# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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/access/V1 
# 
# Audit and citation data items may have 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_L0H-3(AcOEt)
_database_code_depnum_ccdc_archive 'CCDC 1042059'
_audit_update_record             
;
2015-01-05 deposited with the CCDC.
2015-03-18 downloaded from the CCDC.
;
_audit_creation_date             2014-09-04
_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        
; 
[{t-BuC6H4)3CCONH}2C6H3COOH]-3(AcOEt) 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C83 H108 N2 O10'
_chemical_formula_sum            'C83 H108 N2 O10'
_chemical_formula_weight         1293.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   18.9473(8)
_cell_length_b                   13.9306(6)
_cell_length_c                   28.662(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.968(7)
_cell_angle_gamma                90
_cell_volume                     7509.4(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    200
_cell_measurement_reflns_used    14201
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      27.47

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_F_000             2800
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    0.074
_shelx_estimated_absorpt_T_min   0.978
_shelx_estimated_absorpt_T_max   0.978
_exptl_absorpt_correction_type   none
_diffrn_ambient_temperature      200
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   
;
 MicroMax-007HF microfocus rotating anode X-ray generator
;
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            28924
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.011
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.970
_reflns_number_total             13050
_reflns_number_gt                10640
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.970

_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.
;

_computing_data_collection       'RAPID AUTO (Rigaku, 2006)'
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2006)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2006)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
Two t-Bu groups (C118-C120, C218-C220) were disordered. These were separated 
into two parts and the occupancies were refined. Because the C-C bonds in the 
disordered t-Bu group were unusually deviated from the typical values, SADI 
instruction was used. Other unusual distances, C43-C44, C31-C32, and C237-C240 
were restrainted. Unusual displacements of anisotropic factors were restrained 
by ISOR and DELU instructions. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1485P)²+1.6883P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   1(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         13050
_refine_ls_number_parameters     917
_refine_ls_number_restraints     115
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0770
_refine_ls_wR_factor_ref         0.2156
_refine_ls_wR_factor_gt          0.2036
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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 0.7605(3) 0.8232(3) 0.45847(15) 0.0869(17) Uani 1 1 d . . . . .
O2 O 0.6406(3) 0.7589(3) 0.70790(15) 0.0688(12) Uani 1 1 d . . . . .
O11 O 0.6723(3) 0.5403(3) 0.53567(14) 0.0721(12) Uani 1 1 d . . . . .
O12 O 0.7252(3) 0.5211(3) 0.60815(14) 0.0745(13) Uani 1 1 d . . . . .
H3 H 0.7528 0.4799 0.5989 0.089 Uiso 1 1 calc R U . . .
O31 O 0.6919(5) 0.3321(4) 0.5929(3) 0.115(2) Uani 1 1 d . . . . .
O32 O 0.6096(4) 0.2216(4) 0.59236(19) 0.0949(16) Uani 1 1 d . . . . .
O41 O 0.4844(6) 0.5349(8) 0.5922(3) 0.159(4) Uani 1 1 d . . . . .
O42 O 0.4397(4) 0.6631(7) 0.5581(4) 0.155(4) Uani 1 1 d . . . . .
O51 O 0.9452(17) 0.4831(18) 0.6030(12) 0.40(2) Uani 1 1 d . U . . .
O52 O 0.8819(4) 0.5906(6) 0.5694(2) 0.114(2) Uani 1 1 d . . . . .
N1 N 0.7092(2) 0.7039(3) 0.49635(14) 0.0482(10) Uani 1 1 d . . . . .
H1 H 0.6913 0.6457 0.4926 0.058 Uiso 1 1 calc R U . . .
N2 N 0.7037(2) 0.6630(3) 0.66513(14) 0.0495(10) Uani 1 1 d . . . . .
H2 H 0.7229 0.6055 0.6642 0.059 Uiso 1 1 calc R U . . .
C1 C 0.7009(3) 0.5755(4) 0.57323(19) 0.0557(13) Uani 1 1 d . . . . .
C11 C 0.7069(3) 0.6815(4) 0.58074(17) 0.0439(10) Uani 1 1 d . . . . .
C12 C 0.7111(3) 0.7429(3) 0.54133(16) 0.0430(10) Uani 1 1 d . . . . .
C13 C 0.7167(3) 0.8428(4) 0.54855(18) 0.0554(13) Uani 1 1 d . . . . .
H4 H 0.7211 0.8847 0.5229 0.067 Uiso 1 1 calc R U . . .
C14 C 0.7156(4) 0.8788(4) 0.5931(2) 0.0602(14) Uani 1 1 d . . . . .
H5 H 0.7184 0.9464 0.5974 0.072 Uiso 1 1 calc R U . . .
C15 C 0.7106(3) 0.8219(4) 0.63157(18) 0.0529(13) Uani 1 1 d . . . . .
H6 H 0.7101 0.8495 0.6618 0.063 Uiso 1 1 calc R U . . .
C16 C 0.7063(3) 0.7217(4) 0.62539(16) 0.0436(10) Uani 1 1 d . . . . .
C17 C 0.7317(3) 0.7447(4) 0.45736(17) 0.0487(12) Uani 1 1 d . . . . .
C18 C 0.7226(3) 0.6816(3) 0.41192(16) 0.0420(10) Uani 1 1 d . . . . .
C27 C 0.6748(3) 0.6858(3) 0.70452(17) 0.0440(11) Uani 1 1 d . . . . .
C28 C 0.6848(3) 0.6112(3) 0.74559(16) 0.0400(10) Uani 1 1 d . . . . .
C31 C 0.6365(6) 0.3058(6) 0.6032(3) 0.091(2) Uani 1 1 d D . . . .
C32 C 0.5943(6) 0.3676(8) 0.6309(4) 0.119(3) Uani 1 1 d D . . . .
H85 H 0.5661 0.4124 0.6100 0.143 Uiso 1 1 calc R U . . .
H86 H 0.6263 0.4038 0.6540 0.143 Uiso 1 1 calc R U . . .
H87 H 0.5626 0.3278 0.6474 0.143 Uiso 1 1 calc R U . . .
C33 C 0.6462(7) 0.1581(6) 0.5641(3) 0.110(3) Uani 1 1 d . . . . .
H88 H 0.6917 0.1367 0.5818 0.132 Uiso 1 1 calc R U . . .
H89 H 0.6566 0.1910 0.5351 0.132 Uiso 1 1 calc R U . . .
C34 C 0.5989(8) 0.0750(8) 0.5523(5) 0.153(6) Uani 1 1 d . . . . .
H90 H 0.6221 0.0296 0.5329 0.184 Uiso 1 1 calc R U . . .
H91 H 0.5890 0.0431 0.5813 0.184 Uiso 1 1 calc R U . . .
H92 H 0.5542 0.0971 0.5349 0.184 Uiso 1 1 calc R U . . .
C41 C 0.4360(6) 0.5800(8) 0.5760(3) 0.106(3) Uani 1 1 d . . . . .
C42 C 0.3611(7) 0.5469(12) 0.5736(5) 0.143(5) Uani 1 1 d . . . . .
H93 H 0.3523 0.5221 0.6043 0.172 Uiso 1 1 calc R U . . .
H94 H 0.3527 0.4959 0.5500 0.172 Uiso 1 1 calc R U . . .
H95 H 0.3290 0.6008 0.5647 0.172 Uiso 1 1 calc R U . . .
C43 C 0.5146(8) 0.686(2) 0.5538(10) 0.226(10) Uani 1 1 d D U . . .
H96 H 0.5468 0.6490 0.5769 0.271 Uiso 1 1 calc R U . . .
H97 H 0.5260 0.6712 0.5218 0.271 Uiso 1 1 calc R U . . .
C44 C 0.5221(11) 0.788(2) 0.5632(16) 0.36(2) Uani 1 1 d D U . . .
H98 H 0.5712 0.8081 0.5608 0.428 Uiso 1 1 calc R U . . .
H99 H 0.4898 0.8241 0.5401 0.428 Uiso 1 1 calc R U . . .
H100 H 0.5104 0.8021 0.5949 0.428 Uiso 1 1 calc R U . . .
C51 C 0.8930(7) 0.5012(11) 0.5830(5) 0.127(4) Uani 1 1 d . . . . .
C52 C 0.8576(8) 0.4279(8) 0.5500(4) 0.127(4) Uani 1 1 d . . . . .
H101 H 0.8560 0.3663 0.5664 0.153 Uiso 1 1 calc R U . . .
H102 H 0.8846 0.4206 0.5231 0.153 Uiso 1 1 calc R U . . .
H103 H 0.8091 0.4488 0.5389 0.153 Uiso 1 1 calc R U . . .
C53 C 0.9094(7) 0.6622(11) 0.6084(10) 0.214(11) Uani 1 1 d . . . . .
H104 H 0.9584 0.6476 0.6226 0.256 Uiso 1 1 calc R U . . .
H105 H 0.8775 0.6668 0.6333 0.256 Uiso 1 1 calc R U . . .
C54 C 0.9056(8) 0.7545(13) 0.5760(5) 0.154(5) Uani 1 1 d . . . . .
H106 H 0.9216 0.8106 0.5950 0.185 Uiso 1 1 calc R U . . .
H107 H 0.9363 0.7454 0.5512 0.185 Uiso 1 1 calc R U . . .
H108 H 0.8565 0.7644 0.5617 0.185 Uiso 1 1 calc R U . . .
C111 C 0.6674(2) 0.6021(3) 0.41680(15) 0.0399(10) Uani 1 1 d . . . . .
C112 C 0.5975(3) 0.6268(4) 0.42361(17) 0.0457(11) Uani 1 1 d . . . . .
H7 H 0.5846 0.6926 0.4244 0.055 Uiso 1 1 calc R U . . .
C113 C 0.5469(3) 0.5567(4) 0.42921(18) 0.0473(11) Uani 1 1 d . . . . .
H8 H 0.5005 0.5762 0.4345 0.057 Uiso 1 1 calc R U . . .
C114 C 0.5618(3) 0.4594(4) 0.42741(16) 0.0430(11) Uani 1 1 d . . . . .
C115 C 0.6310(3) 0.4358(4) 0.41964(17) 0.0458(11) Uani 1 1 d . . . . .
H9 H 0.6432 0.3699 0.4175 0.055 Uiso 1 1 calc R U . . .
C116 C 0.6830(3) 0.5045(3) 0.41496(16) 0.0428(10) Uani 1 1 d . . . . .
H10 H 0.7296 0.4847 0.4105 0.051 Uiso 1 1 calc R U . . .
C117 C 0.5068(3) 0.3813(4) 0.4337(2) 0.0575(13) Uani 1 1 d D U . . .
C118 C 0.4371(6) 0.4208(8) 0.4446(7) 0.084(5) Uani 0.67(2) 1 d D . P A 1
H11 H 0.4042 0.3678 0.4482 0.101 Uiso 0.67(2) 1 calc R U P A 1
H12 H 0.4445 0.4578 0.4738 0.101 Uiso 0.67(2) 1 calc R U P A 1
H13 H 0.4170 0.4626 0.4188 0.101 Uiso 0.67(2) 1 calc R U P A 1
C119 C 0.4939(8) 0.3215(9) 0.3884(4) 0.086(5) Uani 0.67(2) 1 d D . P A 1
H14 H 0.5392 0.2953 0.3809 0.103 Uiso 0.67(2) 1 calc R U P A 1
H15 H 0.4612 0.2687 0.3929 0.103 Uiso 0.67(2) 1 calc R U P A 1
H16 H 0.4731 0.3624 0.3625 0.103 Uiso 0.67(2) 1 calc R U P A 1
C120 C 0.5380(6) 0.3129(10) 0.4729(5) 0.078(4) Uani 0.67(2) 1 d D . P A 1
H17 H 0.5835 0.2876 0.4653 0.093 Uiso 0.67(2) 1 calc R U P A 1
H18 H 0.5455 0.3478 0.5028 0.093 Uiso 0.67(2) 1 calc R U P A 1
H19 H 0.5049 0.2597 0.4755 0.093 Uiso 0.67(2) 1 calc R U P A 1
C148 C 0.467(2) 0.409(2) 0.4763(12) 0.099(10) Uani 0.33(2) 1 d D U P A 2
H11B H 0.4498 0.4754 0.4725 0.119 Uiso 0.33(2) 1 calc R U P A 2
H12B H 0.4266 0.3659 0.4778 0.119 Uiso 0.33(2) 1 calc R U P A 2
H13B H 0.4997 0.4039 0.5054 0.119 Uiso 0.33(2) 1 calc R U P A 2
C149 C 0.4454(14) 0.392(2) 0.3927(10) 0.102(10) Uani 0.33(2) 1 d D U P A 2
H14B H 0.4278 0.4587 0.3919 0.123 Uiso 0.33(2) 1 calc R U P A 2
H15B H 0.4632 0.3773 0.3629 0.123 Uiso 0.33(2) 1 calc R U P A 2
H16B H 0.4066 0.3485 0.3976 0.123 Uiso 0.33(2) 1 calc R U P A 2
C150 C 0.5351(15) 0.2811(12) 0.4362(16) 0.099(10) Uani 0.33(2) 1 d D U P A 2
H17B H 0.4965 0.2361 0.4402 0.119 Uiso 0.33(2) 1 calc R U P A 2
H18B H 0.5552 0.2660 0.4071 0.119 Uiso 0.33(2) 1 calc R U P A 2
H19B H 0.5723 0.2754 0.4630 0.119 Uiso 0.33(2) 1 calc R U P A 2
C121 C 0.7964(3) 0.6370(4) 0.40750(16) 0.0437(11) Uani 1 1 d . . . . .
