6 H16 N'
_chemical_formula_sum            'C90 H140 Cl N O26'
_chemical_formula_weight         1687.47
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C46 H64 F6 N1 O8 P1'
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'
Cl Cl 0.3639 0.7018 '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'

_shelx_space_group_comment       
;

The structure is solved and refined in space group Pnnn with Z=2.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           48
_space_group_name_H-M_alt        'P n n n'
_space_group_name_Hall           '-P 2ab 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x, -y+1/2, -z+1/2'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x, y-1/2, z-1/2'
'x-1/2, -y, z-1/2'

_cell_length_a                   12.6356(2)
_cell_length_b                   15.1060(2)
_cell_length_c                   23.0509(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4399.81(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7135
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      75.3540
_cell_measurement_theta_min      3.9790
_shelx_estimated_absorpt_T_max   0.806
_shelx_estimated_absorpt_T_min   0.685
_exptl_absorpt_coefficient_mu    1.023
_exptl_absorpt_correction_T_max  0.822
_exptl_absorpt_correction_T_min  0.715
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       brick
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.22
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13394
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.987
_diffrn_reflns_theta_min         3.498
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0445112000
_diffrn_orient_matrix_UB_12      0.0901459000
_diffrn_orient_matrix_UB_13      -0.0195923000
_diffrn_orient_matrix_UB_21      -0.0625468000
_diffrn_orient_matrix_UB_22      0.0073556000
_diffrn_orient_matrix_UB_23      0.0571726000
_diffrn_orient_matrix_UB_31      0.0947146000
_diffrn_orient_matrix_UB_32      0.0471399000
_diffrn_orient_matrix_UB_33      0.0285220000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3752
_reflns_number_total             4163
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4163
_refine_ls_number_restraints     105
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0677
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1038P)²+4.2008P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1868
_refine_ls_wR_factor_ref         0.1921
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Others
 Fixed Sof: H1B(0.5) H1A(0.5) H4B(0.5) H4A(0.5) O6(0.75) H6A(0.75) C29(0.75)
 H29A(0.75) H29B(0.75) H29C(0.75) O6B(0.25) H6B(0.25) C29B(0.25) H29D(0.25)
 H29E(0.25) H29F(0.25) H7A(0.5) H7B(0.5) Cl1(0.15) O9B(0.75) H9BA(0.75)
 H9BB(0.75) Cl1B(0.1) N1(0.25) H1(0.25) C31(0.25) H31A(0.25) H31B(0.25)
 C30(0.25) H30A(0.25) H30B(0.25) C32(0.25) H32A(0.25) H32B(0.25) H32C(0.25)
 C33(0.25) H33A(0.25) H33B(0.25) H33C(0.25) O10(0.25) H10D(0.25) H10E(0.25)
 C34(0.25) H34A(0.25) H34B(0.25) C35(0.25) H35A(0.25) H35B(0.25) H35C(0.25)
 Fixed U13: O7(0) Cl1(0) N1(0) O10(0)
 Fixed U23: O7(0) Cl1(0) N1(0) O10(0)
 Fixed Uiso: H1B(0.058) H1A(0.058) H2(0.065) H3(0.064) H4B(0.063) H4A(0.063)
 H6(0.032) H7(0.034) H8A(0.037) H8B(0.037) H9A(0.063) H9B(0.063) H9C(0.063)
 H10A(0.074) H10B(0.074) H10C(0.074) H16(0.032) H17(0.033) H18A(0.038)
 H18B(0.038) H19A(0.062) H19B(0.062) H19C(0.062) H20A(0.09) H20B(0.09)
 H20C(0.09) H6A(0.111) H29A(0.168) H29B(0.168) H29C(0.168) H6B(0.118)
 H29D(0.151) H29E(0.151) H29F(0.151) H7A(0.1) H7B(0.1) H9BA(0.141) H9BB(0.141)
 H1(0.089) H31A(0.078) H31B(0.078) H30A(0.088) H30B(0.088) H32A(0.098)
 H32B(0.098) H32C(0.098) H33A(0.11) H33B(0.11) H33C(0.11) H10D(0.063)
 H10E(0.063) H34A(0.153) H34B(0.153) H35A(0.131) H35B(0.131) H35C(0.131)
 Fixed X: H6(0.3933) H7(0.3797) H8A(0.4211) H8B(0.3192) H9A(0.2806)
 H9B(0.3101) H9C(0.2081) H10A(0.697) H10B(0.6524) H10C(0.5931) H16(0.1847) H17(-
 0.0906) H18A(-0.02) H18B(0.0528) H19A(-0.0993) H19B(-0.1734) H19C(-0.1008)
 H20A(0.0519) H20B(0.1466) H20C(0.0308) H6A(0.324) H29A(0.4871) H29B(0.3741)
 H29C(0.4489) H6B(0.347) H29D(0.4852) H29E(0.3721) H29F(0.4207) O7(0.25)
 Cl1(0.25) H9BA(0.2362) H9BB(0.1393) N1(0.25) H1(0.25) H31A(0.2181)
 H31B(0.1183) H30A(0.3763) H30B(0.3711) H32A(0.389) H32B(0.4448) H32C(0.4947)
 H33A(0.227) H33B(0.2811) H33C(0.1569) O10(0.25) H10D(0.2771) H10E(0.3011)
 H34A(0.2844) H34B(0.176) H35A(0.1311) H35B(0.0995) H35C(0.2059)
 Fixed Y: H6(0.299) H7(0.5285) H8A(0.4661) H8B(0.4035) H9A(0.5277) H9B(0.5926)
 H9C(0.5303) H10A(0.4198) H10B(0.3367) H10C(0.4301) H16(0.3662) H17(0.3611)
 H18A(0.4011) H18B(0.3145) H19A(0.2885) H19B(0.3111) H19C(0.2243) H20A(0.6263)
 H20B(0.5819) H20C(0.539) H6A(0.3966) H29A(0.2925) H29B(0.2591) H29C(0.3157)
 H6B(0.3334) H29D(0.3225) H29E(0.2952) H29F(0.2421) O7(0.75) Cl1(0.25)
 H9BA(0.4063) H9BB(0.3649) N1(0.25) H1(0.25) H31A(0.3558) H31B(0.3267)
 H30A(0.3392) H30B(0.2943) H32A(0.1497) H32B(0.2135) H32C(0.2019) H33A(0.4669)
 H33B(0.3989) H33C(0.4184) O10(0.25) H10D(0.2327) H10E(0.3007) H34A(0.1433)
 H34B(0.1922) H35A(0.0639) H35B(0.1529) H35C(0.1015)
 Fixed Z: H6(0.0227) H7(0.0591) H8A(-0.0323) H8B(-0.0282) H9A(-0.0864) H9B(-
 0.034) H9C(-0.0295) H10A(0.1849) H10B(0.2203) H10C(0.224) H16(0.0243)
 H17(0.0611) H18A(-0.0309) H18B(-0.0303) H19A(-0.0868) H19B(-0.0325) H19C(-
 0.0316) H20A(0.1859) H20B(0.2217) H20C(0.2235) H6A(-0.173) H29A(-0.196) H29B(-
 0.1735) H29C(-0.1315) H6B(-0.1196) H29D(-0.1989) H29E(-0.2246) H29F(-0.1708)
 H9BA(-0.1852) H9BB(-0.1697) H1(0.2683) H31A(0.1779) H31B(0.2158) H30A(0.24)
 H30B(0.1765) H32A(0.2358) H32B(0.282) H32C(0.2186) H33A(0.2369) H33B(0.2811)
 H33C(0.2852) H10D(0.3839) H10E(0.3433) H34A(0.1826) H34B(0.164) H35A(0.224)
 H35B(0.2574) H35C(0.2742)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.64588(13) 0.22168(10) 0.14557(8) 0.0384(4) Uani 1 1 d D . . . .
H1B H 0.614(5) 0.172(2) 0.146(3) 0.058 Uiso 0.5 1 d DR . P A -1
H1A H 0.710(2) 0.239(5) 0.147(3) 0.058 Uiso 0.5 1 d DR . P B -2
O2 O 0.48070(15) 0.50682(11) 0.14737(8) 0.0432(4) Uani 1 1 d D . . . .
H2 H 0.536(2) 0.533(2) 0.1581(15) 0.065 Uiso 1 1 d DR . . . .
O3 O 0.28237(14) 0.57726(12) 0.14579(8) 0.0429(4) Uani 1 1 d D . . . .
H3 H 0.3444(13) 0.5550(19) 0.1486(15) 0.064 Uiso 1 1 d DR . . . .
O4 O -0.06247(13) 0.44866(12) 0.14801(8) 0.0420(4) Uani 1 1 d D . . . .
H4B H -0.091(3) 0.398(2) 0.146(3) 0.063 Uiso 0.5 1 d DR . P C -1
H4A H -0.091(5) 0.496(3) 0.162(3) 0.063 Uiso 0.5 1 d DR . P D -2
C1 C 0.51011(15) 0.25483(14) 0.07555(9) 0.0269(4) Uani 1 1 d . . . . .
C2 C 0.57326(17) 0.28086(14) 0.12216(10) 0.0319(5) Uani 1 1 d . . . . .
C3 C 0.56516(19) 0.36461(15) 0.14741(10) 0.0359(5) Uani 1 1 d . . . . .
C4 C 0.49180(18) 0.42359(15) 0.12350(10) 0.0330(5) Uani 1 1 d . . . . .
C5 C 0.42761(16) 0.40113(14) 0.07623(9) 0.0277(4) Uani 1 1 d . . . . .
C6 C 0.43775(15) 0.31617(13) 0.05404(9) 0.0263(4) Uani 1 1 d . . . . .
H6 H 0.3933 0.2990 0.0227 0.032 Uiso 1 1 calc R . . . .
C7 C 0.35122(16) 0.46844(13) 0.04958(9) 0.0282(4) Uani 1 1 d . . . . .
H7 H 0.3797 0.5285 0.0591 0.034 Uiso 1 1 calc R . . . .
C8 C 0.34811(17) 0.46193(14) -0.01693(9) 0.0311(5) Uani 1 1 d . . . . .
H8A H 0.4211 0.4661 -0.0323 0.037 Uiso 1 1 calc R . . . .
H8B H 0.3192 0.4035 -0.0282 0.037 Uiso 1 1 calc R . . . .
C9 C 0.2807(2) 0.53463(17) -0.04414(11) 0.0422(6) Uani 1 1 d . . . . .
H9A H 0.2806 0.5277 -0.0864 0.063 Uiso 1 1 calc R . . . .
H9B H 0.3101 0.5926 -0.0340 0.063 Uiso 1 1 calc R . . . .
H9C H 0.2081 0.5303 -0.0295 0.063 Uiso 1 1 calc R . . . .
C10 C 0.6328(2) 0.39002(18) 0.19862(12) 0.0495(7) Uani 1 1 d . . . . .
H10A H 0.6970 0.4198 0.1849 0.074 Uiso 1 1 calc GR . . . .
H10B H 0.6524 0.3367 0.2203 0.074 Uiso 1 1 calc GR . . . .
H10C H 0.5931 0.4301 0.2240 0.074 Uiso 1 1 calc GR . . . .
C11 C 0.24106(17) 0.46294(13) 0.07665(9) 0.0281(4) Uani 1 1 d . . . . .
C12 C 0.21097(18) 0.51772(15) 0.12254(10) 0.0338(5) Uani 1 1 d D . . . .
C13 C 0.1097(2) 0.51364(17) 0.14737(10) 0.0391(5) Uani 1 1 d . . . . .
C14 C 0.03710(17) 0.45431(16) 0.12358(10) 0.0339(5) Uani 1 1 d D . . . .
C15 C 0.06234(16) 0.39986(13) 0.07652(9) 0.0277(4) Uani 1 1 d . . . . .
C16 C 0.16523(16) 0.40464(13) 0.05513(9) 0.0268(4) Uani 1 1 d . . . . .
H16 H 0.1847 0.3662 0.0243 0.032 Uiso 1 1 calc R . . . .
C17 C -0.01945(16) 0.33793(13) 0.04962(9) 0.0279(4) Uani 1 1 d . . . . .
H17 H -0.0906 0.3611 0.0611 0.033 Uiso 1 1 calc R . . . .
C18 C -0.01577(17) 0.33909(14) -0.01721(9) 0.0317(5) Uani 1 1 d . . . . .
H18A H -0.0200 0.4011 -0.0309 0.038 Uiso 1 1 calc R . . . .
H18B H 0.0528 0.3145 -0.0303 0.038 Uiso 1 1 calc R . . . .
C19 C -0.1053(2) 0.28603(17) -0.04447(11) 0.0414(6) Uani 1 1 d . . . . .
H19A H -0.0993 0.2885 -0.0868 0.062 Uiso 1 1 calc R . . . .
H19B H -0.1734 0.3111 -0.0325 0.062 Uiso 1 1 calc R . . . .
H19C H -0.1008 0.2243 -0.0316 0.062 Uiso 1 1 calc R . . . .
C20 C 0.0824(2) 0.5701(2) 0.19914(13) 0.0598(8) Uani 1 1 d . . . . .
H20A H 0.0519 0.6263 0.1859 0.090 Uiso 1 1 calc GR . . . .
H20B H 0.1466 0.5819 0.2217 0.090 Uiso 1 1 calc DGR . . . .
H20C H 0.0308 0.5390 0.2235 0.090 Uiso 1 1 calc GR . . . .
O6 O 0.3791(3) 0.3860(2) -0.1922(2) 0.0738(9) Uani 0.75 1 d . . P E 2
H6A H 0.3240 0.3966 -0.1730 0.111 Uiso 0.75 1 calc GR . P E 2
C29 C 0.4259(10) 0.3074(6) -0.1718(5) 0.112(3) Uani 0.75 1 d . . P E 2
H29A H 0.4871 0.2925 -0.1960 0.168 Uiso 0.75 1 calc GR . P E 2
H29B H 0.3741 0.2591 -0.1735 0.168 Uiso 0.75 1 calc GR . P E 2
H29C H 0.4489 0.3157 -0.1315 0.168 Uiso 0.75 1 calc GR . P E 2
O6B O 0.3641(9) 0.3604(9) -0.1500(6) 0.079(3) Uani 0.25 1 d . . P F 1
H6B H 0.3470 0.3334 -0.1196 0.118 Uiso 0.25 1 calc GR . P F 1
C29B C 0.414(3) 0.300(2) -0.1891(16) 0.101(6) Uani 0.25 1 d . U P F 1
H29D H 0.4852 0.3225 -0.1989 0.151 Uiso 0.25 1 calc GR . P F 1
H29E H 0.3721 0.2952 -0.2246 0.151 Uiso 0.25 1 calc GR . P F 1
H29F H 0.4207 0.2421 -0.1708 0.151 Uiso 0.25 1 calc GR . P F 1
O7 O 0.2500 0.7500 0.18970(14) 0.0666(9) Uani 1 2 d DS T P . .
H7A H 0.250(9) 0.712(4) 0.165(3) 0.100 Uiso 0.5 1 d DR . P G -1
H7B H 0.213(5) 0.757(8) 0.219(2) 0.100 Uiso 0.5 1 d DR . P H -1
Cl1 Cl 0.2500 0.2500 -0.0716(3) 0.0943(15) Uani 0.3 2 d S T P I 1
O9B O 0.1676(3) 0.4104(3) -0.1869(3) 0.0939(14) Uani 0.75 1 d . . P J 1
H9BA H 0.2362 0.4063 -0.1852 0.141 Uiso 0.75 1 d G . P J 1
H9BB H 0.1393 0.3649 -0.1697 0.141 Uiso 0.75 1 d G . P J 1
Cl1B Cl 0.1776(10) 0.3823(9) -0.1445(8) 0.099(3) Uani 0.1 1 d . . P K 2
N1 N 0.2500 0.2500 0.2315(3) 0.0590(18) Uani 0.5 2 d DS T P . .
H1 H 0.2500 0.2500 0.2683 0.089 Uiso 0.5 2 d DRS T P L .
C31 C 0.1956(9) 0.3371(7) 0.2172(5) 0.065(3) Uani 0.25 1 d D U P L -1
H31A H 0.2181 0.3558 0.1779 0.078 Uiso 0.25 1 calc R . P L -1
H31B H 0.1183 0.3267 0.2158 0.078 Uiso 0.25 1 calc R . P L -1
C30 C 0.3606(7) 0.2840(8) 0.2185(6) 0.073(4) Uani 0.25 1 d D U P L -1
H30A H 0.3763 0.3392 0.2400 0.088 Uiso 0.25 1 calc R . P L -1
H30B H 0.3711 0.2943 0.1765 0.088 Uiso 0.25 1 calc R . P L -1
C32 C 0.4286(9) 0.2050(9) 0.2408(4) 0.065(3) Uani 0.25 1 d D U P L -1
H32A H 0.3890 0.1497 0.2358 0.098 Uiso 0.25 1 calc GR . P L -1
H32B H 0.4448 0.2135 0.2820 0.098 Uiso 0.25 1 calc GR . P L -1
H32C H 0.4947 0.2019 0.2186 0.098 Uiso 0.25 1 calc GR . P L -1
C33 C 0.2170(13) 0.4118(10) 0.2587(7) 0.073(4) Uani 0.25 1 d D U P L -1
H33A H 0.2270 0.4669 0.2369 0.110 Uiso 0.25 1 calc DGR . P L -1
H33B H 0.2811 0.3989 0.2811 0.110 Uiso 0.25 1 calc GR . P L -1
H33C H 0.1569 0.4184 0.2852 0.110 Uiso 0.25 1 calc GR . P L -1
O10 O 0.2500 0.2500 0.3512(2) 0.0419(11) Uani 0.5 2 d DS T P M 1
H10D H 0.2771 0.2327 0.3839 0.063 Uiso 0.25 1 d G . P M 1
H10E H 0.3011 0.3007 0.3433 0.063 Uiso 0.25 1 d DG . P M 1
C34 C 0.221(2) 0.1749(12) 0.1972(9) 0.128(8) Uani 0.25 1 d D U P L -1
H34A H 0.2844 0.1433 0.1826 0.153 Uiso 0.25 1 calc R . P L -1
H34B H 0.1760 0.1922 0.1640 0.153 Uiso 0.25 1 calc R . P L -1
C35 C 0.1586(18) 0.1177(12) 0.2423(8) 0.088(5) Uani 0.25 1 d D U P L -1
H35A H 0.1311 0.0639 0.2240 0.131 Uiso 0.25 1 d R . P L -1
H35B H 0.0995 0.1529 0.2574 0.131 Uiso 0.25 1 d R . P L -1
H35C H 0.2059 0.1015 0.2742 0.131 Uiso 0.25 1 d R . P L -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 H1B 0.84(2) . ?
O1 H1A 0.85(2) . ?
O1 C2 1.390(3) . ?
O2 H2 0.843(19) . ?
O2 C4 1.380(3) . ?
O3 H3 0.855(17) . ?
O3 C12 1.382(3) . ?
O4 H4B 0.85(2) . ?
O4 H4A 0.86(2) . ?
O4 C14 1.381(3) . ?
C1 C2 1.395(3) . ?
C1 C6 1.393(3) . ?
C1 C17 1.528(3) 2 ?
C2 C3 1.396(3) . ?
C3 C4 1.399(3) . ?
C3 C10 1.507(3) . ?
C4 C5 1.400(3) . ?
C5 C6 1.388(3) . ?
C5 C7 1.531(3) . ?
C6 H6 0.9500 . ?
C7 H7 1.0000 . ?
C7 C8 1.537(3) . ?
C7 C11 1.528(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.525(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.396(3) . ?
C11 C16 1.393(3) . ?
C12 C13 1.403(3) . ?
C13 C14 1.395(3) . ?
C13 C20 1.507(3) . ?
C14 C15 1.398(3) . ?
C15 C16 1.392(3) . ?
C15 C17 1.526(3) . ?
C16 H16 0.9500 . ?
C17 C1 1.528(3) 2 ?
C17 H17 1.0000 . ?
C17 C18 1.541(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.522(3) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
O6 H6A 0.8400 . ?
O6 C29 1.408(10) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
O6B H6B 0.8400 . ?
O6B C29B 1.429(18) . ?
C29B H29D 0.9800 . ?
C29B H29E 0.9800 . ?
C29B H29F 0.9800 . ?
O7 H7A 0.81(2) . ?
O7 H7B 0.82(2) . ?
O9B H9BA 0.8701 . ?
O9B H9BB 0.8706 . ?
N1 N1 0.853(12) 3 ?
N1 H1 0.8480 . ?
N1 C31 1.520(8) . ?
N1 C30 1.519(9) . ?
N1 C34 1.429(10) . ?
C31 N1 1.898(10) 3 ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C33 1.505(9) . ?
C30 N1 1.883(10) 3 ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C32 1.558(9) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
O10 H10D 0.8695 . ?
O10 H10E 1.0177 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.567(18) . ?
C35 H35A 0.9801 . ?
C35 H35B 0.9796 . ?
C35 H35C 0.9793 . ?

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 O1 H1B 105(5) . . ?
C2 O1 H1A 116(5) . . ?
C4 O2 H2 118(3) . . ?
C12 O3 H3 111.8(18) . . ?
C14 O4 H4B 114(2) . . ?
C14 O4 H4A 119(5) . . ?
C2 C1 C17 121.05(18) . 2 ?
C6 C1 C2 117.52(19) . . ?
C6 C1 C17 121.43(18) . 2 ?
O1 C2 C1 119.69(19) . . ?
O1 C2 C3 117.98(19) . . ?
C1 C2 C3 122.3(2) . . ?
C2 C3 C4 117.5(2) . . ?
C2 C3 C10 121.0(2) . . ?
C4 C3 C10 121.5(2) . . ?
O2 C4 C3 119.4(2) . . ?
O2 C4 C5 118.2(2) . . ?
C3 C4 C5 122.4(2) . . ?
C4 C5 C7 121.11(19) . . ?
C6 C5 C4 117.22(19) . . ?
C6 C5 C7 121.66(18) . . ?
C1 C6 H6 118.5 . . ?
C5 C6 C1 123.00(19) . . ?
C5 C6 H6 118.5 . . ?
C5 C7 H7 106.7 . . ?
C5 C7 C8 111.96(17) . . ?
C8 C7 H7 106.7 . . ?
C11 C7 C5 111.99(17) . . ?
C11 C7 H7 106.7 . . ?
C11 C7 C8 112.37(17) . . ?
C7 C8 H8A 109.2 . . ?
C7 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
C9 C8 C7 112.25(19) . . ?
C9 C8 H8A 109.2 . . ?
C9 C8 H8B 109.2 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C3 C10 H10A 109.5 . . ?
C3 C10 H10B 109.5 . . ?
C3 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C7 121.70(19) . . ?
C16 C11 C7 121.06(18) . . ?
C16 C11 C12 117.2(2) . . ?
O3 C12 C11 120.1(2) . . ?
O3 C12 C13 117.8(2) . . ?
C11 C12 C13 122.1(2) . . ?
C12 C13 C20 120.5(2) . . ?
C14 C13 C12 117.9(2) . . ?
C14 C13 C20 121.6(2) . . ?
O4 C14 C13 118.6(2) . . ?
O4 C14 C15 119.21(19) . . ?
C13 C14 C15 122.2(2) . . ?
C14 C15 C17 121.43(19) . . ?
C16 C15 C14 117.21(19) . . ?
C16 C15 C17 121.36(18) . . ?
C11 C16 H16 118.3 . . ?
C15 C16 C11 123.31(19) . . ?
C15 C16 H16 118.3 . . ?
C1 C17 H17 106.7 2 . ?
C1 C17 C18 113.53(17) 2 . ?
C15 C17 C1 110.55(16) . 2 ?
C15 C17 H17 106.7 . . ?
C15 C17 C18 112.26(17) . . ?
C18 C17 H17 106.7 . . ?
C17 C18 H18A 109.1 . . ?
C17 C18 H18B 109.1 . . ?
H18A C18 H18B 107.8 . . ?
C19 C18 C17 112.59(18) . . ?
C19 C18 H18A 109.1 . . ?
C19 C18 H18B 109.1 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C13 C20 H20A 109.5 . . ?
C13 C20 H20B 109.5 . . ?
C13 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C29 O6 H6A 109.5 . . ?
O6 C29 H29A 109.5 . . ?
O6 C29 H29B 109.5 . . ?
O6 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C29B O6B H6B 109.5 . . ?
O6B C29B H29D 109.5 . . ?
O6B C29B H29E 109.5 . . ?
O6B C29B H29F 109.5 . . ?
H29D C29B H29E 109.5 . . ?
H29D C29B H29F 109.5 . . ?
H29E C29B H29F 109.5 . . ?
H7A O7 H7B 131(10) . . ?
H9BA O9B H9BB 109.5 . . ?
N1 N1 H1 0.0 3 . ?
N1 N1 C31 102.5(5) 3 . ?
N1 N1 C30 101.4(6) 3 . ?
N1 N1 C34 123.6(9) 3 . ?
C31 N1 H1 102.5 . . ?
C30 N1 H1 101.4 . . ?
C30 N1 C31 94.6(6) . . ?
C34 N1 H1 123.6 . . ?
C34 N1 C31 116.8(12) . . ?
C34 N1 C30 113.2(11) . . ?
N1 C31 N1 26.0(4) . 3 ?
N1 C31 H31A 108.4 . . ?
N1 C31 H31A 131.6 3 . ?
N1 C31 H31B 108.4 . . ?
N1 C31 H31B 105.5 3 . ?
H31A C31 H31B 107.5 . . ?
C33 C31 N1 93.3(9) . 3 ?
C33 C31 N1 115.5(10) . . ?
C33 C31 H31A 108.4 . . ?
C33 C31 H31B 108.4 . . ?
N1 C30 N1 26.4(4) . 3 ?
N1 C30 H30A 94.0 3 . ?
N1 C30 H30A 111.7 . . ?
N1 C30 H30B 111.7 . . ?
N1 C30 H30B 137.8 3 . ?
N1 C30 C32 100.5(7) . . ?
H30A C30 H30B 109.4 . . ?
C32 C30 N1 89.9(6) . 3 ?
C32 C30 H30A 111.7 . . ?
C32 C30 H30B 111.7 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
H10D O10 H10E 97.5 . . ?
N1 C34 H34A 111.5 . . ?
N1 C34 H34B 111.5 . . ?
N1 C34 C35 101.5(13) . . ?
H34A C34 H34B 109.3 . . ?
C35 C34 H34A 111.5 . . ?
C35 C34 H34B 111.5 . . ?
C34 C35 H35A 110.5 . . ?
C34 C35 H35B 108.8 . . ?
C34 C35 H35C 109.1 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?

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 C2 C3 C4 -180.0(2) . . . . ?
O1 C2 C3 C10 -0.2(4) . . . . ?
O2 C4 C5 C6 -178.05(19) . . . . ?
O2 C4 C5 C7 3.2(3) . . . . ?
O3 C12 C13 C14 179.3(2) . . . . ?
O3 C12 C13 C20 -2.3(4) . . . . ?
O4 C14 C15 C16 -176.88(19) . . . . ?
O4 C14 C15 C17 3.3(3) . . . . ?
C1 C2 C3 C4 -1.2(4) . . . . ?
C1 C2 C3 C10 178.6(2) . . . . ?
C1 C17 C18 C19 60.5(2) 2 . . . ?
C2 C1 C6 C5 1.1(3) . . . . ?
C2 C3 C4 O2 179.6(2) . . . . ?
C2 C3 C4 C5 0.3(4) . . . . ?
C3 C4 C5 C6 1.2(3) . . . . ?
C3 C4 C5 C7 -177.6(2) . . . . ?
C4 C5 C6 C1 -1.9(3) . . . . ?
C4 C5 C7 C8 140.6(2) . . . . ?
C4 C5 C7 C11 -92.1(2) . . . . ?
C5 C7 C8 C9 -174.33(18) . . . . ?
C5 C7 C11 C12 94.7(2) . . . . ?
C5 C7 C11 C16 -87.4(2) . . . . ?
C6 C1 C2 O1 179.31(19) . . . . ?
C6 C1 C2 C3 0.5(3) . . . . ?
C6 C5 C7 C8 -38.2(3) . . . . ?
C6 C5 C7 C11 89.1(2) . . . . ?
C7 C5 C6 C1 176.84(18) . . . . ?
C7 C11 C12 O3 -1.8(3) . . . . ?
C7 C11 C12 C13 179.5(2) . . . . ?
C7 C11 C16 C15 -177.03(18) . . . . ?
C8 C7 C11 C12 -138.3(2) . . . . ?
C8 C7 C11 C16 39.7(3) . . . . ?
C10 C3 C4 O2 -0.3(4) . . . . ?
C10 C3 C4 C5 -179.5(2) . . . . ?
C11 C7 C8 C9 58.6(2) . . . . ?
C11 C12 C13 C14 -2.0(4) . . . . ?
C11 C12 C13 C20 176.4(3) . . . . ?
C12 C11 C16 C15 1.0(3) . . . . ?
C12 C13 C14 O4 179.2(2) . . . . ?
C12 C13 C14 C15 0.0(4) . . . . ?
C13 C14 C15 C16 2.2(3) . . . . ?
C13 C14 C15 C17 -177.6(2) . . . . ?
C14 C15 C16 C11 -2.8(3) . . . . ?
C14 C15 C17 C1 -95.1(2) . . . 2 ?
C14 C15 C17 C18 137.1(2) . . . . ?
C15 C17 C18 C19 -173.26(18) . . . . ?
C16 C11 C12 O3 -179.81(19) . . . . ?
C16 C11 C12 C13 1.5(3) . . . . ?
C16 C15 C17 C1 85.1(2) . . . 2 ?
C16 C15 C17 C18 -42.8(3) . . . . ?
C17 C1 C2 O1 -0.1(3) 2 . . . ?
C17 C1 C2 C3 -178.8(2) 2 . . . ?
C17 C1 C6 C5 -179.53(18) 2 . . . ?
C17 C15 C16 C11 177.08(18) . . . . ?
C20 C13 C14 O4 0.8(4) . . . . ?
C20 C13 C14 C15 -178.3(3) . . . . ?
N1 N1 C31 C33 34.1(11) 3 . . . ?
N1 N1 C30 C32 67.7(8) 3 . . . ?
N1 N1 C34 C35 19(2) 3 . . . ?
C31 N1 C30 N1 103.8(5) . . . 3 ?
C31 N1 C30 C32 171.5(9) . . . . ?
C31 N1 C34 C35 -110.3(17) . . . . ?
C30 N1 C31 N1 -102.8(7) . . . 3 ?
C30 N1 C31 C33 -68.6(13) . . . . ?
C30 N1 C34 C35 141.4(14) . . . . ?
C34 N1 C31 N1 138.4(10) . . . 3 ?
C34 N1 C31 C33 172.5(14) . . . . ?
C34 N1 C30 N1 -134.4(12) . . . 3 ?
C34 N1 C30 C32 -66.7(15) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_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
-7 -4 -4 0.2087 -7.0000 -4.0000 -4.0002 0.0294 0.1797 -0.9657
-3 4 13 0.1265 -3.0000 4.0000 13.0001 0.2394 0.9603 0.2752
0 -2 15 0.0810 -0.0000 -2.0000 15.0000 -0.4742 0.8429 0.3336
0 2 -15 0.1073 0.0000 2.0000 -15.0000 0.4742 -0.8429 -0.3336
5 -8 -2 0.1278 5.0000 -8.0000 -2.0001 -0.9045 -0.4859 0.0394
7 4 6 0.2001 7.0000 4.0000 6.0002 -0.0686 -0.0654 1.0227
-5 8 2 0.1246 -5.0000 8.0000 2.0001 0.9045 0.4859 -0.0394
-1 -9 -6 0.1465 -1.0000 -9.0000 -6.0002 -0.6492 -0.3467 -0.6901
2 9 6 0.1346 2.0000 9.0000 6.0002 0.6047 0.2842 0.7848
-1 8 -9 0.1000 -1.0000 8.0000 -8.9999 0.9420 -0.3932 0.0257
3 -5 11 0.1138 3.0000 -5.0000 11.0000 -0.7998 0.4045 0.3622
0 -8 9 0.1248 0.0000 -8.0000 8.9999 -0.8975 0.4557 -0.1204
3 9 -5 0.1293 3.0000 9.0000 -4.9998 0.7757 -0.4073 0.5658
-6 -7 -3 0.1775 -6.0000 -7.0000 -3.0002 -0.3052 0.1523 -0.9838
5 2 -12 0.1431 5.0000 2.0000 -11.9999 0.1928 -0.9841 0.2256
-7 -4 2 0.1919 -7.0000 -4.0000 1.9998 -0.0882 0.5227 -0.7945
5 -5 -8 0.1329 5.0000 -5.0000 -8.0000 -0.5165 -0.8069 0.0097
0 -5 -13 0.1380 0.0000 -5.0000 -13.0001 -0.1960 -0.7800 -0.6065

_vrf_PLAT417_5b@2                
;
PROBLEM: Short Inter D-H..H-D       H2     ..  H6A     ..       2.09 Ang.  
RESPONSE: The H atoms with short intermolecular distance are involved in disorder.
;
_vrf_PLAT420_5b@2                
;
PROBLEM: D-H Without Acceptor      >O9B    -  >H9BB   ...     Please Check 
RESPONSE: D-H without acceptor is caused by disorder.
;

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items have may been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5b@3
_database_code_depnum_ccdc_archive 'CCDC 1021706'
_audit_update_record             
;
2014-11-07 deposited with the CCDC.
2014-12-03 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT417_5b@3                
;
PROBLEM: Short Inter D-H..H-D       H8     ..  H15B    ..       1.96 Ang.  
RESPONSE: H15B belongs to the disordered solvent water molecule.
;
_vrf_PLAT420_5b@3                
;
PROBLEM: D-H Without Acceptor       O15    -   H15B   ...     Please Check 
RESPONSE: H15 is hydrogen bonding to a disordered solvent water O.
;
# end Validation Reply Form

_audit_creation_date             2014-08-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(C36 H40 O12), 8.6(H2 O), C6 H16 N, Cl, 3(O)'
_chemical_formula_sum            'C78 H113.20 Cl N O35.60'
_chemical_formula_weight         1669.94
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C80 H80 N8 O3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.1484 0.1585 '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 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.48122(17)
_cell_length_b                   11.7421(2)
_cell_length_c                   17.0131(3)
_cell_angle_alpha                102.6693(14)
_cell_angle_beta                 92.3148(13)
_cell_angle_gamma                102.5625(14)
_cell_volume                     2174.82(6)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    22953
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.3310
_cell_measurement_theta_min      3.9340
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85217
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             890
_exptl_crystal_size_max          0.1924
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.0726
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42658
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.639
_diffrn_reflns_theta_min         1.825
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector_area_resol_mean 5.1977
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -69.00   31.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176   57.0000  -60.0000 100

#__ type_ start__ end____ width___ exp.time_
  2 omega  -64.00   -9.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176  -77.0000   30.0000 55

#__ type_ start__ end____ width___ exp.time_
  3 omega  -48.00   27.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176   37.0000   60.0000 75

#__ type_ start__ end____ width___ exp.time_
  4 omega  -45.00   24.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176   37.0000 -150.0000 69

#__ type_ start__ end____ width___ exp.time_
  5 omega -112.00  -66.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176  -77.0000  -90.0000 46

#__ type_ start__ end____ width___ exp.time_
  6 omega  -47.00   -9.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176  -77.0000  -90.0000 38

#__ type_ start__ end____ width___ exp.time_
  7 omega  -89.00   -4.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176  125.0000   60.0000 85

#__ type_ start__ end____ width___ exp.time_
  8 omega  -42.00  -10.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176  -77.0000 -180.0000 32

#__ type_ start__ end____ width___ exp.time_
  9 omega   20.00   49.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.1176   37.0000   90.0000 29

#__ type_ start__ end____ width___ exp.time_
 10 omega   10.00   51.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.1176   77.0000   60.0000 41

#__ type_ start__ end____ width___ exp.time_
 11 omega   13.00   62.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.1176   57.0000   30.0000 49

#__ type_ start__ end____ width___ exp.time_
 12 omega   10.00   97.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.1176   77.0000 -180.0000 87

#__ type_ start__ end____ width___ exp.time_
 13 omega   13.00  112.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.1176   57.0000  -60.0000 99

#__ type_ start__ end____ width___ exp.time_
 14 omega   58.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.1176   77.0000   60.0000 38

#__ type_ start__ end____ width___ exp.time_
 15 omega   13.00  112.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.1176   57.0000  150.0000 99

#__ type_ start__ end____ width___ exp.time_
 16 omega   57.00   83.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.1176   37.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
 17 omega   49.00   80.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.1176  -99.0000  -60.0000 31

#__ type_ start__ end____ width___ exp.time_
 18 omega   82.00  112.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.1176   57.0000   30.0000 30

#__ type_ start__ end____ width___ exp.time_
 19 omega   79.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000    0.0000 99

#__ type_ start__ end____ width___ exp.time_
 20 omega   58.00  115.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000 -120.0000 57

#__ type_ start__ end____ width___ exp.time_
 21 omega   83.00  156.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000  120.0000 73

#__ type_ start__ end____ width___ exp.time_
 22 omega  116.00  170.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000   60.0000 54

#__ type_ start__ end____ width___ exp.time_
 23 omega  109.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000 -150.0000 68

#__ type_ start__ end____ width___ exp.time_
 24 omega   79.00  111.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  150.0000 32

#__ type_ start__ end____ width___ exp.time_
 25 omega   31.00   88.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000 -180.0000 57

#__ type_ start__ end____ width___ exp.time_
 26 omega  140.00  172.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  120.0000 32

#__ type_ start__ end____ width___ exp.time_
 27 omega   50.00  143.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000  -30.0000 93

#__ type_ start__ end____ width___ exp.time_
 28 omega   79.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000   30.0000 27

#__ type_ start__ end____ width___ exp.time_
 29 omega  117.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000   30.0000 60

#__ type_ start__ end____ width___ exp.time_
 30 omega   79.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000 -150.0000 28

#__ type_ start__ end____ width___ exp.time_
 31 omega   79.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000   60.0000 28

#__ type_ start__ end____ width___ exp.time_
 32 omega   84.00  115.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   55.0000   47.7696 31

#__ type_ start__ end____ width___ exp.time_
 33 omega  130.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000   90.0000 48

#__ type_ start__ end____ width___ exp.time_
 34 omega  115.00  172.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  -60.0000 57

#__ type_ start__ end____ width___ exp.time_
 35 omega   86.00  176.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  150.0000 90