C122 C 0.8175(3) 0.6165(4) 0.36367(17) 0.0492(12) Uani 1 1 d . . . . .
H20 H 0.7883 0.6363 0.3361 0.059 Uiso 1 1 calc R U . . .
C123 C 0.8797(3) 0.5682(4) 0.35939(18) 0.0492(12) Uani 1 1 d . . . . .
H21 H 0.8920 0.5557 0.3288 0.059 Uiso 1 1 calc R U . . .
C124 C 0.9254(3) 0.5370(4) 0.39814(19) 0.0485(12) Uani 1 1 d . . . . .
C125 C 0.9056(3) 0.5608(5) 0.4418(2) 0.0593(14) Uani 1 1 d . . . . .
H22 H 0.9359 0.5432 0.4693 0.071 Uiso 1 1 calc R U . . .
C126 C 0.8432(3) 0.6092(5) 0.44635(18) 0.0584(14) Uani 1 1 d . . . . .
H23 H 0.8318 0.6240 0.4769 0.070 Uiso 1 1 calc R U . . .
C127 C 0.9952(3) 0.4824(4) 0.3917(2) 0.0593(14) Uani 1 1 d . U . . .
C128 C 0.9817(5) 0.4056(9) 0.3547(5) 0.144(5) Uani 1 1 d . U . . .
H24 H 0.9471 0.3594 0.3641 0.173 Uiso 1 1 calc R U . . .
H25 H 0.9629 0.4351 0.3247 0.173 Uiso 1 1 calc R U . . .
H26 H 1.0264 0.3724 0.3511 0.173 Uiso 1 1 calc R U . . .
C129 C 1.0466(5) 0.5482(7) 0.3757(7) 0.166(7) Uani 1 1 d . U . . .
H27 H 1.0569 0.5996 0.3989 0.199 Uiso 1 1 calc R U . . .
H28 H 1.0905 0.5134 0.3720 0.199 Uiso 1 1 calc R U . . .
H29 H 1.0271 0.5761 0.3455 0.199 Uiso 1 1 calc R U . . .
C130 C 1.0240(9) 0.4284(15) 0.4362(5) 0.205(9) Uani 1 1 d . U . . .
H30 H 0.9873 0.3852 0.4454 0.246 Uiso 1 1 calc R U . . .
H31 H 1.0658 0.3909 0.4303 0.246 Uiso 1 1 calc R U . . .
H32 H 1.0375 0.4745 0.4616 0.246 Uiso 1 1 calc R U . . .
C131 C 0.6990(3) 0.7444(3) 0.36835(16) 0.0399(10) Uani 1 1 d . . . . .
C132 C 0.6470(3) 0.7125(4) 0.33274(17) 0.0511(12) Uani 1 1 d . . . . .
H33 H 0.6247 0.6524 0.3363 0.061 Uiso 1 1 calc R U . . .
C133 C 0.6274(3) 0.7657(4) 0.29285(17) 0.0494(12) Uani 1 1 d . . . . .
H34 H 0.5916 0.7410 0.2699 0.059 Uiso 1 1 calc R U . . .
C134 C 0.6575(3) 0.8534(4) 0.28471(18) 0.0457(11) Uani 1 1 d . . . . .
C135 C 0.7118(3) 0.8823(4) 0.3189(2) 0.0632(15) Uani 1 1 d . . . . .
H35 H 0.7363 0.9403 0.3142 0.076 Uiso 1 1 calc R U . . .
C136 C 0.7316(3) 0.8306(4) 0.3592(2) 0.0617(15) Uani 1 1 d . . . . .
H36 H 0.7687 0.8545 0.3815 0.074 Uiso 1 1 calc R U . . .
C137 C 0.6351(3) 0.9129(4) 0.24025(19) 0.0488(12) Uani 1 1 d . . . . .
C138 C 0.5586(4) 0.8902(5) 0.2191(3) 0.0761(19) Uani 1 1 d . . . . .
H37 H 0.5461 0.9292 0.1909 0.091 Uiso 1 1 calc R U . . .
H38 H 0.5548 0.8220 0.2108 0.091 Uiso 1 1 calc R U . . .
H39 H 0.5260 0.9048 0.2422 0.091 Uiso 1 1 calc R U . . .
C139 C 0.6860(4) 0.8903(5) 0.2038(2) 0.0733(18) Uani 1 1 d . . . . .
H40 H 0.7349 0.9047 0.2172 0.088 Uiso 1 1 calc R U . . .
H41 H 0.6822 0.8222 0.1953 0.088 Uiso 1 1 calc R U . . .
H42 H 0.6733 0.9297 0.1757 0.088 Uiso 1 1 calc R U . . .
C140 C 0.6391(4) 1.0212(4) 0.2515(2) 0.0672(16) Uani 1 1 d . . . . .
H43 H 0.6875 1.0378 0.2651 0.081 Uiso 1 1 calc R U . . .
H44 H 0.6265 1.0580 0.2226 0.081 Uiso 1 1 calc R U . . .
H45 H 0.6058 1.0366 0.2741 0.081 Uiso 1 1 calc R U . . .
C211 C 0.6101(2) 0.5675(3) 0.74861(16) 0.0400(10) Uani 1 1 d . . . . .
C212 C 0.5629(3) 0.5502(4) 0.70849(18) 0.0494(12) Uani 1 1 d . . . . .
H46 H 0.5736 0.5727 0.6789 0.059 Uiso 1 1 calc R U . . .
C213 C 0.4997(3) 0.5001(5) 0.71137(19) 0.0548(13) Uani 1 1 d . . . . .
H47 H 0.4685 0.4889 0.6834 0.066 Uiso 1 1 calc R U . . .
C214 C 0.4809(3) 0.4663(4) 0.75340(19) 0.0486(12) Uani 1 1 d . . . . .
C215 C 0.5274(3) 0.4858(4) 0.79361(18) 0.0491(12) Uani 1 1 d . . . . .
H48 H 0.5159 0.4642 0.8232 0.059 Uiso 1 1 calc R U . . .
C216 C 0.5903(3) 0.5364(4) 0.79142(17) 0.0444(11) Uani 1 1 d . . . . .
H49 H 0.6204 0.5499 0.8196 0.053 Uiso 1 1 calc R U . . .
C217 C 0.4121(3) 0.4079(5) 0.7567(2) 0.0634(15) Uani 1 1 d D . . . .
C218 C 0.3609(7) 0.4105(18) 0.7124(4) 0.117(8) Uani 0.71(2) 1 d D . P B 1
H50 H 0.3520 0.4773 0.7027 0.141 Uiso 0.71(2) 1 calc R U P B 1
H51 H 0.3813 0.3757 0.6875 0.141 Uiso 0.71(2) 1 calc R U P B 1
H52 H 0.3161 0.3802 0.7180 0.141 Uiso 0.71(2) 1 calc R U P B 1
C219 C 0.4285(8) 0.3061(10) 0.7739(10) 0.128(9) Uani 0.71(2) 1 d D . P B 1
H53 H 0.4619 0.3081 0.8028 0.154 Uiso 0.71(2) 1 calc R U P B 1
H54 H 0.3844 0.2746 0.7803 0.154 Uiso 0.71(2) 1 calc R U P B 1
H55 H 0.4496 0.2701 0.7498 0.154 Uiso 0.71(2) 1 calc R U P B 1
C220 C 0.3700(5) 0.4576(8) 0.7933(4) 0.083(4) Uani 0.71(2) 1 d D . P B 1
H56 H 0.3993 0.4594 0.8239 0.100 Uiso 0.71(2) 1 calc R U P B 1
H57 H 0.3577 0.5232 0.7830 0.100 Uiso 0.71(2) 1 calc R U P B 1
H58 H 0.3263 0.4214 0.7961 0.100 Uiso 0.71(2) 1 calc R U P B 1
C248 C 0.408(2) 0.333(3) 0.7163(12) 0.116(14) Uani 0.29(2) 1 d D U P B 2
H51B H 0.4462 0.2862 0.7231 0.139 Uiso 0.29(2) 1 calc R U P B 2
H52B H 0.3619 0.3007 0.7137 0.139 Uiso 0.29(2) 1 calc R U P B 2
H53B H 0.4133 0.3662 0.6867 0.139 Uiso 0.29(2) 1 calc R U P B 2
C249 C 0.429(2) 0.333(3) 0.7952(13) 0.111(15) Uani 0.29(2) 1 d D U P B 2
H54B H 0.4772 0.3080 0.7940 0.134 Uiso 0.29(2) 1 calc R U P B 2
H55B H 0.4264 0.3626 0.8260 0.134 Uiso 0.29(2) 1 calc R U P B 2
H56B H 0.3948 0.2803 0.7905 0.134 Uiso 0.29(2) 1 calc R U P B 2
C250 C 0.3499(12) 0.472(2) 0.7395(18) 0.113(14) Uani 0.29(2) 1 d D U P B 2
H57B H 0.3617 0.5106 0.7129 0.135 Uiso 0.29(2) 1 calc R U P B 2
H58B H 0.3080 0.4326 0.7295 0.135 Uiso 0.29(2) 1 calc R U P B 2
H59B H 0.3396 0.5149 0.7649 0.135 Uiso 0.29(2) 1 calc R U P B 2
C221 C 0.7381(3) 0.5315(3) 0.73711(15) 0.0394(10) Uani 1 1 d . . . . .
C222 C 0.8077(3) 0.5534(4) 0.72928(17) 0.0439(11) Uani 1 1 d . . . . .
H59 H 0.8213 0.6189 0.7282 0.053 Uiso 1 1 calc R U . . .
C223 C 0.8577(3) 0.4832(4) 0.72307(18) 0.0462(11) Uani 1 1 d . . . . .
H60 H 0.9041 0.5017 0.7172 0.055 Uiso 1 1 calc R U . . .
C224 C 0.8409(3) 0.3852(4) 0.72537(17) 0.0448(11) Uani 1 1 d . . . . .
C225 C 0.7717(3) 0.3637(3) 0.73368(17) 0.0448(11) Uani 1 1 d . . . . .
H61 H 0.7583 0.2983 0.7356 0.054 Uiso 1 1 calc R U . . .
C226 C 0.7214(3) 0.4348(3) 0.73924(16) 0.0426(11) Uani 1 1 d . . . . .
H62 H 0.6748 0.4165 0.7446 0.051 Uiso 1 1 calc R U . . .
C227 C 0.8943(3) 0.3047(4) 0.7195(2) 0.0534(13) Uani 1 1 d . . . . .
C228 C 0.8680(4) 0.2452(5) 0.6763(3) 0.0723(17) Uani 1 1 d . . . . .
H63 H 0.8208 0.2193 0.6797 0.087 Uiso 1 1 calc R U . . .
H64 H 0.8652 0.2858 0.6483 0.087 Uiso 1 1 calc R U . . .
H65 H 0.9012 0.1922 0.6733 0.087 Uiso 1 1 calc R U . . .
C229 C 0.9679(4) 0.3442(6) 0.7133(4) 0.089(2) Uani 1 1 d . . . . .
H66 H 0.9857 0.3827 0.7408 0.106 Uiso 1 1 calc R U . . .
H67 H 1.0006 0.2907 0.7100 0.106 Uiso 1 1 calc R U . . .
H68 H 0.9646 0.3843 0.6850 0.106 Uiso 1 1 calc R U . . .
C230 C 0.8998(4) 0.2385(5) 0.7628(3) 0.078(2) Uani 1 1 d . . . . .
H69 H 0.9166 0.2755 0.7910 0.094 Uiso 1 1 calc R U . . .
H70 H 0.8529 0.2114 0.7660 0.094 Uiso 1 1 calc R U . . .
H71 H 0.9333 0.1864 0.7589 0.094 Uiso 1 1 calc R U . . .
C231 C 0.7112(2) 0.6647(3) 0.79266(15) 0.0389(10) Uani 1 1 d . . . . .
C232 C 0.7681(3) 0.6338(4) 0.82278(17) 0.0478(11) Uani 1 1 d . . . . .
H72 H 0.7937 0.5789 0.8146 0.057 Uiso 1 1 calc R U . . .
C233 C 0.7897(3) 0.6804(4) 0.86520(18) 0.0509(12) Uani 1 1 d . . . . .
H73 H 0.8290 0.6554 0.8853 0.061 Uiso 1 1 calc R U . . .
C234 C 0.7558(3) 0.7617(4) 0.87893(18) 0.0459(11) Uani 1 1 d . . . . .
C235 C 0.6971(3) 0.7916(4) 0.8491(2) 0.0566(14) Uani 1 1 d . . . . .
H74 H 0.6716 0.8465 0.8575 0.068 Uiso 1 1 calc R U . . .
C236 C 0.6740(3) 0.7439(4) 0.80704(19) 0.0543(13) Uani 1 1 d . . . . .
H75 H 0.6325 0.7655 0.7880 0.065 Uiso 1 1 calc R U . . .
C237 C 0.7829(3) 0.8133(4) 0.92499(19) 0.0585(14) Uani 1 1 d D U . . .
C238 C 0.8594(5) 0.8224(10) 0.9312(4) 0.124(4) Uani 1 1 d . U . . .
H76 H 0.8810 0.7585 0.9313 0.149 Uiso 1 1 calc R U . . .
H77 H 0.8744 0.8604 0.9054 0.149 Uiso 1 1 calc R U . . .
H78 H 0.8746 0.8545 0.9612 0.149 Uiso 1 1 calc R U . . .
C239 C 0.7695(11) 0.7513(13) 0.9657(3) 0.214(9) Uani 1 1 d . U . . .
H79 H 0.7183 0.7402 0.9650 0.257 Uiso 1 1 calc R U . . .
H80 H 0.7939 0.6896 0.9637 0.257 Uiso 1 1 calc R U . . .
H81 H 0.7877 0.7833 0.9952 0.257 Uiso 1 1 calc R U . . .
C240 C 0.7553(9) 0.9120(10) 0.9253(6) 0.232(10) Uani 1 1 d D U . . .
H82 H 0.7032 0.9104 0.9211 0.279 Uiso 1 1 calc R U . . .
H83 H 0.7722 0.9426 0.9553 0.279 Uiso 1 1 calc R U . . .
H84 H 0.7720 0.9485 0.8995 0.279 Uiso 1 1 calc R U . . .


_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 C17 1.221(7) . ?
O2 C27 1.217(6) . ?
O11 C1 1.245(7) . ?
O12 C1 1.295(7) . ?
O12 H3 0.8400 . ?
O31 C31 1.183(11) . ?
O32 C31 1.301(11) . ?
O32 C33 1.434(10) . ?
O41 C41 1.161(12) . ?
O42 C41 1.272(13) . ?
O42 C43 1.475(17) . ?
O51 C51 1.11(2) . ?
O52 C51 1.315(15) . ?
O52 C53 1.54(2) . ?
N1 C17 1.367(7) . ?
N1 C12 1.396(6) . ?
N1 H1 0.8800 . ?
N2 C27 1.351(6) . ?
N2 C16 1.408(6) . ?
N2 H2 0.8800 . ?
C1 C11 1.495(7) . ?
C11 C16 1.398(7) . ?
C11 C12 1.426(7) . ?
C12 C13 1.409(7) . ?
C13 C14 1.375(8) . ?
C13 H4 0.9500 . ?
C14 C15 1.370(8) . ?
C14 H5 0.9500 . ?
C15 C16 1.408(7) . ?
C15 H6 0.9500 . ?
C17 C18 1.564(7) . ?
C18 C111 1.540(7) . ?
C18 C131 1.546(7) . ?
C18 C121 1.549(7) . ?
C27 C28 1.565(7) . ?
C28 C221 1.539(7) . ?
C28 C211 1.553(7) . ?
C28 C231 1.569(6) . ?
C31 C32 1.472(10) . ?
C32 H85 0.9800 . ?
C32 H86 0.9800 . ?
C32 H87 0.9800 . ?
C33 C34 1.478(17) . ?
C33 H88 0.9900 . ?
C33 H89 0.9900 . ?
C34 H90 0.9800 . ?
C34 H91 0.9800 . ?
C34 H92 0.9800 . ?
C41 C42 1.486(16) . ?
C42 H93 0.9800 . ?
C42 H94 0.9800 . ?
C42 H95 0.9800 . ?
C43 C44 1.453(14) . ?
C43 H96 0.9900 . ?
C43 H97 0.9900 . ?
C44 H98 0.9800 . ?
C44 H99 0.9800 . ?
C44 H100 0.9800 . ?
C51 C52 1.493(19) . ?
C52 H101 0.9800 . ?
C52 H102 0.9800 . ?
C52 H103 0.9800 . ?
C53 C54 1.58(3) . ?
C53 H104 0.9900 . ?
C53 H105 0.9900 . ?
C54 H106 0.9800 . ?
C54 H107 0.9800 . ?
C54 H108 0.9800 . ?
C111 C116 1.393(7) . ?
C111 C112 1.404(7) . ?
C112 C113 1.391(7) . ?
C112 H7 0.9500 . ?
C113 C114 1.387(7) . ?
C113 H8 0.9500 . ?
C114 C115 1.396(7) . ?
C114 C117 1.533(7) . ?
C115 C116 1.391(7) . ?
C115 H9 0.9500 . ?
C116 H10 0.9500 . ?
C117 C150 1.495(17) . ?
C117 C118 1.497(11) . ?
C117 C120 1.536(10) . ?
C117 C119 1.537(11) . ?
C117 C149 1.556(19) . ?
C117 C148 1.560(18) . ?
C118 H11 0.9800 . ?
C118 H12 0.9800 . ?
C118 H13 0.9800 . ?
C119 H14 0.9800 . ?
C119 H15 0.9800 . ?
C119 H16 0.9800 . ?
C120 H17 0.9800 . ?
C120 H18 0.9800 . ?
C120 H19 0.9800 . ?
C148 H11B 0.9800 . ?
C148 H12B 0.9800 . ?
C148 H13B 0.9800 . ?
C149 H14B 0.9800 . ?
C149 H15B 0.9800 . ?
C149 H16B 0.9800 . ?
C150 H17B 0.9800 . ?
C150 H18B 0.9800 . ?
C150 H19B 0.9800 . ?
C121 C126 1.392(7) . ?
C121 C122 1.394(7) . ?
C122 C123 1.375(8) . ?
C122 H20 0.9500 . ?
C123 C124 1.391(8) . ?
C123 H21 0.9500 . ?
C124 C125 1.389(8) . ?
C124 C127 1.557(8) . ?
C125 C126 1.382(8) . ?
C125 H22 0.9500 . ?
C126 H23 0.9500 . ?
C127 C129 1.452(11) . ?
C127 C128 1.506(12) . ?
C127 C130 1.524(14) . ?
C128 H24 0.9800 . ?
C128 H25 0.9800 . ?
C128 H26 0.9800 . ?
C129 H27 0.9800 . ?
C129 H28 0.9800 . ?
C129 H29 0.9800 . ?
C130 H30 0.9800 . ?
C130 H31 0.9800 . ?
C130 H32 0.9800 . ?
C131 C136 1.390(7) . ?
C131 C132 1.402(7) . ?
C132 C133 1.375(7) . ?
C132 H33 0.9500 . ?
C133 C134 1.381(7) . ?
C133 H34 0.9500 . ?
C134 C135 1.392(8) . ?
C134 C137 1.535(7) . ?
C135 C136 1.374(8) . ?
C135 H35 0.9500 . ?
C136 H36 0.9500 . ?
C137 C138 1.535(8) . ?
C137 C139 1.538(8) . ?
C137 C140 1.544(8) . ?
C138 H37 0.9800 . ?
C138 H38 0.9800 . ?
C138 H39 0.9800 . ?
C139 H40 0.9800 . ?
C139 H41 0.9800 . ?
C139 H42 0.9800 . ?
C140 H43 0.9800 . ?
C140 H44 0.9800 . ?
C140 H45 0.9800 . ?
C211 C212 1.390(7) . ?
C211 C216 1.394(7) . ?
C212 C213 1.397(8) . ?
C212 H46 0.9500 . ?
C213 C214 1.380(8) . ?
C213 H47 0.9500 . ?
C214 C215 1.389(8) . ?
C214 C217 1.550(8) . ?
C215 C216 1.394(7) . ?
C215 H48 0.9500 . ?
C216 H49 0.9500 . ?
C217 C218 1.502(12) . ?
C217 C250 1.51(2) . ?
C217 C219 1.521(14) . ?
C217 C249 1.53(2) . ?
C217 C248 1.55(2) . ?
C217 C220 1.554(11) . ?
C218 H50 0.9800 . ?
C218 H51 0.9800 . ?
C218 H52 0.9800 . ?
C219 H53 0.9800 . ?
C219 H54 0.9800 . ?
C219 H55 0.9800 . ?
C220 H56 0.9800 . ?
C220 H57 0.9800 . ?
C220 H58 0.9800 . ?
C248 H51B 0.9800 . ?
C248 H52B 0.9800 . ?
C248 H53B 0.9800 . ?
C249 H54B 0.9800 . ?
C249 H55B 0.9800 . ?
C249 H56B 0.9800 . ?
C250 H57B 0.9800 . ?
C250 H58B 0.9800 . ?
C250 H59B 0.9800 . ?
C221 C226 1.386(7) . ?
C221 C222 1.399(7) . ?
C222 C223 1.388(7) . ?
C222 H59 0.9500 . ?
C223 C224 1.406(7) . ?
C223 H60 0.9500 . ?
C224 C225 1.392(7) . ?
C224 C227 1.533(7) . ?
C225 C226 1.398(7) . ?
C225 H61 0.9500 . ?
C226 H62 0.9500 . ?
C227 C228 1.521(9) . ?
C227 C229 1.530(9) . ?
C227 C230 1.539(9) . ?
C228 H63 0.9800 . ?
C228 H64 0.9800 . ?
C228 H65 0.9800 . ?
C229 H66 0.9800 . ?
C229 H67 0.9800 . ?
C229 H68 0.9800 . ?
C230 H69 0.9800 . ?
C230 H70 0.9800 . ?
C230 H71 0.9800 . ?
C231 C232 1.366(7) . ?
C231 C236 1.398(7) . ?
C232 C233 1.395(7) . ?
C232 H72 0.9500 . ?
C233 C234 1.383(8) . ?
C233 H73 0.9500 . ?
C234 C235 1.382(8) . ?
C234 C237 1.536(7) . ?
C235 C236 1.400(8) . ?
C235 H74 0.9500 . ?
C236 H75 0.9500 . ?
C237 C238 1.443(11) . ?
C237 C240 1.471(10) . ?
C237 C239 1.500(14) . ?
C238 H76 0.9800 . ?
C238 H77 0.9800 . ?
C238 H78 0.9800 . ?
C239 H79 0.9800 . ?
C239 H80 0.9800 . ?
C239 H81 0.9800 . ?
C240 H82 0.9800 . ?
C240 H83 0.9800 . ?
C240 H84 0.9800 . ?