#__ type_ start__ end____ width___ exp.time_
 36 omega  144.00  176.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  -30.0000 32

#__ type_ start__ end____ width___ exp.time_
 37 omega   83.00  137.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000    0.0000 54

#__ type_ start__ end____ width___ exp.time_
 38 omega   83.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
 39 omega   79.00  105.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  -30.0000 26

#__ type_ start__ end____ width___ exp.time_
 40 omega   84.00  164.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000  -30.0000 80

#__ type_ start__ end____ width___ exp.time_
 41 omega   53.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  -90.0000 56

#__ type_ start__ end____ width___ exp.time_
 42 omega   79.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  -60.0000 28

#__ type_ start__ end____ width___ exp.time_
 43 omega   91.00  116.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000   90.0000 25

#__ type_ start__ end____ width___ exp.time_
 44 omega   79.00  105.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
 45 omega   83.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000 -180.0000 94

#__ type_ start__ end____ width___ exp.time_
 46 omega   83.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
 47 omega   72.00  114.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000    0.0000 42

#__ type_ start__ end____ width___ exp.time_
 48 omega  122.00  147.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  150.0000 25

#__ type_ start__ end____ width___ exp.time_
 49 omega  116.00  174.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000 -120.0000 58

#__ type_ start__ end____ width___ exp.time_
 50 omega   83.00  134.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000   30.0000 51

#__ type_ start__ end____ width___ exp.time_
 51 omega   42.00  114.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  150.0000 72

#__ type_ start__ end____ width___ exp.time_
 52 omega   79.00  105.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  120.0000 26

#__ type_ start__ end____ width___ exp.time_
 53 omega   83.00  111.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000 -150.0000 28

#__ type_ start__ end____ width___ exp.time_
 54 omega   83.00  151.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000 -120.0000 68

#__ type_ start__ end____ width___ exp.time_
 55 omega   79.00  105.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
 56 omega   83.00  160.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000   90.0000 77

#__ type_ start__ end____ width___ exp.time_
 57 omega   83.00  110.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000  150.0000 27

#__ type_ start__ end____ width___ exp.time_
 58 omega  130.00  156.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 59 omega   83.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
 60 omega   42.00   99.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -30.0000 57

#__ type_ start__ end____ width___ exp.time_
 61 omega   79.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  -90.0000 98

#__ type_ start__ end____ width___ exp.time_
 62 omega   79.00  105.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 63 omega   48.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  -60.0000 33

#__ type_ start__ end____ width___ exp.time_
 64 omega   51.00   77.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
 65 omega   83.00  108.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   67.0000  -58.7440 25

#__ type_ start__ end____ width___ exp.time_
 66 omega   80.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   73.0000  -93.1715 27
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.1220228000
_diffrn_orient_matrix_UB_12      -0.0145601000
_diffrn_orient_matrix_UB_13      -0.0298444000
_diffrn_orient_matrix_UB_21      -0.0638130000
_diffrn_orient_matrix_UB_22      -0.1101861000
_diffrn_orient_matrix_UB_23      -0.0666428000
_diffrn_orient_matrix_UB_31      -0.0100027000
_diffrn_orient_matrix_UB_32      0.0822237000
_diffrn_orient_matrix_UB_33      -0.0579338000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8267
_reflns_number_total             9085
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.672
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         9085
_refine_ls_number_restraints     111
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0871
_refine_ls_restrained_S_all      1.398
_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)+(0.1531P)²+3.4013P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2544
_refine_ls_wR_factor_ref         0.2596
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C41-C42
 1.54 with sigma of 0.02
 C39-C41
 2.2 with sigma of 0.02
 N1-C41
 1.45 with sigma of 0.02
 N1-C42
 2.6 with sigma of 0.02
 O14A-H14A = O14A-H14B = O16B-H16C = O16B-H16D = O16A-H16A = O16A-H16B
 0.84 with sigma of 0.001
 H14A-H14B = H16C-H16D = H16A-H16B
 1.4 with sigma of 0.01
 H7-H8 = H7-H1_$1
 2.1 with sigma of 0.001
 C37-C38 \\sim C39-C40 \\sim C41-C42 \\sim C43-C44
 with sigma of 0.02
 N1-C37 \\sim N1-C39 \\sim N1-C41 \\sim N1-C43
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O17B) \\sim Ueq, Uanis(O16B) \\sim Ueq, Uanis(O18C) \\sim Ueq: with sigma
of 0.002 and sigma for terminal atoms of 0.004
Uanis(O18B) \\sim Ueq, Uanis(O17A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C41) \\sim Ueq, Uanis(C44) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(O17A) \\sim Ueq, Uanis(O18A)
\\sim Ueq, Uanis(O17B) \\sim Ueq, Uanis(O17B) \\sim Ueq, Uanis(O18) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C38) = Uanis(C44)
4. Others
 Fixed Sof: O13A(0.6) H13A(0.6) H13B(0.6) O14A(0.6) H14A(0.6) H14B(0.6)
 O13B(0.4) H13C(0.4) H13D(0.4) O14B(0.4) H14C(0.4) H14D(0.4) O16A(0.6)
 H16A(0.6) H16B(0.6) O16B(0.4) H16C(0.4) H16D(0.4) C37(0.5) H37A(0.5) H37B(0.5)
 C38(0.5) H38A(0.5) H38B(0.5) H38C(0.5) C39(0.3) H39A(0.3) H39B(0.3) C40(0.3)
 H40A(0.3) H40B(0.3) H40C(0.3) C41(0.2) H41A(0.2) H41B(0.2) C42(0.2) H42A(0.2)
 H42B(0.2) H42C(0.2) C43(0.5) H43A(0.5) H43B(0.5) C44(0.5) H44A(0.5) H44B(0.5)
 H44C(0.5) H41C(0.3) H39C(0.2) O18A(0.15) O17A(0.1) O17B(0.15) O18B(0.1)
 O18(0.3) H18D(0.3) H18E(0.3) O18C(0.75) O17C(0.75)
5.a Riding coordinates:
 O3(H3), O4(H4), O5(H5), O9(H9), O10(H10), O13A(H13A,H13B), O13B(H13C,H13D),
 O14B(H14C,H14D), O15(H15A,H15B), O16A(H16A,H16B), O16B(H16C,H16D), N1(H41C),
 N1(H39C), O18(H18D,H18E)
5.b Ternary CH refined with riding coordinates:
 C7(H7A), C16(H16), C25(H25), C34(H34)
5.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C17(H17A,H17B), C26(H26A,H26B), C35(H35A,H35B), C37(H37A,H37B),
 C39(H39A,H39B), C41(H41A,H41B), C43(H43A,H43B)
5.d Aromatic/amide H refined with riding coordinates:
 C4(H4A), C15(H15), C24(H24), C33(H33)
5.e Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C36(H36A,H36B,
 H36C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C44(H44A,
 H44B,H44C)
5.f Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O6(H6), O7(H7), O8(H8), O11(H11), O12(H12)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.27537(19) 0.31608(18) 0.10361(12) 0.0314(4) Uani 1 1 d . . . . .
H1 H 0.2118 0.2891 0.0727 0.047 Uiso 1 1 calc DGR . . . .
O2 O 0.08290(17) 0.21341(16) 0.17269(12) 0.0277(4) Uani 1 1 d . . . . .
H2 H 0.0830 0.2072 0.1226 0.042 Uiso 1 1 calc GR . . . .
O3 O 0.41556(18) 0.53171(17) 0.17611(13) 0.0315(4) Uani 1 1 d . . . . .
H3 H 0.4260 0.6065 0.1846 0.047 Uiso 1 1 d R . . . .
O4 O -0.3522(2) 0.17262(18) 0.13934(15) 0.0419(6) Uani 1 1 d . . . . .
H4 H -0.4240 0.1723 0.1468 0.063 Uiso 1 1 d R . . . .
O5 O -0.15247(19) 0.13339(18) 0.20477(15) 0.0398(5) Uani 1 1 d . . . . .
H5 H -0.0811 0.1399 0.1942 0.060 Uiso 1 1 d R . . . .
O6 O -0.4227(2) 0.37837(18) 0.18960(15) 0.0399(5) Uani 1 1 d . . . . .
H6 H -0.4190 0.4476 0.1826 0.060 Uiso 1 1 calc GR . . . .
O7 O -0.21195(18) 0.78105(19) 0.08140(11) 0.0316(4) Uani 1 1 d . . . . .
H7 H -0.2227 0.7125 0.0504 0.047 Uiso 1 1 calc DGR . . . .
O8 O -0.33279(16) 0.60631(17) 0.15058(11) 0.0269(4) Uani 1 1 d . . . . .
H8 H -0.3592 0.6330 0.1133 0.040 Uiso 1 1 calc DGR . . . .
O9 O -0.01588(18) 0.94290(19) 0.15892(12) 0.0316(4) Uani 1 1 d . . . . .
H9 H 0.0581 0.9625 0.1726 0.047 Uiso 1 1 d R . . . .
O10 O 0.4185(2) 0.9423(2) 0.14673(16) 0.0430(6) Uani 1 1 d . . . . .
H10 H 0.4026 1.0077 0.1436 0.064 Uiso 1 1 d R . . . .
O11 O 0.22305(18) 1.02749(19) 0.19913(14) 0.0351(5) Uani 1 1 d . . . . .
H11 H 0.2726 1.0938 0.2152 0.053 Uiso 1 1 calc GR . . . .
O12 O 0.49397(19) 0.77425(19) 0.21129(15) 0.0374(5) Uani 1 1 d . . . . .
H12 H 0.5540 0.8323 0.2193 0.056 Uiso 1 1 calc GR . . . .
O13A O 0.4054(4) 0.1318(4) 0.0829(2) 0.0437(9) Uani 0.6 1 d . . . A 1
H13A H 0.3655 0.1858 0.1062 0.065 Uiso 0.6 1 d R . . A 1
H13B H 0.4361 0.1591 0.0428 0.065 Uiso 0.6 1 d R . . A 1
O14A O -0.3664(4) 0.9330(4) 0.0831(2) 0.0457(9) Uani 0.6 1 d D . . B 1
H14A H -0.390(6) 0.933(6) 0.0356(11) 0.069 Uiso 0.6 1 d DR . . C 1
H14B H -0.323(3) 0.884(3) 0.085(3) 0.069 Uiso 0.6 1 d DR . . D 1
O13B O 0.4925(7) 0.8230(7) 0.0004(4) 0.0608(18) Uani 0.4 1 d . . . E 2
H13C H 0.4277 0.8161 0.0197 0.091 Uiso 0.4 1 d R . . E 2
H13D H 0.4826 0.7733 -0.0429 0.091 Uiso 0.4 1 d R . . E 2
O14B O 0.3220(8) 0.9937(8) 0.0064(4) 0.0634(19) Uani 0.4 1 d . . . F 2
H14C H 0.2482 0.9906 0.0169 0.095 Uiso 0.4 1 d R . . F 2
H14D H 0.3562 1.0661 0.0032 0.095 Uiso 0.4 1 d R . . F 2
O15 O 0.5565(3) 0.6158(4) 0.00182(19) 0.0774(11) Uani 1 1 d . . . . .
H15A H 0.5894 0.6180 -0.0419 0.116 Uiso 1 1 d R . . . .
H15B H 0.5370 0.6732 0.0344 0.116 Uiso 1 1 d R . . . .
O16A O -0.1092(5) 0.9212(4) -0.0203(3) 0.0578(12) Uani 0.6 1 d D . . G 1
H16A H -0.0365 0.9208 -0.0066 0.087 Uiso 0.6 1 d DR . . G 1
H16B H -0.1512 0.9364 0.0240 0.087 Uiso 0.6 1 d DR . . G 1
O16B O -0.0016(9) 0.8359(9) -0.0116(5) 0.081(2) Uani 0.4 1 d D U . H 2
H16C H 0.0658 0.8837 -0.0072 0.121 Uiso 0.4 1 d DR . . H 2
H16D H 0.0041 0.7657 -0.0117 0.121 Uiso 0.4 1 d DR . . H 2
C1 C 0.2505(2) 0.3760(2) 0.17742(15) 0.0230(5) Uani 1 1 d . . . . .
C2 C 0.1522(2) 0.3224(2) 0.21266(15) 0.0211(5) Uani 1 1 d . . . . .
C3 C 0.1255(2) 0.3793(2) 0.28846(15) 0.0204(5) Uani 1 1 d . . . . .
C4 C 0.1984(2) 0.4909(2) 0.32661(15) 0.0217(5) Uani 1 1 d . . . . .
H4A H 0.1807 0.5301 0.3782 0.026 Uiso 1 1 calc R . . . .
C5 C 0.2965(2) 0.5475(2) 0.29207(15) 0.0211(5) Uani 1 1 d . . . . .
C6 C 0.3215(2) 0.4880(2) 0.21629(15) 0.0224(5) Uani 1 1 d . . . . .
C7 C 0.0166(2) 0.3191(2) 0.32541(15) 0.0222(5) Uani 1 1 d . . . . .
H7A H 0.0121 0.2309 0.3108 0.027 Uiso 1 1 calc R . . . .
C8 C 0.0284(2) 0.3578(2) 0.41821(16) 0.0270(5) Uani 1 1 d . . . . .
H8A H 0.1067 0.3488 0.4393 0.032 Uiso 1 1 calc R . . . .
H8B H 0.0271 0.4438 0.4348 0.032 Uiso 1 1 calc R . . . .
C9 C -0.0713(3) 0.2849(3) 0.45550(19) 0.0366(7) Uani 1 1 d . . . . .
H9A H -0.0745 0.1992 0.4359 0.055 Uiso 1 1 calc GR . . . .
H9B H -0.1481 0.3013 0.4401 0.055 Uiso 1 1 calc GR . . . .
H9C H -0.0554 0.3073 0.5146 0.055 Uiso 1 1 calc GR . . . .
C10 C -0.0984(2) 0.3377(2) 0.28766(15) 0.0223(5) Uani 1 1 d . . . . .
C11 C -0.1747(2) 0.2458(2) 0.23042(17) 0.0266(5) Uani 1 1 d . . . . .
C12 C -0.2804(2) 0.2637(2) 0.19684(18) 0.0291(6) Uani 1 1 d . . . . .
C13 C -0.3129(2) 0.3726(2) 0.22223(17) 0.0268(5) Uani 1 1 d . . . . .
C14 C -0.2381(2) 0.4667(2) 0.27891(15) 0.0219(5) Uani 1 1 d . . . . .
C15 C -0.1308(2) 0.4474(2) 0.30920(15) 0.0220(5) Uani 1 1 d . . . . .
H15 H -0.0775 0.5120 0.3462 0.026 Uiso 1 1 calc R . . . .
C16 C -0.2721(2) 0.5868(2) 0.30810(15) 0.0215(5) Uani 1 1 d . . . . .
H16 H -0.3577 0.5749 0.2876 0.026 Uiso 1 1 calc R . . . .
C17 C -0.2656(2) 0.6246(2) 0.40066(16) 0.0265(5) Uani 1 1 d . . . . .
H17A H -0.1825 0.6332 0.4233 0.032 Uiso 1 1 calc R . . . .
H17B H -0.2854 0.7040 0.4165 0.032 Uiso 1 1 calc R . . . .
C18 C -0.3504(3) 0.5355(3) 0.4372(2) 0.0378(7) Uani 1 1 d . . . . .
H18A H -0.4321 0.5218 0.4120 0.057 Uiso 1 1 calc GR . . . .
H18B H -0.3485 0.5680 0.4956 0.057 Uiso 1 1 calc GR . . . .
H18C H -0.3252 0.4594 0.4276 0.057 Uiso 1 1 calc GR . . . .
C19 C -0.1993(2) 0.6832(2) 0.27116(14) 0.0191(5) Uani 1 1 d . . . . .
C20 C -0.2351(2) 0.6889(2) 0.19289(15) 0.0212(5) Uani 1 1 d . . . . .
C21 C -0.1725(2) 0.7770(2) 0.15797(15) 0.0231(5) Uani 1 1 d . . . . .
C22 C -0.0703(2) 0.8590(2) 0.19893(15) 0.0216(5) Uani 1 1 d . . . . .
C23 C -0.0304(2) 0.8541(2) 0.27648(14) 0.0195(5) Uani 1 1 d . . . . .
C24 C -0.0968(2) 0.7661(2) 0.31092(14) 0.0195(5) Uani 1 1 d . . . . .
H24 H -0.0708 0.7627 0.3639 0.023 Uiso 1 1 calc R . . . .
C25 C 0.0839(2) 0.9419(2) 0.31967(15) 0.0216(5) Uani 1 1 d . . . . .
H25 H 0.0880 1.0188 0.3025 0.026 Uiso 1 1 calc R . . . .
C26 C 0.0838(2) 0.9710(2) 0.41214(16) 0.0261(5) Uani 1 1 d . . . . .
H26A H 0.0088 0.9952 0.4270 0.031 Uiso 1 1 calc R . . . .
H26B H 0.0855 0.8979 0.4317 0.031 Uiso 1 1 calc R . . . .
C27 C 0.1905(3) 1.0711(3) 0.4539(2) 0.0405(7) Uani 1 1 d . . . . .
H27A H 0.1899 1.1434 0.4342 0.061 Uiso 1 1 calc GR . . . .
H27B H 0.2650 1.0458 0.4418 0.061 Uiso 1 1 calc GR . . . .
H27C H 0.1853 1.0885 0.5125 0.061 Uiso 1 1 calc GR . . . .
C28 C 0.1935(2) 0.8967(2) 0.29112(15) 0.0213(5) Uani 1 1 d . . . . .
C29 C 0.2588(2) 0.9423(2) 0.23335(17) 0.0259(5) Uani 1 1 d . . . . .
C30 C 0.3578(2) 0.9005(2) 0.20584(18) 0.0290(6) Uani 1 1 d . . . . .
C31 C 0.3956(2) 0.8147(2) 0.23924(17) 0.0271(5) Uani 1 1 d . . . . .
C32 C 0.3322(2) 0.7669(2) 0.29704(15) 0.0222(5) Uani 1 1 d . . . . .
C33 C 0.2304(2) 0.8072(2) 0.32080(15) 0.0210(5) Uani 1 1 d . . . . .
H33 H 0.1846 0.7725 0.3585 0.025 Uiso 1 1 calc R . . . .
C34 C 0.3728(2) 0.6716(2) 0.33275(16) 0.0235(5) Uani 1 1 d . . . . .
H34 H 0.4567 0.6726 0.3187 0.028 Uiso 1 1 calc R . . . .
C35 C 0.3769(2) 0.7009(2) 0.42561(17) 0.0278(5) Uani 1 1 d . . . . .
H35A H 0.2960 0.7059 0.4419 0.033 Uiso 1 1 calc R . . . .
H35B H 0.3997 0.6350 0.4457 0.033 Uiso 1 1 calc R . . . .
C36 C 0.4661(3) 0.8189(3) 0.4646(2) 0.0408(7) Uani 1 1 d . . . . .
H36A H 0.4419 0.8849 0.4466 0.061 Uiso 1 1 calc GR . . . .
H36B H 0.5463 0.8144 0.4486 0.061 Uiso 1 1 calc GR . . . .
H36C H 0.4671 0.8332 0.5236 0.061 Uiso 1 1 calc GR . . . .
C37 C 0.0328(10) 0.4342(10) -0.0729(5) 0.069(3) Uani 0.5 1 d . . . I -1
H37A H 0.0190 0.3489 -0.0705 0.083 Uiso 0.5 1 calc R . . I -1
H37B H 0.1198 0.4637 -0.0757 0.083 Uiso 0.5 1 calc R . . I -1
C38 C -0.031(4) 0.441(3) -0.1476(9) 0.057(3) Uani 0.5 1 d . U . I -1
H38A H -0.0086 0.3870 -0.1939 0.085 Uiso 0.5 1 calc GR . . I -1
H38B H -0.0100 0.5235 -0.1545 0.085 Uiso 0.5 1 calc GR . . I -1
H38C H -0.1178 0.4172 -0.1442 0.085 Uiso 0.5 1 calc GR . . I -1
C39 C 0.0118(16) 0.6347(12) -0.0041(11) 0.081(5) Uani 0.3 1 d D U . I -2
H39A H -0.0374 0.6299 -0.0544 0.097 Uiso 0.3 1 calc R . . I -2
H39B H -0.0326 0.6676 0.0408 0.097 Uiso 0.3 1 calc R . . I -2
C40 C 0.118(2) 0.733(2) -0.0024(13) 0.117(8) Uani 0.3 1 d . U . I -2
H40A H 0.0924 0.8028 -0.0127 0.175 Uiso 0.3 1 calc GR . . I -2
H40B H 0.1690 0.7059 -0.0443 0.175 Uiso 0.3 1 calc GR . . I -2
H40C H 0.1637 0.7544 0.0508 0.175 Uiso 0.3 1 calc GR . . I -2
C41 C -0.1327(11) 0.4898(18) 0.0046(13) 0.075(7) Uani 0.2 1 d D U . I -3
H41A H -0.1417 0.5446 0.0560 0.090 Uiso 0.2 1 calc R . . I -3
H41B H -0.1603 0.5230 -0.0395 0.090 Uiso 0.2 1 calc R . . I -3
C42 C -0.220(2) 0.373(3) 0.000(2) 0.105(10) Uani 0.2 1 d D U . I -3
H42A H -0.1769 0.3087 -0.0062 0.157 Uiso 0.2 1 calc GR . . I -3
H42B H -0.2797 0.3571 -0.0457 0.157 Uiso 0.2 1 calc GR . . I -3
H42C H -0.2596 0.3781 0.0505 0.157 Uiso 0.2 1 calc GR . . I -3
C43 C 0.0641(10) 0.4970(10) 0.0752(6) 0.075(3) Uani 0.5 1 d . U . I -1
H43A H 0.1510 0.5165 0.0688 0.090 Uiso 0.5 1 calc R . . I -1
H43B H 0.0429 0.4136 0.0821 0.090 Uiso 0.5 1 calc R . . I -1
C44 C 0.043(4) 0.577(3) 0.1499(9) 0.057(3) Uani 0.5 1 d . U . I -1
H44A H 0.0702 0.6603 0.1463 0.085 Uiso 0.5 1 calc GR . . I -1
H44B H 0.0880 0.5634 0.1960 0.085 Uiso 0.5 1 calc GR . . I -1
H44C H -0.0426 0.5595 0.1572 0.085 Uiso 0.5 1 calc GR . . I -1
N1 N 0.0000 0.5000 0.0000 0.0675(15) Uani 1 2 d DS T P . .
H41C H -0.0776 0.4940 0.0025 0.101 Uiso 0.3 1 d R . . I -3
H39C H 0.0067 0.5756 -0.0021 0.101 Uiso 0.2 1 d R . . I -2
O18A Cl -0.3574(10) 1.0477(9) 0.3343(6) 0.095(3) Uani 0.15 1 d . U . J 1
O17A Cl 0.413(2) 0.233(2) 0.2795(12) 0.068(5) Uani 0.1 1 d . U . K 1
O17B Cl 0.4056(8) 0.2705(8) 0.3338(6) 0.0688(18) Uani 0.15 1 d . U . L 2
O18B Cl -0.3065(8) 0.9776(8) 0.3031(8) 0.045(2) Uani 0.1 1 d . U . M 2
O18 O 0.2971(13) 0.5260(10) 0.0125(5) 0.075(3) Uani 0.3 1 d . U . N 2
H18D H 0.2283 0.5440 0.0058 0.112 Uiso 0.3 1 d R . . N 2
H18E H 0.3500 0.5900 0.0377 0.112 Uiso 0.3 1 d R . . N 2
O18C O -0.3285(5) 0.9682(5) 0.2539(5) 0.0877(17) Uani 0.75 1 d . U . O 3
O17C O 0.4060(6) 0.2126(6) 0.2433(6) 0.086(3) Uani 0.75 1 d . . . P 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 H1 0.8400 . ?
O1 C1 1.372(3) . ?
O2 H2 0.8400 . ?
O2 C2 1.366(3) . ?
O3 H3 0.8387 . ?
O3 C6 1.367(3) . ?
O4 H4 0.8386 . ?
O4 C12 1.368(3) . ?
O5 H5 0.8368 . ?
O5 C11 1.379(3) . ?
O6 H6 0.8400 . ?
O6 C13 1.378(3) . ?
O7 H7 0.8400 . ?
O7 C21 1.376(3) . ?
O8 H8 0.8400 . ?
O8 C20 1.368(3) . ?
O9 H9 0.8387 . ?
O9 C22 1.373(3) . ?
O10 H10 0.8389 . ?
O10 C30 1.364(3) . ?
O11 H11 0.8400 . ?
O11 C29 1.386(3) . ?
O12 H12 0.8400 . ?
O12 C31 1.380(3) . ?
O13A H13A 0.8944 . ?
O13A H13B 0.8697 . ?
O14A H14A 0.8401(10) . ?
O14A H14B 0.8401(11) . ?
O13B H13C 0.8215 . ?
O13B H13D 0.8202 . ?
O14B H14C 0.8672 . ?
O14B H14D 0.8696 . ?
O15 H15A 0.8499 . ?
O15 H15B 0.8511 . ?
O16A H16A 0.8586 . ?
O16A H16B 0.9164 . ?
O16B H16C 0.8408 . ?
O16B H16D 0.8398 . ?
C1 C2 1.393(3) . ?
C1 C6 1.392(4) . ?
C2 C3 1.395(3) . ?
C3 C4 1.395(3) . ?
C3 C7 1.527(3) . ?
C4 H4A 0.9500 . ?
C4 C5 1.398(3) . ?
C5 C6 1.398(3) . ?
C5 C34 1.524(3) . ?
C7 H7A 1.0000 . ?
C7 C8 1.536(4) . ?
C7 C10 1.524(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.522(4) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.393(4) . ?
C10 C15 1.394(3) . ?
C11 C12 1.397(4) . ?
C12 C13 1.393(4) . ?
C13 C14 1.393(4) . ?
C14 C15 1.399(4) . ?
C14 C16 1.527(3) . ?
C15 H15 0.9500 . ?
C16 H16 1.0000 . ?
C16 C17 1.534(4) . ?
C16 C19 1.522(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.524(4) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.398(3) . ?
C19 C24 1.393(3) . ?
C20 C21 1.385(4) . ?
C21 C22 1.392(4) . ?
C22 C23 1.396(3) . ?
C23 C24 1.397(3) . ?
C23 C25 1.526(3) . ?
C24 H24 0.9500 . ?
C25 H25 1.0000 . ?
C25 C26 1.535(3) . ?
C25 C28 1.526(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.525(4) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.389(4) . ?
C28 C33 1.395(3) . ?
C29 C30 1.392(4) . ?
C30 C31 1.396(4) . ?
C31 C32 1.390(4) . ?
C32 C33 1.395(3) . ?
C32 C34 1.530(3) . ?
C33 H33 0.9500 . ?
C34 H34 1.0000 . ?
C34 C35 1.538(4) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.528(4) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.468(19) . ?
C37 N1 1.422(7) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.479(17) . ?
C39 N1 1.575(13) . ?
C39 H39C 0.6921 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.492(14) . ?
C41 N1 1.508(12) . ?
C41 H41C 0.6263 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.466(19) . ?
C43 N1 1.461(9) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
N1 H41C 0.8818 . ?
N1 H39C 0.8830 . ?
O18 H18D 0.8701 . ?
O18 H18E 0.8700 . ?