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 O12 H3 109.5 . . ?
C31 O32 C33 119.2(8) . . ?
C41 O42 C43 109.5(14) . . ?
C51 O52 C53 111.8(12) . . ?
C17 N1 C12 128.1(4) . . ?
C17 N1 H1 115.9 . . ?
C12 N1 H1 115.9 . . ?
C27 N2 C16 126.6(4) . . ?
C27 N2 H2 116.7 . . ?
C16 N2 H2 116.7 . . ?
O11 C1 O12 121.0(5) . . ?
O11 C1 C11 122.1(5) . . ?
O12 C1 C11 116.9(5) . . ?
C16 C11 C12 119.5(4) . . ?
C16 C11 C1 121.2(4) . . ?
C12 C11 C1 119.3(4) . . ?
N1 C12 C13 120.9(4) . . ?
N1 C12 C11 120.0(4) . . ?
C13 C12 C11 119.1(4) . . ?
C14 C13 C12 119.2(5) . . ?
C14 C13 H4 120.4 . . ?
C12 C13 H4 120.4 . . ?
C15 C14 C13 123.1(5) . . ?
C15 C14 H5 118.4 . . ?
C13 C14 H5 118.4 . . ?
C14 C15 C16 118.7(5) . . ?
C14 C15 H6 120.6 . . ?
C16 C15 H6 120.6 . . ?
C11 C16 N2 120.8(4) . . ?
C11 C16 C15 120.4(4) . . ?
N2 C16 C15 118.8(4) . . ?
O1 C17 N1 122.3(5) . . ?
O1 C17 C18 122.0(4) . . ?
N1 C17 C18 115.6(4) . . ?
C111 C18 C131 110.4(4) . . ?
C111 C18 C121 110.4(4) . . ?
C131 C18 C121 109.6(4) . . ?
C111 C18 C17 109.6(4) . . ?
C131 C18 C17 110.3(4) . . ?
C121 C18 C17 106.5(4) . . ?
O2 C27 N2 122.5(5) . . ?
O2 C27 C28 120.9(4) . . ?
N2 C27 C28 116.6(4) . . ?
C221 C28 C211 110.2(4) . . ?
C221 C28 C27 112.5(4) . . ?
C211 C28 C27 105.9(4) . . ?
C221 C28 C231 109.4(4) . . ?
C211 C28 C231 109.6(4) . . ?
C27 C28 C231 109.1(4) . . ?
O31 C31 O32 123.6(8) . . ?
O31 C31 C32 120.7(9) . . ?
O32 C31 C32 115.7(9) . . ?
C31 C32 H85 109.5 . . ?
C31 C32 H86 109.5 . . ?
H85 C32 H86 109.5 . . ?
C31 C32 H87 109.5 . . ?
H85 C32 H87 109.5 . . ?
H86 C32 H87 109.5 . . ?
O32 C33 C34 106.9(10) . . ?
O32 C33 H88 110.3 . . ?
C34 C33 H88 110.3 . . ?
O32 C33 H89 110.3 . . ?
C34 C33 H89 110.3 . . ?
H88 C33 H89 108.6 . . ?
C33 C34 H90 109.5 . . ?
C33 C34 H91 109.5 . . ?
H90 C34 H91 109.5 . . ?
C33 C34 H92 109.5 . . ?
H90 C34 H92 109.5 . . ?
H91 C34 H92 109.5 . . ?
O41 C41 O42 125.1(13) . . ?
O41 C41 C42 123.7(12) . . ?
O42 C41 C42 111.3(10) . . ?
C41 C42 H93 109.5 . . ?
C41 C42 H94 109.5 . . ?
H93 C42 H94 109.5 . . ?
C41 C42 H95 109.5 . . ?
H93 C42 H95 109.5 . . ?
H94 C42 H95 109.5 . . ?
C44 C43 O42 105.8(17) . . ?
C44 C43 H96 110.6 . . ?
O42 C43 H96 110.6 . . ?
C44 C43 H97 110.6 . . ?
O42 C43 H97 110.6 . . ?
H96 C43 H97 108.7 . . ?
C43 C44 H98 109.5 . . ?
C43 C44 H99 109.5 . . ?
H98 C44 H99 109.5 . . ?
C43 C44 H100 109.5 . . ?
H98 C44 H100 109.5 . . ?
H99 C44 H100 109.5 . . ?
O51 C51 O52 117.8(19) . . ?
O51 C51 C52 118.4(19) . . ?
O52 C51 C52 114.7(10) . . ?
C51 C52 H101 109.5 . . ?
C51 C52 H102 109.5 . . ?
H101 C52 H102 109.5 . . ?
C51 C52 H103 109.5 . . ?
H101 C52 H103 109.5 . . ?
H102 C52 H103 109.5 . . ?
O52 C53 C54 96.4(17) . . ?
O52 C53 H104 112.5 . . ?
C54 C53 H104 112.5 . . ?
O52 C53 H105 112.5 . . ?
C54 C53 H105 112.5 . . ?
H104 C53 H105 110.0 . . ?
C53 C54 H106 109.5 . . ?
C53 C54 H107 109.5 . . ?
H106 C54 H107 109.5 . . ?
C53 C54 H108 109.5 . . ?
H106 C54 H108 109.5 . . ?
H107 C54 H108 109.5 . . ?
C116 C111 C112 116.8(4) . . ?
C116 C111 C18 123.3(4) . . ?
C112 C111 C18 119.9(4) . . ?
C113 C112 C111 121.3(5) . . ?
C113 C112 H7 119.4 . . ?
C111 C112 H7 119.4 . . ?
C114 C113 C112 122.4(5) . . ?
C114 C113 H8 118.8 . . ?
C112 C113 H8 118.8 . . ?
C113 C114 C115 115.8(5) . . ?
C113 C114 C117 123.0(5) . . ?
C115 C114 C117 121.2(5) . . ?
C116 C115 C114 122.8(5) . . ?
C116 C115 H9 118.6 . . ?
C114 C115 H9 118.6 . . ?
C115 C116 C111 120.8(5) . . ?
C115 C116 H10 119.6 . . ?
C111 C116 H10 119.6 . . ?
C150 C117 C114 115.0(11) . . ?
C118 C117 C114 113.2(6) . . ?
C118 C117 C120 110.3(9) . . ?
C114 C117 C120 108.6(6) . . ?
C118 C117 C119 108.8(10) . . ?
C114 C117 C119 109.0(6) . . ?
C120 C117 C119 106.8(9) . . ?
C150 C117 C149 111.2(19) . . ?
C114 C117 C149 107.3(10) . . ?
C150 C117 C148 113.5(19) . . ?
C114 C117 C148 108.3(12) . . ?
C149 C117 C148 100(2) . . ?
C117 C118 H11 109.5 . . ?
C117 C118 H12 109.5 . . ?
H11 C118 H12 109.5 . . ?
C117 C118 H13 109.5 . . ?
H11 C118 H13 109.5 . . ?
H12 C118 H13 109.5 . . ?
C117 C119 H14 109.5 . . ?
C117 C119 H15 109.5 . . ?
H14 C119 H15 109.5 . . ?
C117 C119 H16 109.5 . . ?
H14 C119 H16 109.5 . . ?
H15 C119 H16 109.5 . . ?
C117 C120 H17 109.5 . . ?
C117 C120 H18 109.5 . . ?
H17 C120 H18 109.5 . . ?
C117 C120 H19 109.5 . . ?
H17 C120 H19 109.5 . . ?
H18 C120 H19 109.5 . . ?
C117 C148 H11B 109.5 . . ?
C117 C148 H12B 109.5 . . ?
H11B C148 H12B 109.5 . . ?
C117 C148 H13B 109.5 . . ?
H11B C148 H13B 109.5 . . ?
H12B C148 H13B 109.5 . . ?
C117 C149 H14B 109.5 . . ?
C117 C149 H15B 109.5 . . ?
H14B C149 H15B 109.5 . . ?
C117 C149 H16B 109.5 . . ?
H14B C149 H16B 109.5 . . ?
H15B C149 H16B 109.5 . . ?
C117 C150 H17B 109.5 . . ?
C117 C150 H18B 109.5 . . ?
H17B C150 H18B 109.5 . . ?
C117 C150 H19B 109.5 . . ?
H17B C150 H19B 109.5 . . ?
H18B C150 H19B 109.5 . . ?
C126 C121 C122 116.0(5) . . ?
C126 C121 C18 122.7(4) . . ?
C122 C121 C18 121.2(4) . . ?
C123 C122 C121 121.6(5) . . ?
C123 C122 H20 119.2 . . ?
C121 C122 H20 119.2 . . ?
C122 C123 C124 122.5(5) . . ?
C122 C123 H21 118.7 . . ?
C124 C123 H21 118.7 . . ?
C125 C124 C123 115.8(5) . . ?
C125 C124 C127 123.3(5) . . ?
C123 C124 C127 120.8(5) . . ?
C126 C125 C124 121.9(5) . . ?
C126 C125 H22 119.0 . . ?
C124 C125 H22 119.0 . . ?
C125 C126 C121 122.0(5) . . ?
C125 C126 H23 119.0 . . ?
C121 C126 H23 119.0 . . ?
C129 C127 C128 106.8(10) . . ?
C129 C127 C130 112.9(12) . . ?
C128 C127 C130 104.6(11) . . ?
C129 C127 C124 109.9(6) . . ?
C128 C127 C124 111.0(5) . . ?
C130 C127 C124 111.4(6) . . ?
C127 C128 H24 109.5 . . ?
C127 C128 H25 109.5 . . ?
H24 C128 H25 109.5 . . ?
C127 C128 H26 109.5 . . ?
H24 C128 H26 109.5 . . ?
H25 C128 H26 109.5 . . ?
C127 C129 H27 109.5 . . ?
C127 C129 H28 109.5 . . ?
H27 C129 H28 109.5 . . ?
C127 C129 H29 109.5 . . ?
H27 C129 H29 109.5 . . ?
H28 C129 H29 109.5 . . ?
C127 C130 H30 109.5 . . ?
C127 C130 H31 109.5 . . ?
H30 C130 H31 109.5 . . ?
C127 C130 H32 109.5 . . ?
H30 C130 H32 109.5 . . ?
H31 C130 H32 109.5 . . ?
C136 C131 C132 115.2(4) . . ?
C136 C131 C18 123.4(4) . . ?
C132 C131 C18 121.2(4) . . ?
C133 C132 C131 122.0(5) . . ?
C133 C132 H33 119.0 . . ?
C131 C132 H33 119.0 . . ?
C132 C133 C134 122.8(5) . . ?
C132 C133 H34 118.6 . . ?
C134 C133 H34 118.6 . . ?
C133 C134 C135 115.0(5) . . ?
C133 C134 C137 122.7(5) . . ?
C135 C134 C137 122.3(5) . . ?
C136 C135 C134 123.0(5) . . ?
C136 C135 H35 118.5 . . ?
C134 C135 H35 118.5 . . ?
C135 C136 C131 121.9(5) . . ?
C135 C136 H36 119.0 . . ?
C131 C136 H36 119.0 . . ?
C138 C137 C134 111.6(4) . . ?
C138 C137 C139 109.2(5) . . ?
C134 C137 C139 108.8(4) . . ?
C138 C137 C140 107.7(5) . . ?
C134 C137 C140 110.6(4) . . ?
C139 C137 C140 108.9(5) . . ?
C137 C138 H37 109.5 . . ?
C137 C138 H38 109.5 . . ?
H37 C138 H38 109.5 . . ?
C137 C138 H39 109.5 . . ?
H37 C138 H39 109.5 . . ?
H38 C138 H39 109.5 . . ?
C137 C139 H40 109.5 . . ?
C137 C139 H41 109.5 . . ?
H40 C139 H41 109.5 . . ?
C137 C139 H42 109.5 . . ?
H40 C139 H42 109.5 . . ?
H41 C139 H42 109.5 . . ?
C137 C140 H43 109.5 . . ?
C137 C140 H44 109.5 . . ?
H43 C140 H44 109.5 . . ?
C137 C140 H45 109.5 . . ?
H43 C140 H45 109.5 . . ?
H44 C140 H45 109.5 . . ?
C212 C211 C216 117.4(4) . . ?
C212 C211 C28 121.4(4) . . ?
C216 C211 C28 121.0(4) . . ?
C211 C212 C213 120.5(5) . . ?
C211 C212 H46 119.7 . . ?
C213 C212 H46 119.7 . . ?
C214 C213 C212 122.4(5) . . ?
C214 C213 H47 118.8 . . ?
C212 C213 H47 118.8 . . ?
C213 C214 C215 116.9(5) . . ?
C213 C214 C217 122.7(5) . . ?
C215 C214 C217 120.3(5) . . ?
C214 C215 C216 121.4(5) . . ?
C214 C215 H48 119.3 . . ?
C216 C215 H48 119.3 . . ?
C215 C216 C211 121.3(5) . . ?
C215 C216 H49 119.4 . . ?
C211 C216 H49 119.4 . . ?
C218 C217 C219 112.5(13) . . ?
C250 C217 C249 137(2) . . ?
C250 C217 C248 101(3) . . ?
C249 C217 C248 94(2) . . ?
C218 C217 C214 113.4(7) . . ?
C250 C217 C214 107.3(13) . . ?
C219 C217 C214 111.6(7) . . ?
C249 C217 C214 107.3(15) . . ?
C248 C217 C214 105.8(11) . . ?
C218 C217 C220 103.2(10) . . ?
C219 C217 C220 107.3(12) . . ?
C214 C217 C220 108.2(6) . . ?
C217 C218 H50 109.5 . . ?
C217 C218 H51 109.5 . . ?
H50 C218 H51 109.5 . . ?
C217 C218 H52 109.5 . . ?
H50 C218 H52 109.5 . . ?
H51 C218 H52 109.5 . . ?
C217 C219 H53 109.5 . . ?
C217 C219 H54 109.5 . . ?
H53 C219 H54 109.5 . . ?
C217 C219 H55 109.5 . . ?
H53 C219 H55 109.5 . . ?
H54 C219 H55 109.5 . . ?
C217 C220 H56 109.5 . . ?
C217 C220 H57 109.5 . . ?
H56 C220 H57 109.5 . . ?
C217 C220 H58 109.5 . . ?
H56 C220 H58 109.5 . . ?
H57 C220 H58 109.5 . . ?
C217 C248 H51B 109.5 . . ?
C217 C248 H52B 109.5 . . ?
H51B C248 H52B 109.5 . . ?
C217 C248 H53B 109.5 . . ?
H51B C248 H53B 109.5 . . ?
H52B C248 H53B 109.5 . . ?
C217 C249 H54B 109.5 . . ?
C217 C249 H55B 109.5 . . ?
H54B C249 H55B 109.5 . . ?
C217 C249 H56B 109.5 . . ?
H54B C249 H56B 109.5 . . ?
H55B C249 H56B 109.5 . . ?
C217 C250 H57B 109.5 . . ?
C217 C250 H58B 109.5 . . ?
H57B C250 H58B 109.5 . . ?
C217 C250 H59B 109.5 . . ?
H57B C250 H59B 109.5 . . ?
H58B C250 H59B 109.5 . . ?
C226 C221 C222 116.3(4) . . ?
C226 C221 C28 122.5(4) . . ?
C222 C221 C28 121.1(4) . . ?
C223 C222 C221 122.6(4) . . ?
C223 C222 H59 118.7 . . ?
C221 C222 H59 118.7 . . ?
C222 C223 C224 121.0(5) . . ?
C222 C223 H60 119.5 . . ?
C224 C223 H60 119.5 . . ?
C225 C224 C223 116.2(4) . . ?
C225 C224 C227 120.6(5) . . ?
C223 C224 C227 123.2(5) . . ?
C224 C225 C226 122.4(4) . . ?
C224 C225 H61 118.8 . . ?
C226 C225 H61 118.8 . . ?
C221 C226 C225 121.5(5) . . ?
C221 C226 H62 119.3 . . ?
C225 C226 H62 119.3 . . ?
C228 C227 C229 108.3(6) . . ?
C228 C227 C224 109.4(5) . . ?
C229 C227 C224 111.9(5) . . ?
C228 C227 C230 108.2(6) . . ?
C229 C227 C230 109.6(6) . . ?
C224 C227 C230 109.3(5) . . ?
C227 C228 H63 109.5 . . ?
C227 C228 H64 109.5 . . ?
H63 C228 H64 109.5 . . ?
C227 C228 H65 109.5 . . ?
H63 C228 H65 109.5 . . ?
H64 C228 H65 109.5 . . ?
C227 C229 H66 109.5 . . ?
C227 C229 H67 109.5 . . ?
H66 C229 H67 109.5 . . ?
C227 C229 H68 109.5 . . ?
H66 C229 H68 109.5 . . ?
H67 C229 H68 109.5 . . ?
C227 C230 H69 109.5 . . ?
C227 C230 H70 109.5 . . ?
H69 C230 H70 109.5 . . ?
C227 C230 H71 109.5 . . ?
H69 C230 H71 109.5 . . ?
H70 C230 H71 109.5 . . ?
C232 C231 C236 116.7(4) . . ?
C232 C231 C28 122.6(4) . . ?
C236 C231 C28 120.6(4) . . ?
C231 C232 C233 122.0(5) . . ?
C231 C232 H72 119.0 . . ?
C233 C232 H72 119.0 . . ?
C234 C233 C232 122.1(5) . . ?
C234 C233 H73 118.9 . . ?
C232 C233 H73 118.9 . . ?
C235 C234 C233 116.0(5) . . ?
C235 C234 C237 123.4(5) . . ?
C233 C234 C237 120.6(5) . . ?
C234 C235 C236 122.2(5) . . ?
C234 C235 H74 118.9 . . ?
C236 C235 H74 118.9 . . ?
C231 C236 C235 120.8(5) . . ?
C231 C236 H75 119.6 . . ?
C235 C236 H75 119.6 . . ?
C238 C237 C240 105.7(10) . . ?
C238 C237 C239 102.5(10) . . ?
C240 C237 C239 116.1(13) . . ?
C238 C237 C234 112.0(5) . . ?
C240 C237 C234 111.1(6) . . ?
C239 C237 C234 109.2(6) . . ?
C237 C238 H76 109.5 . . ?
C237 C238 H77 109.5 . . ?
H76 C238 H77 109.5 . . ?
C237 C238 H78 109.5 . . ?
H76 C238 H78 109.5 . . ?
H77 C238 H78 109.5 . . ?
C237 C239 H79 109.5 . . ?
C237 C239 H80 109.5 . . ?
H79 C239 H80 109.5 . . ?
C237 C239 H81 109.5 . . ?
H79 C239 H81 109.5 . . ?
H80 C239 H81 109.5 . . ?
C237 C240 H82 109.5 . . ?
C237 C240 H83 109.5 . . ?
H82 C240 H83 109.5 . . ?
C237 C240 H84 109.5 . . ?
H82 C240 H84 109.5 . . ?
H83 C240 H84 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
O11 C1 C11 C16 149.2(6) . . . . ?
O12 C1 C11 C16 -29.2(8) . . . . ?
O11 C1 C11 C12 -28.7(8) . . . . ?
O12 C1 C11 C12 152.9(5) . . . . ?
C17 N1 C12 C13 20.3(8) . . . . ?
C17 N1 C12 C11 -160.1(5) . . . . ?
C16 C11 C12 N1 -177.7(5) . . . . ?
C1 C11 C12 N1 0.2(7) . . . . ?
C16 C11 C12 C13 1.9(8) . . . . ?
C1 C11 C12 C13 179.9(5) . . . . ?
N1 C12 C13 C14 177.5(5) . . . . ?
C11 C12 C13 C14 -2.2(9) . . . . ?
C12 C13 C14 C15 1.3(10) . . . . ?
C13 C14 C15 C16 -0.1(10) . . . . ?
C12 C11 C16 N2 -178.7(5) . . . . ?
C1 C11 C16 N2 3.5(8) . . . . ?
C12 C11 C16 C15 -0.8(8) . . . . ?
C1 C11 C16 C15 -178.7(5) . . . . ?
C27 N2 C16 C11 -151.0(5) . . . . ?
C27 N2 C16 C15 31.1(8) . . . . ?
C14 C15 C16 C11 -0.1(8) . . . . ?
C14 C15 C16 N2 177.8(5) . . . . ?
C12 N1 C17 O1 3.5(9) . . . . ?
C12 N1 C17 C18 179.7(5) . . . . ?
O1 C17 C18 C111 -164.4(6) . . . . ?
N1 C17 C18 C111 19.4(6) . . . . ?
O1 C17 C18 C131 -42.7(7) . . . . ?
N1 C17 C18 C131 141.1(5) . . . . ?
O1 C17 C18 C121 76.2(7) . . . . ?
N1 C17 C18 C121 -100.1(5) . . . . ?
C16 N2 C27 O2 7.6(9) . . . . ?
C16 N2 C27 C28 -174.7(5) . . . . ?
O2 C27 C28 C221 -172.0(5) . . . . ?
N2 C27 C28 C221 10.3(6) . . . . ?
O2 C27 C28 C211 67.6(6) . . . . ?
N2 C27 C28 C211 -110.1(5) . . . . ?
O2 C27 C28 C231 -50.4(6) . . . . ?
N2 C27 C28 C231 131.9(5) . . . . ?
C33 O32 C31 O31 -3.6(14) . . . . ?
C33 O32 C31 C32 178.1(8) . . . . ?
C31 O32 C33 C34 -172.5(9) . . . . ?
C43 O42 C41 O41 9.4(19) . . . . ?
C43 O42 C41 C42 -170.3(14) . . . . ?
C41 O42 C43 C44 -144(2) . . . . ?
C53 O52 C51 O51 -43(3) . . . . ?
C53 O52 C51 C52 170.7(11) . . . . ?
C51 O52 C53 C54 166.2(10) . . . . ?
C131 C18 C111 C116 118.4(5) . . . . ?
C121 C18 C111 C116 -2.9(6) . . . . ?
C17 C18 C111 C116 -120.0(5) . . . . ?
C131 C18 C111 C112 -61.8(5) . . . . ?
C121 C18 C111 C112 176.9(4) . . . . ?
C17 C18 C111 C112 59.9(6) . . . . ?
C116 C111 C112 C113 1.3(7) . . . . ?
C18 C111 C112 C113 -178.5(4) . . . . ?
C111 C112 C113 C114 -1.4(7) . . . . ?
C112 C113 C114 C115 0.1(7) . . . . ?
C112 C113 C114 C117 179.8(5) . . . . ?
C113 C114 C115 C116 1.4(7) . . . . ?
C117 C114 C115 C116 -178.4(4) . . . . ?
C114 C115 C116 C111 -1.5(7) . . . . ?
C112 C111 C116 C115 0.1(7) . . . . ?
C18 C111 C116 C115 179.9(4) . . . . ?
C113 C114 C117 C150 -173(2) . . . . ?
C115 C114 C117 C150 7(2) . . . . ?
C113 C114 C117 C118 -3.3(11) . . . . ?
C115 C114 C117 C118 176.5(9) . . . . ?
C113 C114 C117 C120 -126.0(8) . . . . ?
C115 C114 C117 C120 53.7(9) . . . . ?
C113 C114 C117 C119 118.0(8) . . . . ?
C115 C114 C117 C119 -62.3(8) . . . . ?
C113 C114 C117 C149 62.6(16) . . . . ?
C115 C114 C117 C149 -117.7(15) . . . . ?
C113 C114 C117 C148 -45(2) . . . . ?
C115 C114 C117 C148 134.8(19) . . . . ?
C111 C18 C121 C126 -83.6(6) . . . . ?
C131 C18 C121 C126 154.6(5) . . . . ?
C17 C18 C121 C126 35.3(6) . . . . ?
C111 C18 C121 C122 91.9(5) . . . . ?
C131 C18 C121 C122 -29.9(6) . . . . ?
C17 C18 C121 C122 -149.1(5) . . . . ?
C126 C121 C122 C123 2.4(8) . . . . ?
C18 C121 C122 C123 -173.4(5) . . . . ?
C121 C122 C123 C124 -0.1(8) . . . . ?
C122 C123 C124 C125 -2.3(8) . . . . ?
C122 C123 C124 C127 179.8(5) . . . . ?