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
C1 O1 H1 109.5 . . ?
C2 O2 H2 109.5 . . ?
C6 O3 H3 109.0 . . ?
C12 O4 H4 108.7 . . ?
C11 O5 H5 109.7 . . ?
C13 O6 H6 109.5 . . ?
C21 O7 H7 109.5 . . ?
C20 O8 H8 109.5 . . ?
C22 O9 H9 109.6 . . ?
C30 O10 H10 109.1 . . ?
C29 O11 H11 109.5 . . ?
C31 O12 H12 109.5 . . ?
H13A O13A H13B 104.7 . . ?
H14A O14A H14B 112.7(13) . . ?
H13C O13B H13D 107.1 . . ?
H14C O14B H14D 109.5 . . ?
H15A O15 H15B 127.6 . . ?
H16A O16A H16B 111.6 . . ?
H16C O16B H16D 112.3 . . ?
O1 C1 C2 118.4(2) . . ?
O1 C1 C6 121.0(2) . . ?
C6 C1 C2 120.6(2) . . ?
O2 C2 C1 119.5(2) . . ?
O2 C2 C3 120.3(2) . . ?
C1 C2 C3 120.2(2) . . ?
C2 C3 C7 119.1(2) . . ?
C4 C3 C2 118.2(2) . . ?
C4 C3 C7 122.6(2) . . ?
C3 C4 H4A 118.6 . . ?
C3 C4 C5 122.8(2) . . ?
C5 C4 H4A 118.6 . . ?
C4 C5 C34 122.4(2) . . ?
C6 C5 C4 117.7(2) . . ?
C6 C5 C34 119.9(2) . . ?
O3 C6 C1 115.5(2) . . ?
O3 C6 C5 124.0(2) . . ?
C1 C6 C5 120.5(2) . . ?
C3 C7 H7A 106.9 . . ?
C3 C7 C8 112.7(2) . . ?
C8 C7 H7A 106.9 . . ?
C10 C7 C3 110.6(2) . . ?
C10 C7 H7A 106.9 . . ?
C10 C7 C8 112.4(2) . . ?
C7 C8 H8A 109.1 . . ?
C7 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
C9 C8 C7 112.6(2) . . ?
C9 C8 H8A 109.1 . . ?
C9 C8 H8B 109.1 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 C7 121.1(2) . . ?
C11 C10 C15 117.7(2) . . ?
C15 C10 C7 121.2(2) . . ?
O5 C11 C10 122.9(2) . . ?
O5 C11 C12 116.5(2) . . ?
C10 C11 C12 120.6(2) . . ?
O4 C12 C11 119.3(2) . . ?
O4 C12 C13 120.4(2) . . ?
C13 C12 C11 120.3(2) . . ?
O6 C13 C12 115.8(2) . . ?
O6 C13 C14 123.7(2) . . ?
C14 C13 C12 120.5(2) . . ?
C13 C14 C15 117.8(2) . . ?
C13 C14 C16 121.5(2) . . ?
C15 C14 C16 120.7(2) . . ?
C10 C15 C14 123.0(2) . . ?
C10 C15 H15 118.5 . . ?
C14 C15 H15 118.5 . . ?
C14 C16 H16 106.7 . . ?
C14 C16 C17 112.1(2) . . ?
C17 C16 H16 106.7 . . ?
C19 C16 C14 111.24(19) . . ?
C19 C16 H16 106.7 . . ?
C19 C16 C17 112.8(2) . . ?
C16 C17 H17A 109.0 . . ?
C16 C17 H17B 109.0 . . ?
H17A C17 H17B 107.8 . . ?
C18 C17 C16 113.0(2) . . ?
C18 C17 H17A 109.0 . . ?
C18 C17 H17B 109.0 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C16 119.1(2) . . ?
C24 C19 C16 123.4(2) . . ?
C24 C19 C20 117.5(2) . . ?
O8 C20 C19 119.4(2) . . ?
O8 C20 C21 120.0(2) . . ?
C21 C20 C19 120.7(2) . . ?
O7 C21 C20 118.9(2) . . ?
O7 C21 C22 120.3(2) . . ?
C20 C21 C22 120.7(2) . . ?
O9 C22 C21 115.8(2) . . ?
O9 C22 C23 124.0(2) . . ?
C21 C22 C23 120.1(2) . . ?
C22 C23 C24 117.9(2) . . ?
C22 C23 C25 119.6(2) . . ?
C24 C23 C25 122.4(2) . . ?
C19 C24 C23 123.0(2) . . ?
C19 C24 H24 118.5 . . ?
C23 C24 H24 118.5 . . ?
C23 C25 H25 106.9 . . ?
C23 C25 C26 113.0(2) . . ?
C23 C25 C28 110.15(19) . . ?
C26 C25 H25 106.9 . . ?
C28 C25 H25 106.9 . . ?
C28 C25 C26 112.6(2) . . ?
C25 C26 H26A 109.1 . . ?
C25 C26 H26B 109.1 . . ?
H26A C26 H26B 107.9 . . ?
C27 C26 C25 112.3(2) . . ?
C27 C26 H26A 109.1 . . ?
C27 C26 H26B 109.1 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C25 120.7(2) . . ?
C29 C28 C33 117.8(2) . . ?
C33 C28 C25 121.5(2) . . ?
O11 C29 C28 120.3(2) . . ?
O11 C29 C30 118.4(2) . . ?
C28 C29 C30 121.3(2) . . ?
O10 C30 C29 120.9(2) . . ?
O10 C30 C31 119.6(2) . . ?
C29 C30 C31 119.5(2) . . ?
O12 C31 C30 118.7(2) . . ?
O12 C31 C32 120.6(2) . . ?
C32 C31 C30 120.6(2) . . ?
C31 C32 C33 118.3(2) . . ?
C31 C32 C34 120.5(2) . . ?
C33 C32 C34 121.1(2) . . ?
C28 C33 C32 122.3(2) . . ?
C28 C33 H33 118.9 . . ?
C32 C33 H33 118.9 . . ?
C5 C34 C32 109.9(2) . . ?
C5 C34 H34 106.9 . . ?
C5 C34 C35 113.6(2) . . ?
C32 C34 H34 106.9 . . ?
C32 C34 C35 112.1(2) . . ?
C35 C34 H34 106.9 . . ?
C34 C35 H35A 109.2 . . ?
C34 C35 H35B 109.2 . . ?
H35A C35 H35B 107.9 . . ?
C36 C35 C34 112.1(2) . . ?
C36 C35 H35A 109.2 . . ?
C36 C35 H35B 109.2 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
H37A C37 H37B 107.5 . . ?
C38 C37 H37A 108.4 . . ?
C38 C37 H37B 108.4 . . ?
N1 C37 H37A 108.4 . . ?
N1 C37 H37B 108.4 . . ?
N1 C37 C38 115.4(12) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
H39A C39 H39B 105.6 . . ?
H39A C39 H39C 104.6 . . ?
H39B C39 H39C 104.2 . . ?
C40 C39 H39A 104.4 . . ?
C40 C39 H39B 104.4 . . ?
C40 C39 N1 131.4(18) . . ?
C40 C39 H39C 131.4 . . ?
N1 C39 H39A 104.4 . . ?
N1 C39 H39B 104.4 . . ?
N1 C39 H39C 0.3 . . ?
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 . . ?
H41A C41 H41B 106.6 . . ?
H41A C41 H41C 106.8 . . ?
H41B C41 H41C 106.3 . . ?
C42 C41 H41A 106.6 . . ?
C42 C41 H41B 106.6 . . ?
C42 C41 N1 122.9(16) . . ?
C42 C41 H41C 122.9 . . ?
N1 C41 H41A 106.6 . . ?
N1 C41 H41B 106.6 . . ?
N1 C41 H41C 0.3 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
H43A C43 H43B 107.2 . . ?
C44 C43 H43A 108.0 . . ?
C44 C43 H43B 108.0 . . ?
N1 C43 H43A 108.0 . . ?
N1 C43 H43B 108.0 . . ?
N1 C43 C44 117.4(13) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C37 N1 C43 116.6(5) . . ?
C39 N1 H39C 0.2 . . ?
C41 N1 H41C 0.2 . . ?
H18D O18 H18E 109.5 . . ?