C123 C124 C125 C126 2.3(9) . . . . ?
C127 C124 C125 C126 -179.9(6) . . . . ?
C124 C125 C126 C121 0.0(10) . . . . ?
C122 C121 C126 C125 -2.4(9) . . . . ?
C18 C121 C126 C125 173.3(5) . . . . ?
C125 C124 C127 C129 -105.5(10) . . . . ?
C123 C124 C127 C129 72.1(11) . . . . ?
C125 C124 C127 C128 136.5(9) . . . . ?
C123 C124 C127 C128 -45.8(10) . . . . ?
C125 C124 C127 C130 20.4(12) . . . . ?
C123 C124 C127 C130 -161.9(11) . . . . ?
C111 C18 C131 C136 169.1(5) . . . . ?
C121 C18 C131 C136 -69.2(6) . . . . ?
C17 C18 C131 C136 47.8(7) . . . . ?
C111 C18 C131 C132 -17.3(6) . . . . ?
C121 C18 C131 C132 104.5(5) . . . . ?
C17 C18 C131 C132 -138.6(5) . . . . ?
C136 C131 C132 C133 -3.3(8) . . . . ?
C18 C131 C132 C133 -177.4(5) . . . . ?
C131 C132 C133 C134 0.5(9) . . . . ?
C132 C133 C134 C135 2.9(9) . . . . ?
C132 C133 C134 C137 -179.7(5) . . . . ?
C133 C134 C135 C136 -3.6(10) . . . . ?
C137 C134 C135 C136 179.0(6) . . . . ?
C134 C135 C136 C131 0.9(11) . . . . ?
C132 C131 C136 C135 2.6(9) . . . . ?
C18 C131 C136 C135 176.6(6) . . . . ?
C133 C134 C137 C138 25.8(7) . . . . ?
C135 C134 C137 C138 -157.0(6) . . . . ?
C133 C134 C137 C139 -94.8(6) . . . . ?
C135 C134 C137 C139 82.4(7) . . . . ?
C133 C134 C137 C140 145.7(6) . . . . ?
C135 C134 C137 C140 -37.1(7) . . . . ?
C221 C28 C211 C212 -85.2(5) . . . . ?
C27 C28 C211 C212 36.7(6) . . . . ?
C231 C28 C211 C212 154.4(4) . . . . ?
C221 C28 C211 C216 89.2(5) . . . . ?
C27 C28 C211 C216 -148.9(4) . . . . ?
C231 C28 C211 C216 -31.3(6) . . . . ?
C216 C211 C212 C213 -2.6(7) . . . . ?
C28 C211 C212 C213 172.0(5) . . . . ?
C211 C212 C213 C214 0.5(9) . . . . ?
C212 C213 C214 C215 1.2(8) . . . . ?
C212 C213 C214 C217 -178.1(5) . . . . ?
C213 C214 C215 C216 -0.7(8) . . . . ?
C217 C214 C215 C216 178.6(5) . . . . ?
C214 C215 C216 C211 -1.5(8) . . . . ?
C212 C211 C216 C215 3.1(7) . . . . ?
C28 C211 C216 C215 -171.5(5) . . . . ?
C213 C214 C217 C218 -12.6(13) . . . . ?
C215 C214 C217 C218 168.1(11) . . . . ?
C213 C214 C217 C250 -62(2) . . . . ?
C215 C214 C217 C250 119(2) . . . . ?
C213 C214 C217 C219 115.6(13) . . . . ?
C215 C214 C217 C219 -63.6(13) . . . . ?
C213 C214 C217 C249 144(2) . . . . ?
C215 C214 C217 C249 -35(2) . . . . ?
C213 C214 C217 C248 45(2) . . . . ?
C215 C214 C217 C248 -135(2) . . . . ?
C213 C214 C217 C220 -126.5(8) . . . . ?
C215 C214 C217 C220 54.2(8) . . . . ?
C211 C28 C221 C226 -8.8(6) . . . . ?
C27 C28 C221 C226 -126.7(5) . . . . ?
C231 C28 C221 C226 111.8(5) . . . . ?
C211 C28 C221 C222 174.8(4) . . . . ?
C27 C28 C221 C222 56.8(6) . . . . ?
C231 C28 C221 C222 -64.7(5) . . . . ?
C226 C221 C222 C223 1.1(7) . . . . ?
C28 C221 C222 C223 177.8(4) . . . . ?
C221 C222 C223 C224 -1.3(7) . . . . ?
C222 C223 C224 C225 0.6(7) . . . . ?
C222 C223 C224 C227 -179.1(5) . . . . ?
C223 C224 C225 C226 0.3(7) . . . . ?
C227 C224 C225 C226 -180.0(5) . . . . ?
C222 C221 C226 C225 -0.2(6) . . . . ?
C28 C221 C226 C225 -176.8(4) . . . . ?
C224 C225 C226 C221 -0.5(7) . . . . ?
C225 C224 C227 C228 63.0(7) . . . . ?
C223 C224 C227 C228 -117.3(6) . . . . ?
C225 C224 C227 C229 -177.0(6) . . . . ?
C223 C224 C227 C229 2.7(8) . . . . ?
C225 C224 C227 C230 -55.4(7) . . . . ?
C223 C224 C227 C230 124.3(6) . . . . ?
C221 C28 C231 C232 -7.5(6) . . . . ?
C211 C28 C231 C232 113.4(5) . . . . ?
C27 C28 C231 C232 -131.0(5) . . . . ?
C221 C28 C231 C236 176.5(5) . . . . ?
C211 C28 C231 C236 -62.6(6) . . . . ?
C27 C28 C231 C236 53.1(6) . . . . ?
C236 C231 C232 C233 -2.0(8) . . . . ?
C28 C231 C232 C233 -178.1(5) . . . . ?
C231 C232 C233 C234 -1.3(9) . . . . ?
C232 C233 C234 C235 2.9(8) . . . . ?
C232 C233 C234 C237 -177.6(5) . . . . ?
C233 C234 C235 C236 -1.2(9) . . . . ?
C237 C234 C235 C236 179.2(6) . . . . ?
C232 C231 C236 C235 3.5(8) . . . . ?
C28 C231 C236 C235 179.7(5) . . . . ?
C234 C235 C236 C231 -2.0(10) . . . . ?
C235 C234 C237 C238 -136.8(8) . . . . ?
C233 C234 C237 C238 43.7(10) . . . . ?
C235 C234 C237 C240 -18.9(13) . . . . ?
C233 C234 C237 C240 161.6(11) . . . . ?
C235 C234 C237 C239 110.4(11) . . . . ?
C233 C234 C237 C239 -69.1(11) . . . . ?

_refine_diff_density_max         0.674
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.066

_shelxl_version_number           2014/6
####################################################################### 
# 
# 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/access/V1 
# 
# Audit and citation data items may have 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_(NMe4)[L1]-2H2O-1,4-dioxane
_database_code_depnum_ccdc_archive 'CCDC 1042060'
_audit_update_record             
;
2015-01-05 deposited with the CCDC.
2015-03-18 downloaded from the CCDC.
;
_audit_creation_date             2014-09-04
_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        
; 
(NMe4)[OCOC6H3{NHCOC(C6H4-t-Bu)3}(NHCO-n-Bu)]-2(H2O)-dioxane
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H77 N3 O8'
_chemical_formula_sum            'C52 H77 N3 O8'
_chemical_formula_weight         872.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.5622(9)
_cell_length_b                   11.6068(8)
_cell_length_c                   19.7688(14)
_cell_angle_alpha                92.302(6)
_cell_angle_beta                 105.780(7)
_cell_angle_gamma                100.231(7)
_cell_volume                     2501.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    200
_cell_measurement_reflns_used    6274
_cell_measurement_theta_min      3.11
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_F_000             948
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.077
_shelx_estimated_absorpt_T_min   0.981
_shelx_estimated_absorpt_T_max   0.992
_exptl_absorpt_correction_type   none
_diffrn_ambient_temperature      200
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   
;
 MicroMax-007HF microfocus rotating anode X-ray generator
;
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            19110
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.104
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.973
_reflns_number_total             8785
_reflns_number_gt                5625
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'RAPID AUTO (Rigaku, 2006)'
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2006)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2006)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_refine_special_details          
;The n-Bu group and the dioxane molecule were disordered, which were separated 
into two parts and the occupancies were refined. The disordered dioxane was 
partially separated but C41 and C44 are identical to C41B and C44B, 
respectively, which were constrained by EXYZ and EADP. DFIX, SADI, ISOR, and
DELU instructions were uesed for these disordered structures. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0948P)²+1.4048P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8785
_refine_ls_number_parameters     639
_refine_ls_number_restraints     97
_refine_ls_R_factor_all          0.1177
_refine_ls_R_factor_gt           0.0741
_refine_ls_wR_factor_ref         0.2071
_refine_ls_wR_factor_gt          0.1812
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1714(3) 0.6333(3) 0.87373(17) 0.0547(9) Uani 1 1 d . . . . .
C11 C 0.0920(3) 0.7227(2) 0.87857(15) 0.0416(7) Uani 1 1 d . . . . .
C12 C 0.0251(3) 0.7664(2) 0.81772(14) 0.0354(6) Uani 1 1 d . . . . .
C13 C -0.0423(3) 0.8538(3) 0.82296(16) 0.0482(8) Uani 1 1 d . . . . .
H3 H -0.0866 0.8833 0.7817 0.058 Uiso 1 1 calc R U . . .
C14 C -0.0433(3) 0.8963(3) 0.88892(17) 0.0569(9) Uani 1 1 d . . . . .
H4 H -0.0879 0.9565 0.8924 0.068 Uiso 1 1 calc R U . . .
C15 C 0.0179(3) 0.8548(3) 0.94942(17) 0.0562(9) Uani 1 1 d . . . . .
H5 H 0.0147 0.8851 0.9941 0.067 Uiso 1 1 calc R U . . .
C16 C 0.0846(3) 0.7683(3) 0.94499(15) 0.0496(8) Uani 1 1 d . . . . .
C17 C -0.0154(3) 0.7593(2) 0.68695(14) 0.0346(6) Uani 1 1 d . . . . .
C18 C -0.0015(2) 0.6821(2) 0.62364(13) 0.0300(6) Uani 1 1 d . . . . .
C21 C 0.1586(9) 0.5609(9) 1.1463(6) 0.097(3) Uani 0.570(11) 1 d D U P A 1
H47 H 0.0962 0.5117 1.1063 0.117 Uiso 0.570(11) 1 calc R U P A 1
H48 H 0.1150 0.5954 1.1762 0.117 Uiso 0.570(11) 1 calc R U P A 1
C22 C 0.2417(12) 0.4802(9) 1.1912(6) 0.097(3) Uani 0.570(11) 1 d D U P A 1
H49 H 0.3131 0.5314 1.2253 0.117 Uiso 0.570(11) 1 calc R U P A 1
H50 H 0.1940 0.4327 1.2186 0.117 Uiso 0.570(11) 1 calc R U P A 1
C23 C 0.2870(14) 0.4000(11) 1.1489(6) 0.117(4) Uani 0.570(11) 1 d D U P A 1
H51 H 0.3373 0.3535 1.1804 0.140 Uiso 0.570(11) 1 calc R U P A 1
H52 H 0.2171 0.3473 1.1158 0.140 Uiso 0.570(11) 1 calc R U P A 1
H53 H 0.3364 0.4461 1.1225 0.140 Uiso 0.570(11) 1 calc R U P A 1
C28 C 0.2322(12) 0.6606(11) 1.1175(6) 0.093(5) Uani 0.570(11) 1 d D U P A 1
H45 H 0.2772 0.6280 1.0876 0.112 Uiso 0.570(11) 1 calc R U P A 1
H46 H 0.2923 0.7134 1.1568 0.112 Uiso 0.570(11) 1 calc R U P A 1
C21B C 0.1710(14) 0.5299(10) 1.1011(7) 0.104(4) Uani 0.430(11) 1 d D U P A 2
H47B H 0.1993 0.5226 1.0584 0.125 Uiso 0.430(11) 1 calc R U P A 2
H48B H 0.0806 0.5050 1.0859 0.125 Uiso 0.430(11) 1 calc R U P A 2
C22B C 0.2232(17) 0.4426(17) 1.1510(13) 0.139(7) Uani 0.430(11) 1 d D U P A 2
H49B H 0.1774 0.4264 1.1864 0.167 Uiso 0.430(11) 1 calc R U P A 2
H50B H 0.2212 0.3676 1.1247 0.167 Uiso 0.430(11) 1 calc R U P A 2
C23B C 0.3483(18) 0.504(2) 1.1843(12) 0.185(9) Uani 0.430(11) 1 d D U P A 2
H51B H 0.3908 0.4546 1.2179 0.222 Uiso 0.430(11) 1 calc R U P A 2
H52B H 0.3910 0.5197 1.1481 0.222 Uiso 0.430(11) 1 calc R U P A 2
H53B H 0.3475 0.5780 1.2093 0.222 Uiso 0.430(11) 1 calc R U P A 2
C28B C 0.2007(19) 0.6572(13) 1.1276(8) 0.088(6) Uani 0.430(11) 1 d D U P A 2
H45B H 0.2904 0.6857 1.1401 0.106 Uiso 0.430(11) 1 calc R U P A 2
H46B H 0.1744 0.6667 1.1708 0.106 Uiso 0.430(11) 1 calc R U P A 2
C27 C 0.1371(5) 0.7306(4) 1.07217(19) 0.0784(13) Uani 1 1 d D . . . .
C31 C 0.1805(5) 0.3217(4) 0.8472(2) 0.0915(14) Uani 1 1 d . . . . .
H54 H 0.0965 0.3154 0.8505 0.110 Uiso 1 1 calc R U . . .
H55 H 0.2217 0.4045 0.8552 0.110 Uiso 1 1 calc R U . . .
H56 H 0.1784 0.2897 0.8002 0.110 Uiso 1 1 calc R U . . .
C32 C 0.1842(6) 0.1286(4) 0.8866(3) 0.1121(18) Uani 1 1 d . . . . .
H57 H 0.2279 0.0827 0.9220 0.135 Uiso 1 1 calc R U . . .
H58 H 0.0998 0.1218 0.8890 0.135 Uiso 1 1 calc R U . . .
H59 H 0.1836 0.0985 0.8394 0.135 Uiso 1 1 calc R U . . .
C33 C 0.3747(5) 0.2628(6) 0.8973(3) 0.126(2) Uani 1 1 d . . . . .
H60 H 0.4179 0.2179 0.9334 0.151 Uiso 1 1 calc R U . . .
H61 H 0.3736 0.2305 0.8505 0.151 Uiso 1 1 calc R U . . .
H62 H 0.4170 0.3454 0.9055 0.151 Uiso 1 1 calc R U . . .
C34 C 0.2466(5) 0.3017(5) 0.9719(2) 0.0949(14) Uani 1 1 d . . . . .
H63 H 0.2912 0.2577 1.0080 0.114 Uiso 1 1 calc R U . . .
H64 H 0.2862 0.3850 0.9806 0.114 Uiso 1 1 calc R U . . .
H65 H 0.1617 0.2933 0.9738 0.114 Uiso 1 1 calc R U . . .
C41 C 0.5773(9) 1.0229(9) 0.8564(4) 0.186(4) Uani 0.459(11) 1 d D U P B 1
H66 H 0.5948 1.1073 0.8489 0.223 Uiso 0.459(11) 1 calc R U P B 1
H67 H 0.6210 0.9822 0.8292 0.223 Uiso 0.459(11) 1 calc R U P B 1
C42 C 0.6348(10) 1.0130(10) 0.9317(6) 0.091(4) Uani 0.459(11) 1 d D U P B 1
H68 H 0.7222 1.0102 0.9382 0.110 Uiso 0.459(11) 1 calc R U P B 1
H69 H 0.6318 1.0849 0.9593 0.110 Uiso 0.459(11) 1 calc R U P B 1
C43 C 0.4529(9) 0.8968(10) 0.9383(5) 0.085(3) Uani 0.459(11) 1 d D U P B 1
H70 H 0.4269 0.9586 0.9634 0.102 Uiso 0.459(11) 1 calc R U P B 1
H71 H 0.4184 0.8198 0.9519 0.102 Uiso 0.459(11) 1 calc R U P B 1
C44 C 0.4035(6) 0.9001(7) 0.8630(3) 0.132(2) Uani 0.459(11) 1 d D U P B 1
H72 H 0.4026 0.8220 0.8406 0.158 Uiso 0.459(11) 1 calc R U P B 1
H73 H 0.3169 0.9076 0.8546 0.158 Uiso 0.459(11) 1 calc R U P B 1
C41B C 0.5773(9) 1.0229(9) 0.8564(4) 0.186(4) Uani 0.541(11) 1 d D U P B 2
H66B H 0.6119 1.0548 0.8189 0.223 Uiso 0.541(11) 1 calc R U P B 2
H67B H 0.5855 1.0903 0.8909 0.223 Uiso 0.541(11) 1 calc R U P B 2
C42B C 0.6491(12) 0.9538(15) 0.8891(11) 0.158(5) Uani 0.541(11) 1 d D U P B 2
H68B H 0.7298 1.0015 0.9158 0.190 Uiso 0.541(11) 1 calc R U P B 2
H69B H 0.6623 0.8979 0.8542 0.190 Uiso 0.541(11) 1 calc R U P B 2
C43B C 0.4792(12) 0.8321(10) 0.8945(8) 0.137(5) Uani 0.541(11) 1 d D U P B 2
H70B H 0.4903 0.7779 0.8579 0.164 Uiso 0.541(11) 1 calc R U P B 2
H71B H 0.4401 0.7835 0.9253 0.164 Uiso 0.541(11) 1 calc R U P B 2
C44B C 0.4035(6) 0.9001(7) 0.8630(3) 0.132(2) Uani 0.541(11) 1 d D U P B 2
H72B H 0.3765 0.9409 0.8992 0.158 Uiso 0.541(11) 1 calc R U P B 2
H73B H 0.3299 0.8499 0.8300 0.158 Uiso 0.541(11) 1 calc R U P B 2
C111 C -0.0414(2) 0.5518(2) 0.63402(13) 0.0294(6) Uani 1 1 d . . . . .
C112 C 0.0277(2) 0.4666(2) 0.63092(14) 0.0326(6) Uani 1 1 d . . . . .
H6 H 0.1064 0.4887 0.6238 0.039 Uiso 1 1 calc R U . . .
C113 C -0.0158(2) 0.3498(2) 0.63804(14) 0.0342(6) Uani 1 1 d . . . . .
H7 H 0.0343 0.2940 0.6357 0.041 Uiso 1 1 calc R U . . .
C114 C -0.1295(2) 0.3115(2) 0.64842(13) 0.0312(6) Uani 1 1 d . . . . .
C115 C -0.1981(3) 0.3977(2) 0.65227(15) 0.0369(6) Uani 1 1 d . . . . .
H8 H -0.2766 0.3757 0.6597 0.044 Uiso 1 1 calc R U . . .
C116 C -0.1552(2) 0.5140(2) 0.64561(15) 0.0363(6) Uani 1 1 d . . . . .
H9 H -0.2046 0.5700 0.6490 0.044 Uiso 1 1 calc R U . . .
C117 C -0.1756(3) 0.1809(2) 0.65405(15) 0.0385(7) Uani 1 1 d . . . . .
C118 C -0.1735(4) 0.1072(3) 0.5895(2) 0.0658(10) Uani 1 1 d . . . . .
H10 H -0.0906 0.1223 0.5840 0.079 Uiso 1 1 calc R U . . .
H11 H -0.1977 0.0237 0.5953 0.079 Uiso 1 1 calc R U . . .
H12 H -0.2309 0.1278 0.5475 0.079 Uiso 1 1 calc R U . . .
C119 C -0.3039(3) 0.1576(3) 0.6626(2) 0.0663(10) Uani 1 1 d . . . . .
H13 H -0.3052 0.2053 0.7044 0.080 Uiso 1 1 calc R U . . .
H14 H -0.3613 0.1782 0.6206 0.080 Uiso 1 1 calc R U . . .
H15 H -0.3281 0.0741 0.6684 0.080 Uiso 1 1 calc R U . . .
C120 C -0.0910(3) 0.1408(3) 0.7198(2) 0.0618(9) Uani 1 1 d . . . . .
H16 H -0.0911 0.1875 0.7621 0.074 Uiso 1 1 calc R U . . .
H17 H -0.1207 0.0575 0.7235 0.074 Uiso 1 1 calc R U . . .
H18 H -0.0074 0.1518 0.7154 0.074 Uiso 1 1 calc R U . . .
C121 C 0.1323(2) 0.7076(2) 0.62038(13) 0.0296(6) Uani 1 1 d . . . . .
C122 C 0.2315(3) 0.7591(3) 0.67588(15) 0.0412(7) Uani 1 1 d . . . . .
H19 H 0.2180 0.7879 0.7182 0.049 Uiso 1 1 calc R U . . .
C123 C 0.3503(3) 0.7698(3) 0.67150(15) 0.0451(7) Uani 1 1 d . . . . .
H20 H 0.4162 0.8061 0.7110 0.054 Uiso 1 1 calc R U . . .
C124 C 0.3766(2) 0.7294(2) 0.61145(15) 0.0361(6) Uani 1 1 d . . . . .
C125 C 0.2758(3) 0.6826(2) 0.55466(15) 0.0388(7) Uani 1 1 d . . . . .
H21 H 0.2891 0.6567 0.5117 0.047 Uiso 1 1 calc R U . . .
C126 C 0.1575(3) 0.6725(2) 0.55853(14) 0.0368(6) Uani 1 1 d . . . . .
H22 H 0.0914 0.6408 0.5181 0.044 Uiso 1 1 calc R U . . .
C127 C 0.5067(3) 0.7352(3) 0.60540(17) 0.0466(7) Uani 1 1 d . . . . .
C128 C 0.6044(3) 0.7897(4) 0.6728(2) 0.0730(11) Uani 1 1 d . . . . .
H23 H 0.5942 0.8696 0.6841 0.088 Uiso 1 1 calc R U . . .
H24 H 0.5963 0.7420 0.7116 0.088 Uiso 1 1 calc R U . . .
H25 H 0.6858 0.7927 0.6660 0.088 Uiso 1 1 calc R U . . .
C129 C 0.5261(3) 0.8100(4) 0.5462(2) 0.0725(11) Uani 1 1 d . . . . .
H26 H 0.4643 0.7772 0.5018 0.087 Uiso 1 1 calc R U . . .
H27 H 0.5183 0.8907 0.5576 0.087 Uiso 1 1 calc R U . . .
H28 H 0.6081 0.8103 0.5411 0.087 Uiso 1 1 calc R U . . .
C130 C 0.5231(3) 0.6112(3) 0.5881(3) 0.0898(15) Uani 1 1 d . . . . .
H29 H 0.4602 0.5757 0.5446 0.108 Uiso 1 1 calc R U . . .
H30 H 0.6045 0.6143 0.5814 0.108 Uiso 1 1 calc R U . . .
H31 H 0.5151 0.5636 0.6270 0.108 Uiso 1 1 calc R U . . .
C131 C -0.0834(2) 0.7170(2) 0.55485(13) 0.0297(6) Uani 1 1 d . . . . .
C132 C -0.0624(2) 0.8325(2) 0.53790(14) 0.0349(6) Uani 1 1 d . . . . .
H32 H 0.0029 0.8881 0.5687 0.042 Uiso 1 1 calc R U . . .
C133 C -0.1334(2) 0.8687(2) 0.47765(14) 0.0353(6) Uani 1 1 d . . . . .
H33 H -0.1168 0.9488 0.4685 0.042 Uiso 1 1 calc R U . . .
C134 C -0.2296(2) 0.7905(2) 0.42953(14) 0.0324(6) Uani 1 1 d . . . . .
C135 C -0.2467(2) 0.6748(2) 0.44538(14) 0.0364(6) Uani 1 1 d . . . . .
H34 H -0.3089 0.6180 0.4134 0.044 Uiso 1 1 calc R U . . .
C136 C -0.1755(2) 0.6390(2) 0.50677(14) 0.0346(6) Uani 1 1 d . . . . .
H35 H -0.1908 0.5587 0.5156 0.041 Uiso 1 1 calc R U . . .