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 C1 C2 O2 -0.9(4) . . . . ?
O1 C1 C2 C3 178.6(2) . . . . ?
O1 C1 C6 O3 -0.3(4) . . . . ?
O1 C1 C6 C5 -179.0(2) . . . . ?
O2 C2 C3 C4 -179.5(2) . . . . ?
O2 C2 C3 C7 -1.0(3) . . . . ?
O4 C12 C13 O6 3.8(4) . . . . ?
O4 C12 C13 C14 -178.0(3) . . . . ?
O5 C11 C12 O4 -2.5(4) . . . . ?
O5 C11 C12 C13 176.9(3) . . . . ?
O6 C13 C14 C15 177.8(2) . . . . ?
O6 C13 C14 C16 -1.5(4) . . . . ?
O7 C21 C22 O9 1.5(4) . . . . ?
O7 C21 C22 C23 -179.8(2) . . . . ?
O8 C20 C21 O7 1.4(4) . . . . ?
O8 C20 C21 C22 -177.6(2) . . . . ?
O9 C22 C23 C24 178.0(2) . . . . ?
O9 C22 C23 C25 -3.3(4) . . . . ?
O10 C30 C31 O12 0.0(4) . . . . ?
O10 C30 C31 C32 -177.2(3) . . . . ?
O11 C29 C30 O10 0.1(4) . . . . ?
O11 C29 C30 C31 -179.9(2) . . . . ?
O12 C31 C32 C33 -177.3(2) . . . . ?
O12 C31 C32 C34 2.0(4) . . . . ?
C1 C2 C3 C4 0.9(4) . . . . ?
C1 C2 C3 C7 179.5(2) . . . . ?
C2 C1 C6 O3 179.9(2) . . . . ?
C2 C1 C6 C5 1.2(4) . . . . ?
C2 C3 C4 C5 0.0(4) . . . . ?
C2 C3 C7 C8 154.5(2) . . . . ?
C2 C3 C7 C10 -78.7(3) . . . . ?
C3 C4 C5 C6 -0.3(4) . . . . ?
C3 C4 C5 C34 177.6(2) . . . . ?
C3 C7 C8 C9 -171.8(2) . . . . ?
C3 C7 C10 C11 103.6(3) . . . . ?
C3 C7 C10 C15 -76.3(3) . . . . ?
C4 C3 C7 C8 -27.0(3) . . . . ?
C4 C3 C7 C10 99.8(3) . . . . ?
C4 C5 C6 O3 -178.8(2) . . . . ?
C4 C5 C6 C1 -0.2(4) . . . . ?
C4 C5 C34 C32 -97.7(3) . . . . ?
C4 C5 C34 C35 28.9(3) . . . . ?
C5 C34 C35 C36 172.9(2) . . . . ?
C6 C1 C2 O2 178.9(2) . . . . ?
C6 C1 C2 C3 -1.5(4) . . . . ?
C6 C5 C34 C32 80.2(3) . . . . ?
C6 C5 C34 C35 -153.2(2) . . . . ?
C7 C3 C4 C5 -178.5(2) . . . . ?
C7 C10 C11 O5 0.4(4) . . . . ?
C7 C10 C11 C12 179.4(2) . . . . ?
C7 C10 C15 C14 -176.9(2) . . . . ?
C8 C7 C10 C11 -129.4(2) . . . . ?
C8 C7 C10 C15 50.6(3) . . . . ?
C10 C7 C8 C9 62.4(3) . . . . ?
C10 C11 C12 O4 178.5(3) . . . . ?
C10 C11 C12 C13 -2.1(4) . . . . ?
C11 C10 C15 C14 3.1(4) . . . . ?
C11 C12 C13 O6 -175.6(3) . . . . ?
C11 C12 C13 C14 2.6(4) . . . . ?
C12 C13 C14 C15 -0.3(4) . . . . ?
C12 C13 C14 C16 -179.6(2) . . . . ?
C13 C14 C15 C10 -2.6(4) . . . . ?
C13 C14 C16 C17 127.1(3) . . . . ?
C13 C14 C16 C19 -105.5(3) . . . . ?
C14 C16 C17 C18 -60.8(3) . . . . ?
C14 C16 C19 C20 81.4(3) . . . . ?
C14 C16 C19 C24 -97.6(3) . . . . ?
C15 C10 C11 O5 -179.6(2) . . . . ?
C15 C10 C11 C12 -0.6(4) . . . . ?
C15 C14 C16 C17 -52.2(3) . . . . ?
C15 C14 C16 C19 75.2(3) . . . . ?
C16 C14 C15 C10 176.7(2) . . . . ?
C16 C19 C20 O8 -1.5(3) . . . . ?
C16 C19 C20 C21 178.7(2) . . . . ?
C16 C19 C24 C23 179.9(2) . . . . ?
C17 C16 C19 C20 -151.5(2) . . . . ?
C17 C16 C19 C24 29.4(3) . . . . ?
C19 C16 C17 C18 172.7(2) . . . . ?
C19 C20 C21 O7 -178.7(2) . . . . ?
C19 C20 C21 C22 2.3(4) . . . . ?
C20 C19 C24 C23 0.8(4) . . . . ?
C20 C21 C22 O9 -179.5(2) . . . . ?
C20 C21 C22 C23 -0.8(4) . . . . ?
C21 C22 C23 C24 -0.6(3) . . . . ?
C21 C22 C23 C25 178.0(2) . . . . ?
C22 C23 C24 C19 0.6(4) . . . . ?
C22 C23 C25 C26 151.0(2) . . . . ?
C22 C23 C25 C28 -82.1(3) . . . . ?
C23 C25 C26 C27 -172.3(2) . . . . ?
C23 C25 C28 C29 99.6(3) . . . . ?
C23 C25 C28 C33 -79.3(3) . . . . ?
C24 C19 C20 O8 177.7(2) . . . . ?
C24 C19 C20 C21 -2.2(3) . . . . ?
C24 C23 C25 C26 -30.4(3) . . . . ?
C24 C23 C25 C28 96.5(3) . . . . ?
C25 C23 C24 C19 -178.0(2) . . . . ?
C25 C28 C29 O11 -1.8(4) . . . . ?
C25 C28 C29 C30 -179.0(2) . . . . ?
C25 C28 C33 C32 -178.3(2) . . . . ?
C26 C25 C28 C29 -133.2(2) . . . . ?
C26 C25 C28 C33 47.9(3) . . . . ?
C28 C25 C26 C27 62.1(3) . . . . ?
C28 C29 C30 O10 177.3(3) . . . . ?
C28 C29 C30 C31 -2.7(4) . . . . ?
C29 C28 C33 C32 2.8(4) . . . . ?
C29 C30 C31 O12 -180.0(2) . . . . ?
C29 C30 C31 C32 2.8(4) . . . . ?
C30 C31 C32 C33 -0.2(4) . . . . ?
C30 C31 C32 C34 179.2(2) . . . . ?
C31 C32 C33 C28 -2.7(4) . . . . ?
C31 C32 C34 C5 -100.5(3) . . . . ?
C31 C32 C34 C35 132.1(2) . . . . ?
C32 C34 C35 C36 -61.7(3) . . . . ?
C33 C28 C29 O11 177.1(2) . . . . ?
C33 C28 C29 C30 -0.1(4) . . . . ?
C33 C32 C34 C5 78.8(3) . . . . ?
C33 C32 C34 C35 -48.6(3) . . . . ?
C34 C5 C6 O3 3.2(4) . . . . ?
C34 C5 C6 C1 -178.2(2) . . . . ?
C34 C32 C33 C28 177.9(2) . . . . ?
C38 C37 N1 C39 -54(2) . . . . ?
C38 C37 N1 C41 43(2) . . . . ?
C38 C37 N1 C43 -179(2) . . . . ?
C40 C39 N1 C37 -70(2) . . . . ?
C40 C39 N1 C41 173(2) . . . . ?
C40 C39 N1 C43 59(2) . . . . ?
C42 C41 N1 C37 61(3) . . . . ?
C42 C41 N1 C39 172(3) . . . . ?
C42 C41 N1 C43 -78(2) . . . . ?
C44 C43 N1 C37 172(2) . . . . ?
C44 C43 N1 C39 47(2) . . . . ?
C44 C43 N1 C41 -49(2) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_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
0 -7 0 0.0446 0.0038 -6.9998 -0.0011 0.1024 0.7711 -0.5755
0 7 0 0.0541 -0.0038 6.9998 0.0011 -0.1024 -0.7711 0.5755
-2 1 -10 0.0858 -2.0044 1.0027 -10.0003 0.0393 0.6839 0.6819
2 0 10 0.0758 2.0039 -0.0027 10.0005 -0.0539 -0.7940 -0.5996
-7 2 2 0.0445 -7.0001 2.0003 2.0025 -0.9431 0.0928 0.1185
7 -2 -2 0.0281 7.0001 -2.0003 -2.0025 0.9431 -0.0928 -0.1185
1 -6 9 0.0869 1.0068 -6.0022 8.9997 -0.0583 -0.0026 -1.0250
5 4 0 0.0487 4.9977 3.9993 -0.0008 0.5516 -0.7595 0.2789
2 -1 -10 0.0773 1.9965 -0.9977 -10.0018 0.5566 0.6491 0.4774

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items have may been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4a@2
_database_code_depnum_ccdc_archive 'CCDC 1021707'
_audit_update_record             
;
2014-11-07 deposited with the CCDC.
2014-12-03 downloaded from the CCDC.
;

_vrf_CHEMW03_4a@2                
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: Some disordered solvent molecules were removed by using 
          "SQUEEZE". The reported value is for the compound including
          the removed solvent molecules. 
;
_audit_creation_date             2014-05-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C40 H48 O8, C2 H8 N, Cl, O H2, 2(C H4 O)'
_chemical_formula_sum            'C44 H66 Cl N O11'
_chemical_formula_weight         820.42
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C53 H39 N9 O7 Ru1'
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'
Cl Cl 0.1484 0.1585 '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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   22.4355(13)
_cell_length_b                   12.3522(6)
_cell_length_c                   15.3459(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4252.8(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4354
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.3530
_cell_measurement_theta_min      2.1120
_shelx_estimated_absorpt_T_max   0.991
_shelx_estimated_absorpt_T_min   0.984
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1348
_diffrn_reflns_av_unetI/netI     0.1119
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            52560
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_min         1.815
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0107
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0150695000
_diffrn_orient_matrix_UB_12      -0.0502546000
_diffrn_orient_matrix_UB_13      0.0042090000
_diffrn_orient_matrix_UB_21      -0.0254587000
_diffrn_orient_matrix_UB_22      -0.0224830000
_diffrn_orient_matrix_UB_23      0.0205454000
_diffrn_orient_matrix_UB_31      -0.0111485000
_diffrn_orient_matrix_UB_32      -0.0163358000
_diffrn_orient_matrix_UB_33      -0.0411853000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.923
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5414
_reflns_number_total             7694
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 
;
 Flack x determined using 1712 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.05(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         7694
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1130
_refine_ls_R_factor_gt           0.0793
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0642P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1652
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(H42D)=Sof(H42E)=Sof(H42F)=Sof(N1B)=
 Sof(H1BA)=Sof(H1BB)=1-FVAR(1)
 Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(N1A)=Sof(H1AA)=Sof(H1AB)=Sof(H42A)=
 Sof(H42B)=Sof(H42C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C38(H38), C28(H28), C8(H8A), C18(H18)
4.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C39(H39A,H39B), C19(H19A,H19B), C29(H29A,H29B), N1A(H1AA,H1AB),
 N1B(H1BA,H1BB)
4.c Me refined with riding coordinates:
 C41(H41A,H41B,H41C), C41(H41D,H41E,H41F), C42(H42A,H42B,H42C), C42(H42D,H42E,
 H42F)
4.d Aromatic/amide H refined with riding coordinates:
 C36(H36), C6(H6A), C16(H16), C26(H26)
4.e Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C7(H7A,H7B,H7C), C30(H30A,H30B,H30C), C20(H20A,H20B,
 H20C), C37(H37A,H37B,H37C), C40(H40A,H40B,H40C), C27(H27A,H27B,H27C), C17(H17A,
 H17B,H17C)
4.f Idealised tetrahedral OH refined as rotating group:
 O2(H2), O8(H8), O3(H3), O1(H1), O6(H6), O7(H7), O4(H4), O5(H5)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.46706(8) 1.11501(15) 0.64294(12) 0.0351(4) Uani 1 1 d . . . . .
O2 O 0.5823(2) 1.2621(3) 0.6351(3) 0.0272(11) Uani 1 1 d . . . . .
H2 H 0.5466 1.2418 0.6337 0.041 Uiso 1 1 calc GR . . . .
O8 O 0.6168(2) 0.9088(4) 0.9803(3) 0.0330(13) Uani 1 1 d . . . . .
H8 H 0.5962 0.8772 1.0182 0.049 Uiso 1 1 calc GR . . . .
O3 O 0.5841(2) 1.2000(4) 0.4559(3) 0.0359(13) Uani 1 1 d . . . . .
H3 H 0.5843 1.2225 0.5075 0.054 Uiso 1 1 calc GR . . . .
O1 O 0.6047(2) 1.1139(4) 0.9197(3) 0.0309(12) Uani 1 1 d . . . . .
H1 H 0.6189 1.0592 0.9446 0.046 Uiso 1 1 calc GR . . . .
O6 O 0.6112(2) 0.4784(4) 0.6816(3) 0.0369(13) Uani 1 1 d . . . . .
H6 H 0.5917 0.4291 0.6569 0.055 Uiso 1 1 calc GR . . . .
O7 O 0.6070(2) 0.5598(4) 0.8467(3) 0.0358(13) Uani 1 1 d . . . . .
H7 H 0.6166 0.5286 0.8001 0.054 Uiso 1 1 calc GR . . . .
O4 O 0.5996(2) 0.8511(4) 0.3230(3) 0.0352(13) Uani 1 1 d . . . . .
H4 H 0.5888 0.8824 0.2770 0.053 Uiso 1 1 calc GR . . . .
O5 O 0.5865(2) 0.6517(4) 0.4062(3) 0.0385(13) Uani 1 1 d . . . . .
H5 H 0.5948 0.7104 0.3813 0.058 Uiso 1 1 calc GR . . . .
C36 C 0.7024(3) 0.7943(5) 0.8029(4) 0.0203(15) Uani 1 1 d . . . . .
H36 H 0.7334 0.8159 0.7645 0.024 Uiso 1 1 calc R . . . .
C34 C 0.6371(3) 0.8327(5) 0.9190(4) 0.0224(16) Uani 1 1 d . . . . .
C15 C 0.6643(3) 0.8973(5) 0.4385(4) 0.0223(16) Uani 1 1 d . . . . .
C6 C 0.6939(3) 1.0742(5) 0.7215(4) 0.0218(16) Uani 1 1 d . . . . .
H6A H 0.7283 1.0367 0.7018 0.026 Uiso 1 1 calc R . . . .
C3 C 0.5955(3) 1.1896(5) 0.7794(4) 0.0254(17) Uani 1 1 d . . . . .
C24 C 0.6282(3) 0.5554(5) 0.6204(4) 0.0239(16) Uani 1 1 d . . . . .
C21 C 0.6688(3) 0.7067(5) 0.4990(4) 0.0203(16) Uani 1 1 d . . . . .
C38 C 0.7085(3) 0.9829(5) 0.8682(4) 0.0234(16) Uani 1 1 d . . . . .
H38 H 0.7009 1.0097 0.9287 0.028 Uiso 1 1 calc R . . . .
C28 C 0.7083(3) 0.6086(5) 0.7303(4) 0.0207(15) Uani 1 1 d . . . . .
H28 H 0.6997 0.5341 0.7523 0.025 Uiso 1 1 calc R . . . .
C1 C 0.6751(3) 1.0584(5) 0.8064(4) 0.0207(15) Uani 1 1 d . . . . .
C33 C 0.6118(3) 0.7302(5) 0.9133(4) 0.0246(16) Uani 1 1 d . . . . .
C2 C 0.6254(3) 1.1185(5) 0.8356(4) 0.0236(16) Uani 1 1 d . . . . .
C16 C 0.6838(3) 0.9704(5) 0.4999(4) 0.0195(15) Uani 1 1 d . . . . .
H16 H 0.7146 0.9497 0.5390 0.023 Uiso 1 1 calc R . . . .
C22 C 0.6185(3) 0.6443(6) 0.4842(5) 0.0297(17) Uani 1 1 d . . . . .
C9 C 0.7556(3) 1.1600(5) 0.5628(4) 0.0282(17) Uani 1 1 d . . . . .
H9A H 0.7718 1.0900 0.5834 0.034 Uiso 1 1 calc R . . . .
H9B H 0.7668 1.1686 0.5008 0.034 Uiso 1 1 calc R . . . .
C32 C 0.6336(3) 0.6601(5) 0.8502(4) 0.0232(16) Uani 1 1 d . . . . .
C39 C 0.7750(3) 0.9832(5) 0.8554(4) 0.0252(16) Uani 1 1 d . . . . .
H39A H 0.7897 1.0585 0.8606 0.030 Uiso 1 1 calc R . . . .
H39B H 0.7841 0.9577 0.7957 0.030 Uiso 1 1 calc R . . . .
C11 C 0.6593(3) 1.0757(5) 0.5067(4) 0.0228(16) Uani 1 1 d . . . . .
C12 C 0.6117(3) 1.1005(5) 0.4519(4) 0.0222(16) Uani 1 1 d . . . . .
C25 C 0.6781(3) 0.6193(5) 0.6421(5) 0.0241(15) Uani 1 1 d . . . . .
C19 C 0.7616(3) 0.7918(5) 0.4334(4) 0.0237(16) Uani 1 1 d . . . . .
H19A H 0.7743 0.8240 0.4895 0.028 Uiso 1 1 calc R . . . .
H19B H 0.7778 0.7174 0.4307 0.028 Uiso 1 1 calc R . . . .
C4 C 0.6147(3) 1.1966(5) 0.6947(4) 0.0242(16) Uani 1 1 d . . . . .
C8 C 0.6871(3) 1.1580(5) 0.5703(4) 0.0215(16) Uani 1 1 d . . . . .
H8A H 0.6728 1.2310 0.5514 0.026 Uiso 1 1 calc R . . . .
C31 C 0.6804(3) 0.6893(5) 0.7959(4) 0.0227(16) Uani 1 1 d . . . . .
C26 C 0.6968(3) 0.6939(5) 0.5786(4) 0.0247(16) Uani 1 1 d . . . . .
H26 H 0.7304 0.7379 0.5910 0.030 Uiso 1 1 calc R . . . .
C29 C 0.7767(3) 0.6209(5) 0.7265(5) 0.0293(17) Uani 1 1 d . . . . .
H29A H 0.7865 0.6922 0.7007 0.035 Uiso 1 1 calc R . . . .
H29B H 0.7926 0.6199 0.7867 0.035 Uiso 1 1 calc R . . . .
C5 C 0.6646(3) 1.1422(5) 0.6639(4) 0.0211(16) Uani 1 1 d . . . . .
C14 C 0.6183(3) 0.9272(5) 0.3827(4) 0.0236(16) Uani 1 1 d . . . . .
C18 C 0.6941(3) 0.7862(5) 0.4314(4) 0.0211(15) Uani 1 1 d . . . . .
H18 H 0.6831 0.7568 0.3729 0.025 Uiso 1 1 calc R . . . .
C13 C 0.5901(3) 1.0267(6) 0.3905(4) 0.0281(17) Uani 1 1 d . . . . .
C10 C 0.7832(4) 1.2515(6) 0.6157(5) 0.045(2) Uani 1 1 d . . . . .
H10A H 0.7699 1.3213 0.5924 0.067 Uiso 1 1 calc GR . . . .
H10B H 0.8268 1.2471 0.6119 0.067 Uiso 1 1 calc GR . . . .
H10C H 0.7709 1.2451 0.6767 0.067 Uiso 1 1 calc GR . . . .
C23 C 0.5969(3) 0.5674(5) 0.5429(4) 0.0257(17) Uani 1 1 d . . . . .
C35 C 0.6815(3) 0.8688(5) 0.8626(4) 0.0241(17) Uani 1 1 d . . . . .
C7 C 0.5448(3) 1.2582(6) 0.8140(5) 0.0349(19) Uani 1 1 d . . . . .
H7A H 0.5153 1.2114 0.8423 0.052 Uiso 1 1 calc GR . . . .
H7B H 0.5260 1.2972 0.7657 0.052 Uiso 1 1 calc GR . . . .
H7C H 0.5603 1.3103 0.8565 0.052 Uiso 1 1 calc GR . . . .
C30 C 0.8067(4) 0.5344(6) 0.6748(5) 0.045(2) Uani 1 1 d . . . . .
H30A H 0.7928 0.5373 0.6143 0.068 Uiso 1 1 calc GR . . . .
H30B H 0.7972 0.4634 0.6998 0.068 Uiso 1 1 calc GR . . . .
H30C H 0.8500 0.5455 0.6763 0.068 Uiso 1 1 calc GR . . . .
C20 C 0.7878(4) 0.8570(6) 0.3604(5) 0.038(2) Uani 1 1 d . . . . .
H20A H 0.7783 0.8224 0.3046 0.058 Uiso 1 1 calc GR . . . .
H20B H 0.8312 0.8607 0.3673 0.058 Uiso 1 1 calc GR . . . .
H20C H 0.7712 0.9303 0.3614 0.058 Uiso 1 1 calc GR . . . .
C37 C 0.5632(4) 0.6945(6) 0.9739(5) 0.039(2) Uani 1 1 d . . . . .
H37A H 0.5678 0.7312 1.0301 0.059 Uiso 1 1 calc GR . . . .
H37B H 0.5658 0.6160 0.9825 0.059 Uiso 1 1 calc GR . . . .
H37C H 0.5244 0.7128 0.9486 0.059 Uiso 1 1 calc GR . . . .
C40 C 0.8082(4) 0.9121(6) 0.9209(5) 0.045(2) Uani 1 1 d . . . . .
H40A H 0.8512 0.9173 0.9103 0.067 Uiso 1 1 calc GR . . . .
H40B H 0.7954 0.8367 0.9141 0.067 Uiso 1 1 calc GR . . . .
H40C H 0.7993 0.9366 0.9802 0.067 Uiso 1 1 calc GR . . . .
C27 C 0.5430(3) 0.5024(6) 0.5229(5) 0.041(2) Uani 1 1 d . . . . .
H27A H 0.5549 0.4339 0.4959 0.061 Uiso 1 1 calc GR . . . .
H27B H 0.5173 0.5428 0.4828 0.061 Uiso 1 1 calc GR . . . .
H27C H 0.5212 0.4877 0.5770 0.061 Uiso 1 1 calc GR . . . .
C17 C 0.5372(3) 1.0606(6) 0.3350(5) 0.043(2) Uani 1 1 d . . . . .
H17A H 0.5152 1.1182 0.3648 0.065 Uiso 1 1 calc GR . . . .
H17B H 0.5110 0.9982 0.3259 0.065 Uiso 1 1 calc GR . . . .
H17C H 0.5515 1.0872 0.2786 0.065 Uiso 1 1 calc GR . . . .
C41 C 0.5767(4) 0.8680(7) 0.6770(6) 0.051(2) Uani 1 1 d . . . . .
H41A H 0.6066 0.8146 0.6592 0.076 Uiso 0.54(2) 1 calc R . P A 1
H41B H 0.5456 0.8321 0.7114 0.076 Uiso 0.54(2) 1 calc R . P A 1
H41C H 0.5957 0.9243 0.7122 0.076 Uiso 0.54(2) 1 calc R . P A 1
H41D H 0.6076 0.8649 0.6319 0.076 Uiso 0.46(2) 1 calc R . P A 2
H41E H 0.5787 0.8026 0.7130 0.076 Uiso 0.46(2) 1 calc R . P A 2
H41F H 0.5830 0.9319 0.7136 0.076 Uiso 0.46(2) 1 calc R . P A 2
N1A N 0.5490(6) 0.9187(10) 0.5969(8) 0.032(4) Uani 0.54(2) 1 d . U P A 1
H1AA H 0.5262 0.9834 0.6153 0.039 Uiso 0.54(2) 1 calc R . P A 1
H1AB H 0.5815 0.9439 0.5583 0.039 Uiso 0.54(2) 1 calc R . P A 1
C42 C 0.5108(5) 0.8516(8) 0.5478(6) 0.071(3) Uani 1 1 d . . . . .
H42A H 0.5178 0.8637 0.4855 0.106 Uiso 0.54(2) 1 calc R . P A 1
H42B H 0.4693 0.8688 0.5617 0.106 Uiso 0.54(2) 1 calc R . P A 1
H42C H 0.5188 0.7756 0.5620 0.106 Uiso 0.54(2) 1 calc R . P A 1
H42D H 0.5259 0.9127 0.5135 0.106 Uiso 0.46(2) 1 calc R . P A 2
H42E H 0.4690 0.8383 0.5329 0.106 Uiso 0.46(2) 1 calc R . P A 2
H42F H 0.5344 0.7868 0.5347 0.106 Uiso 0.46(2) 1 calc R . P A 2
N1B N 0.5152(8) 0.8749(14) 0.6337(11) 0.048(6) Uani 0.46(2) 1 d . . P A 2
H1BA H 0.4881 0.8255 0.6655 0.058 Uiso 0.46(2) 1 calc R . P A 2
H1BB H 0.5000 0.9493 0.6424 0.058 Uiso 0.46(2) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
O2 C4 1.422(8) . ?
O8 C34 1.406(8) . ?
O3 C12 1.378(8) . ?
O1 C2 1.372(8) . ?
O6 C24 1.390(7) . ?
O7 C32 1.377(8) . ?
O4 C14 1.377(8) . ?
O5 C22 1.398(8) . ?
C36 C31 1.392(9) . ?
C36 C35 1.379(9) . ?
C34 C33 1.390(9) . ?
C34 C35 1.393(9) . ?
C15 C16 1.377(9) . ?
C15 C14 1.392(9) . ?
C15 C18 1.530(9) . ?
C6 C1 1.384(9) . ?
C6 C5 1.386(9) . ?
C3 C2 1.402(9) . ?
C3 C4 1.371(9) . ?
C3 C7 1.515(9) . ?
C24 C25 1.410(9) . ?
C24 C23 1.390(9) . ?
C21 C22 1.385(10) . ?
C21 C26 1.382(9) . ?
C21 C18 1.538(9) . ?
C38 C1 1.526(9) . ?
C38 C39 1.504(9) . ?
C38 C35 1.536(8) . ?
C28 C25 1.519(9) . ?
C28 C31 1.549(9) . ?
C28 C29 1.543(9) . ?
C1 C2 1.413(9) . ?
C33 C32 1.389(9) . ?
C33 C37 1.498(9) . ?
C16 C11 1.415(8) . ?
C22 C23 1.396(10) . ?
C9 C8 1.541(9) . ?
C9 C10 1.523(9) . ?
C32 C31 1.387(9) . ?
C39 C40 1.530(9) . ?
C11 C12 1.392(9) . ?
C11 C8 1.541(9) . ?
C12 C13 1.397(9) . ?
C25 C26 1.405(10) . ?
C19 C18 1.517(9) . ?
C19 C20 1.500(9) . ?
C4 C5 1.388(9) . ?
C8 C5 1.534(9) . ?
C29 C30 1.493(9) . ?
C14 C13 1.387(9) . ?
C13 C17 1.520(9) . ?
C23 C27 1.482(9) . ?
C41 N1A 1.513(14) . ?
C41 N1B 1.533(17) . ?
N1A C42 1.410(14) . ?
C42 N1B 1.353(17) . ?

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
C35 C36 C31 123.5(6) . . ?
C33 C34 O8 121.2(6) . . ?
C33 C34 C35 123.1(6) . . ?
C35 C34 O8 115.7(6) . . ?
C16 C15 C14 118.8(6) . . ?
C16 C15 C18 120.0(6) . . ?
C14 C15 C18 121.2(6) . . ?
C1 C6 C5 122.8(6) . . ?
C2 C3 C7 119.5(6) . . ?
C4 C3 C2 118.2(6) . . ?
C4 C3 C7 122.2(7) . . ?
O6 C24 C25 116.2(6) . . ?
O6 C24 C23 120.8(6) . . ?
C23 C24 C25 122.9(6) . . ?
C22 C21 C18 123.0(6) . . ?
C26 C21 C22 116.9(6) . . ?
C26 C21 C18 120.1(6) . . ?
C1 C38 C35 109.5(5) . . ?
C39 C38 C1 113.8(5) . . ?
C39 C38 C35 112.7(5) . . ?
C25 C28 C31 110.1(5) . . ?
C25 C28 C29 113.7(5) . . ?
C29 C28 C31 111.3(5) . . ?
C6 C1 C38 121.4(6) . . ?
C6 C1 C2 117.7(6) . . ?
C2 C1 C38 120.8(6) . . ?
C34 C33 C37 121.8(6) . . ?
C32 C33 C34 117.8(6) . . ?
C32 C33 C37 120.3(6) . . ?
O1 C2 C3 116.3(6) . . ?
O1 C2 C1 122.9(6) . . ?
C3 C2 C1 120.8(6) . . ?
C15 C16 C11 122.0(6) . . ?
C21 C22 O5 121.5(6) . . ?
C21 C22 C23 123.8(6) . . ?
C23 C22 O5 114.7(6) . . ?
C10 C9 C8 112.3(6) . . ?
O7 C32 C33 115.8(6) . . ?
O7 C32 C31 122.7(6) . . ?
C31 C32 C33 121.6(6) . . ?
C38 C39 C40 113.3(6) . . ?
C16 C11 C8 119.7(6) . . ?
C12 C11 C16 117.1(6) . . ?
C12 C11 C8 123.2(6) . . ?
O3 C12 C11 121.0(6) . . ?
O3 C12 C13 117.1(6) . . ?
C11 C12 C13 121.9(6) . . ?
C24 C25 C28 121.0(6) . . ?
C26 C25 C24 116.1(6) . . ?
C26 C25 C28 122.8(6) . . ?
C20 C19 C18 113.6(6) . . ?
C3 C4 O2 119.0(6) . . ?
C3 C4 C5 123.1(6) . . ?
C5 C4 O2 117.9(6) . . ?
C9 C8 C11 111.5(5) . . ?
C5 C8 C9 113.6(5) . . ?
C5 C8 C11 112.1(5) . . ?
C36 C31 C28 120.4(6) . . ?
C32 C31 C36 117.6(6) . . ?
C32 C31 C28 121.9(6) . . ?
C21 C26 C25 123.5(6) . . ?
C30 C29 C28 113.5(6) . . ?
C6 C5 C4 117.3(6) . . ?
C6 C5 C8 121.2(6) . . ?
C4 C5 C8 121.5(6) . . ?
O4 C14 C15 116.9(6) . . ?
O4 C14 C13 121.6(6) . . ?
C13 C14 C15 121.3(6) . . ?
C15 C18 C21 111.3(5) . . ?
C19 C18 C15 113.2(5) . . ?
C19 C18 C21 112.6(5) . . ?
C12 C13 C17 118.0(6) . . ?
C14 C13 C12 118.6(6) . . ?
C14 C13 C17 123.4(6) . . ?
C24 C23 C22 116.7(6) . . ?
C24 C23 C27 122.1(6) . . ?
C22 C23 C27 121.3(6) . . ?
C36 C35 C34 116.2(6) . . ?
C36 C35 C38 121.0(6) . . ?
C34 C35 C38 122.7(6) . . ?
C42 N1A C41 116.1(10) . . ?
C42 N1B C41 118.4(14) . . ?

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
O2 C4 C5 C6 -176.7(5) . . . . ?
O2 C4 C5 C8 4.3(9) . . . . ?
O8 C34 C33 C32 179.0(6) . . . . ?
O8 C34 C33 C37 -2.1(10) . . . . ?
O8 C34 C35 C36 179.2(5) . . . . ?
O8 C34 C35 C38 2.0(9) . . . . ?
O3 C12 C13 C14 177.8(6) . . . . ?
O3 C12 C13 C17 -1.6(10) . . . . ?
O6 C24 C25 C28 -4.0(9) . . . . ?
O6 C24 C25 C26 177.5(6) . . . . ?
O6 C24 C23 C22 -177.9(6) . . . . ?
O6 C24 C23 C27 2.2(10) . . . . ?
O7 C32 C31 C36 177.5(6) . . . . ?
O7 C32 C31 C28 -3.2(10) . . . . ?
O4 C14 C13 C12 -179.4(6) . . . . ?
O4 C14 C13 C17 0.0(11) . . . . ?
O5 C22 C23 C24 178.5(6) . . . . ?
O5 C22 C23 C27 -1.7(10) . . . . ?
C34 C33 C32 O7 -179.7(6) . . . . ?
C34 C33 C32 C31 1.8(10) . . . . ?
C15 C16 C11 C12 3.9(9) . . . . ?
C15 C16 C11 C8 -173.8(6) . . . . ?
C15 C14 C13 C12 4.5(10) . . . . ?
C15 C14 C13 C17 -176.2(7) . . . . ?
C6 C1 C2 O1 -176.5(6) . . . . ?
C6 C1 C2 C3 1.3(9) . . . . ?
C3 C4 C5 C6 3.1(9) . . . . ?
C3 C4 C5 C8 -175.9(6) . . . . ?
C24 C25 C26 C21 0.4(10) . . . . ?
C21 C22 C23 C24 0.6(10) . . . . ?
C21 C22 C23 C27 -179.6(7) . . . . ?
C38 C1 C2 O1 0.8(10) . . . . ?
C38 C1 C2 C3 178.6(6) . . . . ?
C28 C25 C26 C21 -178.1(6) . . . . ?
C1 C6 C5 C4 0.6(9) . . . . ?
C1 C6 C5 C8 179.6(6) . . . . ?
C1 C38 C39 C40 176.8(6) . . . . ?
C1 C38 C35 C36 89.3(7) . . . . ?
C1 C38 C35 C34 -93.7(7) . . . . ?
C33 C34 C35 C36 -4.0(10) . . . . ?
C33 C34 C35 C38 178.8(6) . . . . ?
C33 C32 C31 C36 -4.0(10) . . . . ?
C33 C32 C31 C28 175.2(6) . . . . ?
C2 C3 C4 O2 175.3(5) . . . . ?
C2 C3 C4 C5 -4.4(10) . . . . ?
C16 C15 C14 O4 -179.2(6) . . . . ?
C16 C15 C14 C13 -2.9(10) . . . . ?
C16 C15 C18 C21 82.4(7) . . . . ?
C16 C15 C18 C19 -45.6(8) . . . . ?
C16 C11 C12 O3 178.1(6) . . . . ?
C16 C11 C12 C13 -2.2(10) . . . . ?
C16 C11 C8 C9 46.2(8) . . . . ?
C16 C11 C8 C5 -82.4(7) . . . . ?
C22 C21 C26 C25 2.4(10) . . . . ?
C22 C21 C18 C15 86.9(8) . . . . ?
C22 C21 C18 C19 -144.8(6) . . . . ?
C9 C8 C5 C6 -37.4(9) . . . . ?
C9 C8 C5 C4 141.5(6) . . . . ?
C39 C38 C1 C6 35.5(8) . . . . ?
C39 C38 C1 C2 -141.7(6) . . . . ?
C39 C38 C35 C36 -38.4(8) . . . . ?
C39 C38 C35 C34 138.6(6) . . . . ?
C11 C12 C13 C14 -1.8(10) . . . . ?
C11 C12 C13 C17 178.8(7) . . . . ?
C11 C8 C5 C6 90.1(7) . . . . ?
C11 C8 C5 C4 -91.0(7) . . . . ?
C12 C11 C8 C9 -131.4(7) . . . . ?
C12 C11 C8 C5 100.1(7) . . . . ?
C25 C24 C23 C22 2.4(10) . . . . ?
C25 C24 C23 C27 -177.4(7) . . . . ?
C25 C28 C31 C36 -88.0(7) . . . . ?
C25 C28 C31 C32 92.8(7) . . . . ?
C25 C28 C29 C30 -63.8(8) . . . . ?
C4 C3 C2 O1 -179.9(6) . . . . ?
C4 C3 C2 C1 2.1(10) . . . . ?
C8 C11 C12 O3 -4.3(10) . . . . ?
C8 C11 C12 C13 175.4(6) . . . . ?
C31 C36 C35 C34 1.5(10) . . . . ?
C31 C36 C35 C38 178.8(6) . . . . ?
C31 C28 C25 C24 -91.1(7) . . . . ?
C31 C28 C25 C26 87.3(7) . . . . ?
C31 C28 C29 C30 171.2(6) . . . . ?
C26 C21 C22 O5 179.4(6) . . . . ?
C26 C21 C22 C23 -2.9(10) . . . . ?
C26 C21 C18 C15 -94.0(7) . . . . ?
C26 C21 C18 C19 34.3(8) . . . . ?
C29 C28 C25 C24 143.3(6) . . . . ?
C29 C28 C25 C26 -38.3(8) . . . . ?
C29 C28 C31 C36 39.0(8) . . . . ?
C29 C28 C31 C32 -140.2(6) . . . . ?
C5 C6 C1 C38 -180.0(6) . . . . ?
C5 C6 C1 C2 -2.7(10) . . . . ?
C14 C15 C16 C11 -1.4(10) . . . . ?
C14 C15 C18 C21 -98.8(7) . . . . ?
C14 C15 C18 C19 133.2(7) . . . . ?
C18 C15 C16 C11 177.4(6) . . . . ?
C18 C15 C14 O4 2.0(10) . . . . ?
C18 C15 C14 C13 178.3(6) . . . . ?
C18 C21 C22 O5 -1.5(10) . . . . ?
C18 C21 C22 C23 176.3(6) . . . . ?
C18 C21 C26 C25 -176.8(6) . . . . ?
C10 C9 C8 C11 172.0(5) . . . . ?
C10 C9 C8 C5 -60.2(8) . . . . ?
C23 C24 C25 C28 175.7(6) . . . . ?
C23 C24 C25 C26 -2.9(10) . . . . ?
C35 C36 C31 C28 -176.9(6) . . . . ?
C35 C36 C31 C32 2.3(10) . . . . ?
C35 C34 C33 C32 2.4(10) . . . . ?
C35 C34 C33 C37 -178.8(7) . . . . ?
C35 C38 C1 C6 -91.6(7) . . . . ?
C35 C38 C1 C2 91.3(7) . . . . ?
C35 C38 C39 C40 -57.8(7) . . . . ?
C7 C3 C2 O1 1.8(9) . . . . ?
C7 C3 C2 C1 -176.2(6) . . . . ?
C7 C3 C4 O2 -6.4(10) . . . . ?
C7 C3 C4 C5 173.8(6) . . . . ?
C20 C19 C18 C15 -60.6(7) . . . . ?
C20 C19 C18 C21 172.2(6) . . . . ?
C37 C33 C32 O7 1.5(10) . . . . ?
C37 C33 C32 C31 -177.0(6) . . . . ?
C41 N1A C42 N1B 48.6(11) . . . . ?
N1A C41 N1B C42 49.8(14) . . . . ?
N1A C42 N1B C41 -49.1(14) . . . . ?
N1B C41 N1A C42 -45.9(12) . . . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.090 0.077 0.178 166 37 '1 H2O and 2 MeOH'
2 0.910 -0.077 0.678 166 37 '1 H2O and 2 MeOH'
3 0.590 0.423 0.178 166 37 '1 H2O and 2 MeOH'
4 0.410 0.577 0.678 166 37 '1 H2O and 2 MeOH'
_platon_squeeze_details          
;
Summary and Remarks : N = NOTE, W = WARNING, E = ERROR
#================================================================================

N: DISORDERED structure - ATOMS with Pop. .LT. 1.0 are not moved or as a group.
#--------------------------------------------------------------------------------
N: Number of moved primary input atoms: ..................................  117
N: Number of modified (= # ) ATOM labels .................................    4
N: Total Potential Solvent Accessible Void Vol ..................   667.4 Ang^3
N: Electron Count / Cell =    147 - To be included in D(calc), F000 & Mol.Wght.

#================================================================================
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items have may been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5c@1
_database_code_depnum_ccdc_archive 'CCDC 1021708'
_audit_update_record             
;
2014-11-07 deposited with the CCDC.
2014-12-03 downloaded from the CCDC.
;

_vrf_PLAT413_5c@1                
;
PROBLEM: Short Inter XH3 .. XHn     H30    ..  H43C    ..       1.85 Ang.  
RESPONSE: The short intermolecular H H distances are caused by disordered 
          guest molecules.
;
_vrf_PLAT417_5c@1                
;
PROBLEM: Short Inter D-H..H-D       H7A    ..  H9BA    ..       1.63 Ang.  
RESPONSE: The short intermolecular H H distances are caused by disordered 
          guest molecules.
;
_vrf_PLAT415_5c@1                
;
PROBLEM: Short Inter D-H..H-X       H7A    ..  H43C    ..       2.05 Ang.  
RESPONSE: The short intermolecular H H distances are caused by disordered 
          guest molecules.
;


_audit_creation_date             2014-05-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'C36 H40 O8, 3(C H4 O) 2(H2 O) C6 H16 N2, 2(Cl)'
_chemical_formula_sum            'C45 H72 Cl2 N2 O13'
_chemical_formula_weight         919.97
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C40 H52 F6 N2 O8 P1 '
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'
Cl Cl 0.3639 0.7018 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.5090(3)
_cell_length_b                   11.5275(2)
_cell_length_c                   18.1749(4)
_cell_angle_alpha                94.3636(17)
_cell_angle_beta                 101.9147(18)
_cell_angle_gamma                97.3470(18)
_cell_volume                     2326.86(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    21152
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      76.0750
_cell_measurement_theta_min      3.8670
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.794
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       brick
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.2083
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.1033
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24223
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.750
_diffrn_reflns_theta_max         66.748
_diffrn_reflns_theta_min         3.888
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0618862000
_diffrn_orient_matrix_UB_12      0.1002129000
_diffrn_orient_matrix_UB_13      -0.0362789000
_diffrn_orient_matrix_UB_21      -0.0261607000
_diffrn_orient_matrix_UB_22      -0.0791198000
_diffrn_orient_matrix_UB_23      -0.0754676000
_diffrn_orient_matrix_UB_31      -0.1209967000
_diffrn_orient_matrix_UB_32      0.0454812000
_diffrn_orient_matrix_UB_33      -0.0239998000
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.6890 18063 25203
2 0.3110 18087 25203

_diffrn_oxdiff_twin_integration_method simultaneous
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                20623
_reflns_number_total             24223
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         24223
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0562
_refine_ls_restrained_S_all      3.079
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0981P)²+0.9142P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1590
_refine_ls_wR_factor_ref         0.1638
_refine_special_details          
;
 Refined as a 2-component twin.
;
_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, All C(H,H,H,H,H,H) groups, All O(H) groups, All O(H,H)
  groups
2. Shared sites
{O9A, O9B}
3. Restrained distances
 H9AA-O4
 2 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Cl3A) \\sim Ueq, Uanis(Cl3D) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O12C) \\sim Ueq, Uanis(O12D) \\sim Ueq, Uanis(Cl3A) \\sim Ueq,
Uanis(Cl3B) \\sim Ueq, Uanis(Cl3C) \\sim Ueq, Uanis(O12E) \\sim Ueq,
Uanis(O12F) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O9A) = Uanis(O9B)
5. Others
 Fixed Sof: Cl3A(0.15) N2A(0.3) H2A(0.3) H40A(0.3) H40B(0.3) H40C(0.3)
 H40D(0.7) H40E(0.7) H40F(0.7) H41A(0.3) H41B(0.3) H41C(0.7) H41D(0.7)
 C42B(0.3) H42A(0.3) H42B(0.3) O9B(0.25) H9BA(0.25) C43A(0.75) H43D(0.75)
 H43E(0.75) H43F(0.75) O9A(0.75) H9AA(0.75) C43B(0.25) H43A(0.25) H43B(0.25)
 H43C(0.25) Cl3B(0.35) Cl3C(0.35) C42A(0.7) H42C(0.7) H42D(0.7) N2B(0.7)
 H2B(0.7) O12A(0.3) H12A(0.3) H12B(0.3) Cl3D(0.15) O12D(0.2) O12B(0.5)
 O12E(0.6) O12C(0.15) O12F(0.1) O12G(0.15)
6.a Free rotating group:
 O12A(H12A,H12B)
6.b Ternary CH refined with riding coordinates:
 C7(H7), C25(H25), C34(H34), C16(H16), N1(H1A), N2A(H2A), N2B(H2B)
6.c Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C17(H17A,H17B), C8(H8A,H8B), C35(H35A,H35B), C37(H37A,H37B),
 C39(H39A,H39B), C41(H41A,H41B), C41(H41C,H41D), C42B(H42A,H42B), C42A(H42C,
 H42D)
6.d Me refined with riding coordinates:
 C40(H40A,H40B,H40C), C40(H40D,H40E,H40F)
6.e Aromatic/amide H refined with riding coordinates:
 C24(H24), C6(H6A), C33(H33), C15(H15), C21(H21), C12(H12), C3(H3A), C30(H30)
6.f Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C9(H9A,H9B,H9C), C27(H27A,H27B,H27C), C36(H36A,H36B,
 H36C), C38(H38A,H38B,H38C), C43A(H43D,H43E,H43F), C44(H44A,H44B,H44C),
 C45(H45A,H45B,H45C), C43B(H43A,H43B,H43C)
6.g Idealised tetrahedral OH refined as rotating group:
 O2(H2), O5(H5), O1(H1), O8(H8), O4(H4), O3(H3), O7(H7A), O11(H11), O9B(H9BA),
 O10(H10), O9A(H9AA)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.14064(8) 0.64274(9) 0.50182(5) 0.0526(2) Uani 1 1 d . . . . .
O6 O -0.15389(17) 0.41338(16) 0.66827(10) 0.0321(4) Uani 1 1 d . . . . .
O2 O -0.2241(2) 1.11750(18) 0.69068(11) 0.0414(5) Uani 1 1 d . . . . .
H2 H -0.2719 1.1241 0.6501 0.062 Uiso 1 1 calc GR . . . .
O5 O 0.16715(18) 0.72732(16) 0.66910(10) 0.0343(4) Uani 1 1 d . . . . .
H5 H 0.1579 0.6970 0.6244 0.051 Uiso 1 1 calc GR . . . .
O1 O -0.5406(2) 0.80621(18) 0.69397(12) 0.0467(6) Uani 1 1 d . . . . .
H1 H -0.5698 0.8323 0.6534 0.070 Uiso 1 1 calc GR . . . .
C24 C 0.0162(2) 0.6366(2) 0.81632(12) 0.0231(5) Uani 1 1 d . . . . .
H24 H 0.0196 0.6599 0.8681 0.028 Uiso 1 1 calc R . . . .
O8 O -0.62700(17) 0.58509(17) 0.74252(13) 0.0400(5) Uani 1 1 d . . . . .
H8 H -0.6242 0.6572 0.7377 0.060 Uiso 1 1 calc GR . . . .
O4 O 0.29721(19) 0.97587(18) 0.73292(14) 0.0451(5) Uani 1 1 d D . . . .
H4 H 0.2921 0.9026 0.7242 0.068 Uiso 1 1 calc GR . . . .
C28 C -0.2787(2) 0.5001(2) 0.79854(14) 0.0252(5) Uani 1 1 d . . . . .
O3 O 0.02460(19) 1.24755(18) 0.76027(15) 0.0505(6) Uani 1 1 d . . . . .
H3 H 0.0838 1.3002 0.7640 0.076 Uiso 1 1 calc GR . . . .
C7 C -0.1047(2) 1.0984(2) 0.84145(13) 0.0272(5) Uani 1 1 d . . . . .
H7 H -0.1137 1.1804 0.8292 0.033 Uiso 1 1 calc R . . . .
C14 C 0.1390(2) 0.9224(2) 0.79789(13) 0.0255(5) Uani 1 1 d . . . . .
C25 C -0.1521(2) 0.4687(2) 0.82009(13) 0.0252(5) Uani 1 1 d . . . . .
H25 H -0.1567 0.3840 0.8013 0.030 Uiso 1 1 calc R . . . .
C34 C -0.4395(2) 0.7608(2) 0.84135(15) 0.0305(6) Uani 1 1 d . . . . .
H34 H -0.5282 0.7618 0.8294 0.037 Uiso 1 1 calc R . . . .
C23 C -0.0671(2) 0.5396(2) 0.78056(13) 0.0238(5) Uani 1 1 d . . . . .
C19 C 0.0946(2) 0.7013(2) 0.78035(13) 0.0246(5) Uani 1 1 d . . . . .
C6 C -0.2768(2) 0.9327(2) 0.83859(13) 0.0279(5) Uani 1 1 d . . . . .
H6A H -0.2400 0.9225 0.8890 0.033 Uiso 1 1 calc R . . . .
C33 C -0.3037(2) 0.6101(2) 0.82140(14) 0.0277(5) Uani 1 1 d . . . . .
H33 H -0.2387 0.6670 0.8481 0.033 Uiso 1 1 calc R . . . .
C13 C 0.1998(2) 1.0024(2) 0.75978(16) 0.0313(6) Uani 1 1 d . . . . .
C15 C 0.0391(2) 0.9557(2) 0.82068(13) 0.0265(5) Uani 1 1 d . . . . .
H15 H -0.0051 0.9013 0.8451 0.032 Uiso 1 1 calc R . . . .
C16 C 0.1839(2) 0.8079(2) 0.81849(13) 0.0248(5) Uani 1 1 d . . . . .
H16 H 0.2582 0.8045 0.7985 0.030 Uiso 1 1 calc R . . . .
C32 C -0.4184(2) 0.6422(2) 0.80759(14) 0.0279(6) Uani 1 1 d . . . . .
C10 C -0.0004(2) 1.0640(2) 0.81004(14) 0.0267(5) Uani 1 1 d . . . . .
C26 C -0.1083(2) 0.4798(2) 0.90671(14) 0.0286(5) Uani 1 1 d . . . . .
H26A H -0.0266 0.4580 0.9193 0.034 Uiso 1 1 calc R . . . .
H26B H -0.1036 0.5626 0.9273 0.034 Uiso 1 1 calc R . . . .
C21 C 0.0058(2) 0.5693(2) 0.66605(12) 0.0281(5) Uani 1 1 d . . . . .
H21 H 0.0017 0.5466 0.6141 0.034 Uiso 1 1 calc R . . . .
C11 C 0.0644(2) 1.1416(2) 0.77292(16) 0.0321(6) Uani 1 1 d . . . . .
C29 C -0.3758(3) 0.4181(2) 0.75855(17) 0.0340(6) Uani 1 1 d . . . . .
C12 C 0.1628(3) 1.1112(2) 0.74775(17) 0.0362(6) Uani 1 1 d . . . . .
H12 H 0.2056 1.1648 0.7221 0.043 Uiso 1 1 calc R . . . .
C17 C 0.2207(2) 0.8092(2) 0.90472(13) 0.0270(5) Uani 1 1 d . . . . .
H17A H 0.1491 0.8140 0.9264 0.032 Uiso 1 1 calc R . . . .
H17B H 0.2502 0.7344 0.9168 0.032 Uiso 1 1 calc R . . . .
C5 C -0.2223(2) 1.0200(2) 0.80303(13) 0.0273(5) Uani 1 1 d . . . . .
C20 C 0.0885(2) 0.6644(2) 0.70422(14) 0.0273(5) Uani 1 1 d . . . . .
C3 C -0.3825(3) 0.9641(2) 0.69242(14) 0.0396(7) Uani 1 1 d . . . . .
H3A H -0.4189 0.9745 0.6419 0.048 Uiso 1 1 calc R . . . .
C22 C -0.0706(2) 0.5076(2) 0.70412(13) 0.0265(5) Uani 1 1 d . . . . .
O7 O -0.3572(2) 0.30688(18) 0.73574(18) 0.0592(7) Uani 1 1 d . . . . .
H7A H -0.4143 0.2576 0.7413 0.089 Uiso 1 1 calc GR . . . .
C18 C 0.3180(3) 0.9116(3) 0.94178(14) 0.0337(6) Uani 1 1 d . . . . .
H18A H 0.3883 0.9090 0.9194 0.051 Uiso 1 1 calc GR . . . .
H18B H 0.3411 0.9054 0.9962 0.051 Uiso 1 1 calc GR . . . .
H18C H 0.2872 0.9861 0.9336 0.051 Uiso 1 1 calc GR . . . .
C2 C -0.4357(3) 0.8780(2) 0.72968(16) 0.0363(6) Uani 1 1 d . . . . .
C8 C -0.0764(2) 1.1016(2) 0.92849(13) 0.0279(5) Uani 1 1 d . . . . .
H8A H -0.1457 1.1239 0.9477 0.033 Uiso 1 1 calc R . . . .
H8B H -0.0647 1.0219 0.9425 0.033 Uiso 1 1 calc R . . . .
C31 C -0.5112(2) 0.5590(2) 0.76451(16) 0.0311(6) Uani 1 1 d . . . . .
C4 C -0.2766(3) 1.0344(2) 0.72886(14) 0.0333(6) Uani 1 1 d . . . . .
C1 C -0.3834(2) 0.8591(2) 0.80375(14) 0.0296(6) Uani 1 1 d . . . . .
C30 C -0.4905(2) 0.4475(2) 0.74078(17) 0.0355(6) Uani 1 1 d . . . . .
H30 H -0.5549 0.3915 0.7124 0.043 Uiso 1 1 calc R . . . .
C35 C -0.3981(2) 0.7735(2) 0.92803(15) 0.0333(6) Uani 1 1 d . . . . .
H35A H -0.3112 0.7684 0.9417 0.040 Uiso 1 1 calc R . . . .
H35B H -0.4102 0.8520 0.9486 0.040 Uiso 1 1 calc R . . . .
C9 C 0.0353(3) 1.1880(3) 0.96596(14) 0.0327(6) Uani 1 1 d . . . . .
H9A H 0.1056 1.1624 0.9506 0.049 Uiso 1 1 calc GR . . . .
H9B H 0.0465 1.1909 1.0210 0.049 Uiso 1 1 calc GR . . . .
H9C H 0.0258 1.2664 0.9504 0.049 Uiso 1 1 calc GR . . . .
C27 C -0.1913(3) 0.4014(3) 0.94370(15) 0.0349(6) Uani 1 1 d . . . . .
H27A H -0.2024 0.3204 0.9200 0.052 Uiso 1 1 calc GR . . . .
H27B H -0.2692 0.4295 0.9372 0.052 Uiso 1 1 calc GR . . . .
H27C H -0.1557 0.4038 0.9978 0.052 Uiso 1 1 calc GR . . . .
C36 C -0.4661(3) 0.6791(3) 0.96424(17) 0.0413(7) Uani 1 1 d . . . . .
H36A H -0.5523 0.6829 0.9503 0.062 Uiso 1 1 calc GR . . . .
H36B H -0.4387 0.6924 1.0194 0.062 Uiso 1 1 calc GR . . . .
H36C H -0.4508 0.6013 0.9463 0.062 Uiso 1 1 calc GR . . . .
O11 O 0.2191(2) 0.40953(19) 0.78295(12) 0.0480(5) Uani 1 1 d . . . . .
H11 H 0.2465 0.4690 0.7645 0.072 Uiso 1 1 calc GR . . . .
Cl3A Cl -0.3700(17) 0.7790(17) 0.4523(8) 0.092(6) Uani 0.15 1 d . U P A 1
N1 N -0.0557(3) 0.9294(2) 0.54919(14) 0.0452(6) Uani 1 1 d . . . . .
H1A H -0.0904 0.8607 0.5105 0.054 Uiso 1 1 calc R . . . .
C38 C -0.0887(3) 0.8993(3) 0.62106(16) 0.0470(8) Uani 1 1 d . . . . .
H38A H -0.0609 0.8251 0.6343 0.070 Uiso 1 1 calc GR . . . .
H38B H -0.1762 0.8908 0.6147 0.070 Uiso 1 1 calc GR . . . .
H38C H -0.0509 0.9621 0.6615 0.070 Uiso 1 1 calc GR . . . .
C37 C 0.0758(3) 0.9470(4) 0.5553(2) 0.0578(9) Uani 1 1 d . . . . .
H37A H 0.1090 0.8765 0.5730 0.069 Uiso 1 1 calc R . . . .
H37B H 0.1135 1.0150 0.5930 0.069 Uiso 1 1 calc R . . . .
C39 C -0.1057(4) 1.0310(4) 0.5207(3) 0.0659(11) Uani 1 1 d . . . . .
H39A H -0.0729 1.1012 0.5575 0.079 Uiso 1 1 calc R . . . .
H39B H -0.1940 1.0175 0.5150 0.079 Uiso 1 1 calc R . . . .
N2A N -0.4061(9) 0.5380(10) 0.5674(5) 0.033(2) Uani 0.3 1 d . . P B 1
H2A H -0.3961 0.4605 0.5873 0.040 Uiso 0.3 1 calc R . P B 1
C40 C -0.3330(3) 0.6407(3) 0.62290(18) 0.0488(8) Uani 1 1 d . . . . .
H40A H -0.3433 0.7148 0.6009 0.073 Uiso 0.3 1 calc R . P B 1
H40B H -0.2479 0.6313 0.6330 0.073 Uiso 0.3 1 calc R . P B 1
H40C H -0.3610 0.6419 0.6703 0.073 Uiso 0.3 1 calc R . P B 1
H40D H -0.3585 0.7130 0.6420 0.073 Uiso 0.7 1 calc R . P B 2
H40E H -0.2511 0.6584 0.6153 0.073 Uiso 0.7 1 calc R . P B 2
H40F H -0.3353 0.5829 0.6596 0.073 Uiso 0.7 1 calc R . P B 2
C41 C -0.5422(3) 0.5641(3) 0.55732(18) 0.0513(8) Uani 1 1 d . . . . .
H41A H -0.5637 0.5755 0.6071 0.062 Uiso 0.3 1 calc R . P B 1
H41B H -0.5528 0.6356 0.5313 0.062 Uiso 0.3 1 calc R . P B 1
H41C H -0.5691 0.6356 0.5778 0.062 Uiso 0.7 1 calc R . P B 2
H41D H -0.5484 0.5036 0.5927 0.062 Uiso 0.7 1 calc R . P B 2
C42B C -0.3827(10) 0.5401(12) 0.4886(6) 0.042(2) Uani 0.3 1 d . . P B 1
H42A H -0.4043 0.6129 0.4673 0.050 Uiso 0.3 1 calc R . P B 1
H42B H -0.2968 0.5370 0.4898 0.050 Uiso 0.3 1 calc R . P B 1
O9B O -0.5406(2) 1.1695(2) 0.76429(16) 0.0613(6) Uani 0.25 1 d . . P C 2
H9BA H -0.4748 1.1438 0.7752 0.092 Uiso 0.25 1 calc GR . P C 2
C43A C -0.4988(5) 1.1638(5) 0.8426(3) 0.0669(14) Uani 0.75 1 d . . P D 1
H43D H -0.4466 1.1029 0.8501 0.100 Uiso 0.75 1 calc GR . P D 1
H43E H -0.5674 1.1445 0.8660 0.100 Uiso 0.75 1 calc GR . P D 1
H43F H -0.4535 1.2400 0.8661 0.100 Uiso 0.75 1 calc GR . P D 1
O10 O -0.1188(3) 0.6961(3) 0.47900(15) 0.0750(9) Uani 1 1 d . . . . .
H10 H -0.0455 0.6897 0.4876 0.113 Uiso 1 1 calc GR . . . .
C44 C -0.1719(4) 0.6578(4) 0.4017(2) 0.0671(11) Uani 1 1 d . . . . .
H44A H -0.1125 0.6753 0.3709 0.101 Uiso 1 1 calc GR . . . .
H44B H -0.2406 0.6990 0.3851 0.101 Uiso 1 1 calc GR . . . .
H44C H -0.1991 0.5729 0.3959 0.101 Uiso 1 1 calc GR . . . .
C45 C 0.2661(4) 0.4209(4) 0.8607(2) 0.0748(12) Uani 1 1 d . . . . .
H45A H 0.3539 0.4305 0.8703 0.112 Uiso 1 1 calc GR . . . .
H45B H 0.2362 0.3503 0.8819 0.112 Uiso 1 1 calc GR . . . .
H45C H 0.2411 0.4900 0.8845 0.112 Uiso 1 1 calc GR . . . .
O9A O -0.5406(2) 1.1695(2) 0.76429(16) 0.0613(6) Uani 0.75 1 d . . P D 1
H9AA H -0.6109 1.1332 0.7504 0.092 Uiso 0.75 1 calc DGR . P D 1
C43B C -0.5811(12) 1.1605(11) 0.6832(7) 0.048(3) Uani 0.25 1 d . . P C 2
H43A H -0.6642 1.1208 0.6687 0.073 Uiso 0.25 1 calc GR . P C 2
H43B H -0.5297 1.1152 0.6593 0.073 Uiso 0.25 1 calc GR . P C 2
H43C H -0.5767 1.2395 0.6664 0.073 Uiso 0.25 1 calc GR . P C 2
Cl3B Cl -0.3802(7) 0.8595(6) 0.4773(5) 0.0694(15) Uani 0.35 1 d . U P E 2
Cl3C Cl -0.3985(11) 0.8030(11) 0.4667(8) 0.092(3) Uani 0.35 1 d . U P F 3
C42A C -0.3764(5) 0.4823(5) 0.5221(3) 0.0503(12) Uani 0.7 1 d . . P B 2
H42C H -0.3836 0.4225 0.5579 0.060 Uiso 0.7 1 calc R . P B 2
H42D H -0.2914 0.4980 0.5183 0.060 Uiso 0.7 1 calc R . P B 2
N2B N -0.4153(4) 0.5919(5) 0.5499(3) 0.0424(10) Uani 0.7 1 d . . P B 2
H2B H -0.4109 0.6503 0.5122 0.051 Uiso 0.7 1 calc R . P B 2
O12A O -0.3902(6) 0.3073(7) 0.5906(4) 0.0442(17) Uani 0.3 1 d . . P G 1
H12A H -0.4490 0.2495 0.5754 0.066 Uiso 0.3 1 d G . P G 1
H12B H -0.3462 0.2942 0.6333 0.066 Uiso 0.3 1 d G . P G 1
Cl3D Cl -0.367(3) 0.830(3) 0.4581(14) 0.094(8) Uani 0.15 1 d . U P H 4
O12D O -0.3461(16) 0.075(2) 0.4171(15) 0.098(7) Uani 0.2 1 d . U P I 4
O12B O -0.3393(7) 0.1568(9) 0.5592(4) 0.091(2) Uani 0.5 1 d . . P J 2
O12E O -0.3562(6) 0.1404(5) 0.4412(3) 0.0776(18) Uani 0.6 1 d . U P K 5
O12C O -0.373(3) 0.212(2) 0.5760(17) 0.095(10) Uani 0.15 1 d . U P L 3
O12F O -0.368(4) 0.152(4) 0.499(2) 0.099(11) Uani 0.1 1 d . U P M 6
O12G O -0.4051(18) 0.068(2) 0.5494(12) 0.084(6) Uani 0.15 1 d . . P N 7
H6 H -0.139(3) 0.396(3) 0.628(2) 0.051(11) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
O6 C22 1.376(3) . ?
O2 C4 1.375(4) . ?
O5 C20 1.376(3) . ?
O1 C2 1.379(3) . ?
C24 C23 1.396(3) . ?
C24 C19 1.394(4) . ?
O8 C31 1.388(3) . ?
O4 C13 1.371(3) . ?
C28 C25 1.526(4) . ?
C28 C33 1.387(4) . ?
C28 C29 1.400(4) . ?
O3 C11 1.378(3) . ?
C7 C10 1.514(4) . ?
C7 C5 1.529(4) . ?
C7 C8 1.544(3) . ?
C14 C13 1.397(4) . ?
C14 C15 1.387(4) . ?
C14 C16 1.523(4) . ?
C25 C23 1.522(3) . ?
C25 C26 1.541(3) . ?
C34 C32 1.524(4) . ?
C34 C1 1.510(4) . ?
C34 C35 1.539(4) . ?
C23 C22 1.401(3) . ?
C19 C16 1.517(3) . ?
C19 C20 1.401(3) . ?
C6 C5 1.389(4) . ?
C6 C1 1.399(4) . ?
C33 C32 1.395(4) . ?
C13 C12 1.393(4) . ?
C15 C10 1.397(4) . ?
C16 C17 1.535(3) . ?
C32 C31 1.398(4) . ?
C10 C11 1.393(4) . ?
C26 C27 1.522(4) . ?
C21 C20 1.391(4) . ?
C21 C22 1.387(4) . ?
C11 C12 1.380(4) . ?
C29 O7 1.374(3) . ?
C29 C30 1.384(4) . ?
C17 C18 1.527(4) . ?
C5 C4 1.396(4) . ?
C3 C2 1.391(4) . ?
C3 C4 1.383(4) . ?
C2 C1 1.402(4) . ?
C8 C9 1.522(4) . ?
C31 C30 1.389(4) . ?
C35 C36 1.527(4) . ?
O11 C45 1.394(4) . ?
N1 C38 1.487(4) . ?
N1 C37 1.481(5) . ?
N1 C39 1.453(5) . ?
C37 C39 1.523(5) 2_576 ?
C39 C37 1.523(5) 2_576 ?
N2A C40 1.529(10) . ?
N2A C41 1.608(11) . ?
N2A C42B 1.512(14) . ?
C40 N2B 1.486(5) . ?
C41 C42B 1.473(13) 2_466 ?
C41 C42A 1.563(6) 2_466 ?
C41 N2B 1.490(6) . ?
C42B C41 1.473(12) 2_466 ?
O9B C43B 1.443(13) . ?
O10 C44 1.422(4) . ?
C42A C41 1.563(6) 2_466 ?
C42A N2B 1.480(7) . ?

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
C19 C24 C23 123.7(2) . . ?
C33 C28 C25 121.1(2) . . ?
C33 C28 C29 116.9(2) . . ?
C29 C28 C25 121.9(2) . . ?
C10 C7 C5 111.37(19) . . ?
C10 C7 C8 110.5(2) . . ?
C5 C7 C8 113.3(2) . . ?
C13 C14 C16 122.2(2) . . ?
C15 C14 C13 116.7(2) . . ?
C15 C14 C16 121.0(2) . . ?
C28 C25 C26 110.7(2) . . ?
C23 C25 C28 111.0(2) . . ?
C23 C25 C26 113.5(2) . . ?
C32 C34 C35 110.5(2) . . ?
C1 C34 C32 110.3(2) . . ?
C1 C34 C35 114.3(2) . . ?
C24 C23 C25 123.6(2) . . ?
C24 C23 C22 116.9(2) . . ?
C22 C23 C25 119.5(2) . . ?
C24 C19 C16 124.0(2) . . ?
C24 C19 C20 117.0(2) . . ?
C20 C19 C16 119.0(2) . . ?
C5 C6 C1 123.2(2) . . ?
C28 C33 C32 124.1(2) . . ?
O4 C13 C14 120.9(2) . . ?
O4 C13 C12 118.2(2) . . ?
C12 C13 C14 120.9(3) . . ?
C14 C15 C10 124.1(2) . . ?
C14 C16 C17 110.35(19) . . ?
C19 C16 C14 111.8(2) . . ?
C19 C16 C17 113.6(2) . . ?
C33 C32 C34 120.5(2) . . ?
C33 C32 C31 116.7(2) . . ?
C31 C32 C34 122.8(2) . . ?
C15 C10 C7 121.5(2) . . ?
C11 C10 C7 121.5(2) . . ?
C11 C10 C15 117.0(2) . . ?
C27 C26 C25 112.0(2) . . ?
C22 C21 C20 119.7(2) . . ?
O3 C11 C10 117.6(3) . . ?
O3 C11 C12 121.5(2) . . ?
C12 C11 C10 120.9(3) . . ?
O7 C29 C28 119.7(3) . . ?
O7 C29 C30 119.2(2) . . ?
C30 C29 C28 121.1(2) . . ?
C11 C12 C13 120.4(2) . . ?
C18 C17 C16 113.1(2) . . ?
C6 C5 C7 122.5(2) . . ?
C6 C5 C4 118.2(2) . . ?
C4 C5 C7 119.3(2) . . ?
O5 C20 C19 116.9(2) . . ?
O5 C20 C21 121.8(2) . . ?
C21 C20 C19 121.3(2) . . ?
C4 C3 C2 120.0(2) . . ?
O6 C22 C23 117.2(2) . . ?
O6 C22 C21 121.5(2) . . ?
C21 C22 C23 121.4(2) . . ?
O1 C2 C3 120.8(2) . . ?
O1 C2 C1 117.7(3) . . ?
C3 C2 C1 121.5(2) . . ?
C9 C8 C7 112.5(2) . . ?
O8 C31 C32 121.4(2) . . ?
O8 C31 C30 117.5(2) . . ?
C30 C31 C32 121.1(2) . . ?
O2 C4 C5 120.2(2) . . ?
O2 C4 C3 119.2(2) . . ?
C3 C4 C5 120.6(3) . . ?
C6 C1 C34 123.0(2) . . ?
C6 C1 C2 116.6(3) . . ?
C2 C1 C34 120.4(2) . . ?
C29 C30 C31 120.0(2) . . ?
C36 C35 C34 112.5(2) . . ?
C37 N1 C38 112.4(3) . . ?
C39 N1 C38 113.1(3) . . ?
C39 N1 C37 109.8(3) . . ?
N1 C37 C39 110.9(3) . 2_576 ?
N1 C39 C37 110.8(3) . 2_576 ?
C40 N2A C41 103.9(6) . . ?
C42B N2A C40 113.2(8) . . ?
C42B N2A C41 103.7(8) . . ?
C42B C41 N2A 105.6(6) 2_466 . ?
N2B C41 C42A 109.2(3) . 2_466 ?
C41 C42B N2A 106.7(9) 2_466 . ?
N2B C42A C41 108.6(4) . 2_466 ?
C40 N2B C41 112.3(3) . . ?
C42A N2B C40 108.8(4) . . ?
C42A N2B C41 108.4(4) . . ?

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 C2 C1 C34 1.7(4) . . . . ?
O1 C2 C1 C6 179.7(2) . . . . ?
C24 C23 C22 O6 -178.9(2) . . . . ?
C24 C23 C22 C21 0.4(4) . . . . ?
C24 C19 C16 C14 -100.8(3) . . . . ?
C24 C19 C16 C17 24.9(3) . . . . ?
C24 C19 C20 O5 -179.1(2) . . . . ?
C24 C19 C20 C21 1.5(4) . . . . ?
O8 C31 C30 C29 177.5(3) . . . . ?
O4 C13 C12 C11 179.3(3) . . . . ?
C28 C25 C23 C24 102.9(3) . . . . ?
C28 C25 C23 C22 -77.2(3) . . . . ?
C28 C25 C26 C27 58.2(3) . . . . ?
C28 C33 C32 C34 174.0(2) . . . . ?
C28 C33 C32 C31 -3.5(4) . . . . ?
C28 C29 C30 C31 -1.8(4) . . . . ?
O3 C11 C12 C13 -178.6(3) . . . . ?
C7 C10 C11 O3 -5.1(4) . . . . ?
C7 C10 C11 C12 176.9(3) . . . . ?
C7 C5 C4 O2 0.6(4) . . . . ?
C7 C5 C4 C3 179.4(2) . . . . ?
C14 C13 C12 C11 -0.5(4) . . . . ?
C14 C15 C10 C7 -175.4(2) . . . . ?
C14 C15 C10 C11 1.2(4) . . . . ?
C14 C16 C17 C18 -58.2(3) . . . . ?
C25 C28 C33 C32 -176.0(2) . . . . ?
C25 C28 C29 O7 -2.0(4) . . . . ?
C25 C28 C29 C30 178.7(3) . . . . ?
C25 C23 C22 O6 1.2(3) . . . . ?
C25 C23 C22 C21 -179.5(2) . . . . ?
C34 C32 C31 O8 7.6(4) . . . . ?
C34 C32 C31 C30 -173.7(3) . . . . ?
C23 C24 C19 C16 179.0(2) . . . . ?
C23 C24 C19 C20 -0.6(3) . . . . ?
C23 C25 C26 C27 -176.2(2) . . . . ?
C19 C24 C23 C25 179.6(2) . . . . ?
C19 C24 C23 C22 -0.3(3) . . . . ?
C19 C16 C17 C18 175.3(2) . . . . ?
C6 C5 C4 O2 -178.2(2) . . . . ?
C6 C5 C4 C3 0.6(4) . . . . ?
C33 C28 C25 C23 -67.9(3) . . . . ?
C33 C28 C25 C26 59.1(3) . . . . ?
C33 C28 C29 O7 -178.6(3) . . . . ?
C33 C28 C29 C30 2.1(4) . . . . ?
C33 C32 C31 O8 -175.0(3) . . . . ?
C33 C32 C31 C30 3.7(4) . . . . ?
C13 C14 C15 C10 -2.2(4) . . . . ?
C13 C14 C16 C19 -118.1(2) . . . . ?
C13 C14 C16 C17 114.4(2) . . . . ?
C15 C14 C13 O4 -177.9(2) . . . . ?
C15 C14 C13 C12 1.8(4) . . . . ?
C15 C14 C16 C19 66.1(3) . . . . ?
C15 C14 C16 C17 -61.4(3) . . . . ?
C15 C10 C11 O3 178.3(2) . . . . ?
C15 C10 C11 C12 0.3(4) . . . . ?
C16 C14 C13 O4 6.2(4) . . . . ?
C16 C14 C13 C12 -174.1(2) . . . . ?
C16 C14 C15 C10 173.8(2) . . . . ?
C16 C19 C20 O5 1.3(3) . . . . ?
C16 C19 C20 C21 -178.1(2) . . . . ?
C32 C34 C1 C6 -104.9(3) . . . . ?
C32 C34 C1 C2 73.0(3) . . . . ?
C32 C34 C35 C36 -60.7(3) . . . . ?
C32 C31 C30 C29 -1.2(4) . . . . ?
C10 C7 C5 C6 105.7(3) . . . . ?
C10 C7 C5 C4 -73.1(3) . . . . ?
C10 C7 C8 C9 59.0(3) . . . . ?
C10 C11 C12 C13 -0.7(4) . . . . ?
C26 C25 C23 C24 -22.5(3) . . . . ?
C26 C25 C23 C22 157.4(2) . . . . ?
C29 C28 C25 C23 115.6(3) . . . . ?
C29 C28 C25 C26 -117.4(3) . . . . ?
C29 C28 C33 C32 0.6(4) . . . . ?
C5 C7 C10 C15 -66.1(3) . . . . ?
C5 C7 C10 C11 117.5(3) . . . . ?
C5 C7 C8 C9 -175.1(2) . . . . ?
C5 C6 C1 C34 177.2(2) . . . . ?
C5 C6 C1 C2 -0.7(4) . . . . ?
C20 C19 C16 C14 78.8(3) . . . . ?
C20 C19 C16 C17 -155.5(2) . . . . ?
C20 C21 C22 O6 179.7(2) . . . . ?
C20 C21 C22 C23 0.5(4) . . . . ?
C3 C2 C1 C34 -176.7(2) . . . . ?
C3 C2 C1 C6 1.3(4) . . . . ?
C22 C21 C20 O5 179.2(2) . . . . ?
C22 C21 C20 C19 -1.4(4) . . . . ?
O7 C29 C30 C31 178.9(3) . . . . ?
C2 C3 C4 O2 178.7(3) . . . . ?
C2 C3 C4 C5 -0.1(4) . . . . ?
C8 C7 C10 C15 60.8(3) . . . . ?
C8 C7 C10 C11 -115.6(3) . . . . ?
C8 C7 C5 C6 -19.7(3) . . . . ?
C8 C7 C5 C4 161.6(2) . . . . ?
C4 C3 C2 O1 -179.3(3) . . . . ?
C4 C3 C2 C1 -1.0(4) . . . . ?
C1 C34 C32 C33 70.0(3) . . . . ?
C1 C34 C32 C31 -112.7(3) . . . . ?
C1 C34 C35 C36 174.3(2) . . . . ?
C1 C6 C5 C7 -179.0(2) . . . . ?
C1 C6 C5 C4 -0.2(4) . . . . ?
C35 C34 C32 C33 -57.3(3) . . . . ?
C35 C34 C32 C31 120.1(3) . . . . ?
C35 C34 C1 C6 20.2(3) . . . . ?
C35 C34 C1 C2 -161.9(2) . . . . ?
C38 N1 C37 C39 175.9(3) . . . 2_576 ?
C38 N1 C39 C37 -176.4(3) . . . 2_576 ?
C37 N1 C39 C37 57.1(5) . . . 2_576 ?
C39 N1 C37 C39 -57.2(5) . . . 2_576 ?
N2A C40 N2B C41 80.7(10) . . . . ?
N2A C40 N2B C42A -39.3(9) . . . . ?
N2A C41 N2B C40 -76.6(10) . . . . ?
N2A C41 N2B C42A 43.7(9) . . . . ?
C40 N2A C41 C42B -173.5(6) . . . 2_466 ?
C40 N2A C41 C42A 149.5(5) . . . 2_466 ?
C40 N2A C41 N2B 64.3(9) . . . . ?
C40 N2A C42B C41 179.3(7) . . . 2_466 ?
C41 N2A C40 N2B -60.7(9) . . . . ?
C41 N2A C42B C41 -68.7(10) . . . 2_466 ?
C41 C42A N2B C40 -176.2(4) 2_466 . . . ?
C41 C42A N2B C41 61.4(6) 2_466 . . . ?
C42B N2A C40 N2B 51.2(9) . . . . ?
C42B N2A C41 C42B 67.9(11) . . . 2_466 ?
C42B N2A C41 C42A 30.9(10) . . . 2_466 ?
C42B N2A C41 N2B -54.3(9) . . . . ?
C42B C41 N2B C40 -144.1(6) 2_466 . . . ?
C42B C41 N2B C42A -23.8(9) 2_466 . . . ?
C42A C41 N2B C40 178.0(4) 2_466 . . . ?
C42A C41 N2B C42A -61.8(6) 2_466 . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_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
0 0 11 0.0565 0.0080 -0.0103 11.4957 -0.4176 -0.8669 -0.2773
-4 0 -9 0.0551 -3.5075 -0.4873 -8.7385 0.0511 0.7898 0.6119
-6 3 7 0.0881 -5.9962 3.0002 6.5228 -0.3071 -0.5728 0.7054
-4 -1 11 0.0680 -4.4942 -0.5034 10.7569 -0.7188 -0.6544 0.2627
1 -3 -11 0.0639 0.9918 -2.9901 -10.5075 0.1429 1.0036 -0.0038
5 1 6 0.0534 5.0066 0.9870 6.4866 0.1734 -0.6986 -0.7166
3 2 -11 0.0738 2.9942 2.0046 -10.9984 0.7852 0.5931 -0.0072
2 -7 2 0.0909 1.9995 -7.0004 2.4733 -0.6675 0.3149 -0.6197
0 0 -12 0.0402 0.4918 -0.4899 -11.7484 0.4076 0.9125 0.2002
-7 -1 0 0.0699 -7.0027 -0.9902 0.0164 -0.5332 0.2603 0.8019
7 1 0 0.0741 7.0027 0.9902 -0.0164 0.5332 -0.2603 -0.8019
6 -3 5 0.0762 6.0042 -3.0104 4.9729 -0.1105 -0.2942 -0.9828
-2 7 -2 0.1056 -1.9995 7.0004 -2.4733 0.6675 -0.3149 0.6197
-2 5 7 0.0934 -2.4935 5.4933 7.2700 0.1324 -0.9181 0.3771
6 -4 -5 0.0946 6.4970 -3.5016 -5.2761 0.2426 0.5053 -0.8188