C137 C -0.3087(3) 0.8357(3) 0.36483(15) 0.0392(7) Uani 1 1 d . . . . .
C138 C -0.2295(3) 0.8838(3) 0.31728(17) 0.0581(9) Uani 1 1 d . . . . .
H36 H -0.1617 0.9459 0.3444 0.070 Uiso 1 1 calc R U . . .
H37 H -0.1964 0.8200 0.3000 0.070 Uiso 1 1 calc R U . . .
H38 H -0.2797 0.9161 0.2771 0.070 Uiso 1 1 calc R U . . .
C139 C -0.4130(3) 0.7395(3) 0.32141(17) 0.0556(9) Uani 1 1 d . . . . .
H39 H -0.4613 0.7721 0.2806 0.067 Uiso 1 1 calc R U . . .
H40 H -0.3791 0.6756 0.3051 0.067 Uiso 1 1 calc R U . . .
H41 H -0.4656 0.7091 0.3506 0.067 Uiso 1 1 calc R U . . .
C140 C -0.3620(3) 0.9367(3) 0.38851(17) 0.0495(8) Uani 1 1 d . . . . .
H42 H -0.2951 0.9988 0.4165 0.059 Uiso 1 1 calc R U . . .
H43 H -0.4090 0.9685 0.3469 0.059 Uiso 1 1 calc R U . . .
H44 H -0.4159 0.9075 0.4173 0.059 Uiso 1 1 calc R U . . .
N1 N 0.0242(2) 0.7185(2) 0.75089(12) 0.0374(6) Uani 1 1 d . . . . .
H1 H 0.063(3) 0.659(3) 0.7557(16) 0.045 Uiso 1 1 d . U . . .
N2 N 0.1484(3) 0.7224(3) 1.00595(14) 0.0683(9) Uani 1 1 d . . . . .
H2 H 0.203(4) 0.677(4) 0.998(2) 0.082 Uiso 1 1 d . U . . .
N3 N 0.2476(3) 0.2550(3) 0.90094(17) 0.0753(9) Uani 1 1 d . . . . .
O1 O -0.0575(3) 0.8469(2) 0.67877(11) 0.0676(7) Uani 1 1 d . . . . .
O2 O 0.0738(3) 0.7902(3) 1.09173(14) 0.1016(11) Uani 1 1 d . . . . .
O3 O 0.3480(4) 0.5260(3) 0.7637(2) 0.1188(12) Uani 1 1 d . . . . .
O4 O 0.4660(4) 0.5598(4) 0.9231(4) 0.191(3) Uani 1 1 d . . . . .
O11 O 0.1616(3) 0.5840(2) 0.81478(12) 0.0760(8) Uani 1 1 d . . . . .
O12 O 0.2453(3) 0.6121(3) 0.92854(13) 0.0895(10) Uani 1 1 d . . . . .
O41 O 0.4553(4) 0.9829(4) 0.8262(2) 0.1271(13) Uani 1 1 d . U . . .
O42 O 0.5806(14) 0.9137(14) 0.9597(9) 0.098(4) Uani 0.459(11) 1 d D U P B 1
O42B O 0.5949(15) 0.8923(16) 0.9352(10) 0.149(7) Uani 0.541(11) 1 d D U P B 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
C1 O11 1.245(4) . ?
C1 O12 1.248(4) . ?
C1 C11 1.519(4) . ?
C11 C12 1.409(4) . ?
C11 C16 1.425(4) . ?
C12 C13 1.401(4) . ?
C12 N1 1.409(3) . ?
C13 C14 1.379(4) . ?
C13 H3 0.9500 . ?
C14 C15 1.368(5) . ?
C14 H4 0.9500 . ?
C15 C16 1.384(4) . ?
C15 H5 0.9500 . ?
C16 N2 1.410(4) . ?
C17 O1 1.202(3) . ?
C17 N1 1.357(4) . ?
C17 C18 1.570(3) . ?
C18 C111 1.539(3) . ?
C18 C121 1.543(3) . ?
C18 C131 1.546(4) . ?
C21 C28 1.535(13) . ?
C21 C22 1.584(12) . ?
C21 H47 0.9900 . ?
C21 H48 0.9900 . ?
C22 C23 1.479(13) . ?
C22 H49 0.9900 . ?
C22 H50 0.9900 . ?
C23 H51 0.9800 . ?
C23 H52 0.9800 . ?
C23 H53 0.9800 . ?
C28 C27 1.586(11) . ?
C28 H45 0.9900 . ?
C28 H46 0.9900 . ?
C21B C28B 1.495(15) . ?
C21B C22B 1.530(15) . ?
C21B H47B 0.9900 . ?
C21B H48B 0.9900 . ?
C22B C23B 1.452(17) . ?
C22B H49B 0.9900 . ?
C22B H50B 0.9900 . ?
C23B H51B 0.9800 . ?
C23B H52B 0.9800 . ?
C23B H53B 0.9800 . ?
C28B C27 1.525(12) . ?
C28B H45B 0.9900 . ?
C28B H46B 0.9900 . ?
C27 O2 1.215(5) . ?
C27 N2 1.352(5) . ?
C31 N3 1.470(5) . ?
C31 H54 0.9800 . ?
C31 H55 0.9800 . ?
C31 H56 0.9800 . ?
C32 N3 1.497(6) . ?
C32 H57 0.9800 . ?
C32 H58 0.9800 . ?
C32 H59 0.9800 . ?
C33 N3 1.477(6) . ?
C33 H60 0.9800 . ?
C33 H61 0.9800 . ?
C33 H62 0.9800 . ?
C34 N3 1.487(5) . ?
C34 H63 0.9800 . ?
C34 H64 0.9800 . ?
C34 H65 0.9800 . ?
C41 O41 1.360(9) . ?
C41 C42 1.473(11) . ?
C41 H66 0.9900 . ?
C41 H67 0.9900 . ?
C42 O42 1.419(14) . ?
C42 H68 0.9900 . ?
C42 H69 0.9900 . ?
C43 O42 1.396(15) . ?
C43 C44 1.447(10) . ?
C43 H70 0.9900 . ?
C43 H71 0.9900 . ?
C44 O41 1.379(7) . ?
C44 H72 0.9900 . ?
C44 H73 0.9900 . ?
C41B C42B 1.318(13) . ?
C41B O41 1.360(9) . ?
C41B H66B 0.9900 . ?
C41B H67B 0.9900 . ?
C42B O42B 1.391(15) . ?
C42B H68B 0.9900 . ?
C42B H69B 0.9900 . ?
C43B C44B 1.329(11) . ?
C43B O42B 1.401(15) . ?
C43B H70B 0.9900 . ?
C43B H71B 0.9900 . ?
C44B O41 1.379(7) . ?
C44B H72B 0.9900 . ?
C44B H73B 0.9900 . ?
C111 C112 1.387(3) . ?
C111 C116 1.394(4) . ?
C112 C113 1.387(4) . ?
C112 H6 0.9500 . ?
C113 C114 1.384(4) . ?
C113 H7 0.9500 . ?
C114 C115 1.395(4) . ?
C114 C117 1.533(4) . ?
C115 C116 1.377(4) . ?
C115 H8 0.9500 . ?
C116 H9 0.9500 . ?
C117 C118 1.516(4) . ?
C117 C119 1.517(4) . ?
C117 C120 1.543(4) . ?
C118 H10 0.9800 . ?
C118 H11 0.9800 . ?
C118 H12 0.9800 . ?
C119 H13 0.9800 . ?
C119 H14 0.9800 . ?
C119 H15 0.9800 . ?
C120 H16 0.9800 . ?
C120 H17 0.9800 . ?
C120 H18 0.9800 . ?
C121 C122 1.377(4) . ?
C121 C126 1.394(4) . ?
C122 C123 1.384(4) . ?
C122 H19 0.9500 . ?
C123 C124 1.387(4) . ?
C123 H20 0.9500 . ?
C124 C125 1.388(4) . ?
C124 C127 1.531(4) . ?
C125 C126 1.375(4) . ?
C125 H21 0.9500 . ?
C126 H22 0.9500 . ?
C127 C128 1.520(5) . ?
C127 C130 1.523(5) . ?
C127 C129 1.526(5) . ?
C128 H23 0.9800 . ?
C128 H24 0.9800 . ?
C128 H25 0.9800 . ?
C129 H26 0.9800 . ?
C129 H27 0.9800 . ?
C129 H28 0.9800 . ?
C130 H29 0.9800 . ?
C130 H30 0.9800 . ?
C130 H31 0.9800 . ?
C131 C136 1.376(4) . ?
C131 C132 1.391(4) . ?
C132 C133 1.379(4) . ?
C132 H32 0.9500 . ?
C133 C134 1.401(4) . ?
C133 H33 0.9500 . ?
C134 C135 1.383(4) . ?
C134 C137 1.528(4) . ?
C135 C136 1.394(4) . ?
C135 H34 0.9500 . ?
C136 H35 0.9500 . ?
C137 C139 1.522(4) . ?
C137 C140 1.531(4) . ?
C137 C138 1.537(4) . ?
C138 H36 0.9800 . ?
C138 H37 0.9800 . ?
C138 H38 0.9800 . ?
C139 H39 0.9800 . ?
C139 H40 0.9800 . ?
C139 H41 0.9800 . ?
C140 H42 0.9800 . ?
C140 H43 0.9800 . ?
C140 H44 0.9800 . ?
N1 H1 0.89(3) . ?
N2 H2 0.93(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
O11 C1 O12 121.8(3) . . ?
O11 C1 C11 118.8(3) . . ?
O12 C1 C11 119.4(3) . . ?
C12 C11 C16 117.2(2) . . ?
C12 C11 C1 121.4(2) . . ?
C16 C11 C1 121.4(3) . . ?
C13 C12 C11 121.0(2) . . ?
C13 C12 N1 120.1(2) . . ?
C11 C12 N1 118.9(2) . . ?
C14 C13 C12 119.0(3) . . ?
C14 C13 H3 120.5 . . ?
C12 C13 H3 120.5 . . ?
C15 C14 C13 122.2(3) . . ?
C15 C14 H4 118.9 . . ?
C13 C14 H4 118.9 . . ?
C14 C15 C16 119.4(3) . . ?
C14 C15 H5 120.3 . . ?
C16 C15 H5 120.3 . . ?
C15 C16 N2 121.3(3) . . ?
C15 C16 C11 121.2(3) . . ?
N2 C16 C11 117.5(3) . . ?
O1 C17 N1 123.5(2) . . ?
O1 C17 C18 122.3(2) . . ?
N1 C17 C18 114.3(2) . . ?
C111 C18 C121 110.6(2) . . ?
C111 C18 C131 111.7(2) . . ?
C121 C18 C131 108.23(19) . . ?
C111 C18 C17 108.30(19) . . ?
C121 C18 C17 110.4(2) . . ?
C131 C18 C17 107.58(19) . . ?
C28 C21 C22 112.9(9) . . ?
C28 C21 H47 109.0 . . ?
C22 C21 H47 109.0 . . ?
C28 C21 H48 109.0 . . ?
C22 C21 H48 109.0 . . ?
H47 C21 H48 107.8 . . ?
C23 C22 C21 114.6(10) . . ?
C23 C22 H49 108.6 . . ?
C21 C22 H49 108.6 . . ?
C23 C22 H50 108.6 . . ?
C21 C22 H50 108.6 . . ?
H49 C22 H50 107.6 . . ?
C22 C23 H51 109.5 . . ?
C22 C23 H52 109.5 . . ?
H51 C23 H52 109.5 . . ?
C22 C23 H53 109.5 . . ?
H51 C23 H53 109.5 . . ?
H52 C23 H53 109.5 . . ?
C21 C28 C27 107.1(9) . . ?
C21 C28 H45 110.3 . . ?
C27 C28 H45 110.3 . . ?
C21 C28 H46 110.3 . . ?
C27 C28 H46 110.3 . . ?
H45 C28 H46 108.6 . . ?
C28B C21B C22B 118.3(13) . . ?
C28B C21B H47B 107.7 . . ?
C22B C21B H47B 107.7 . . ?
C28B C21B H48B 107.7 . . ?
C22B C21B H48B 107.7 . . ?
H47B C21B H48B 107.1 . . ?
C23B C22B C21B 102.8(15) . . ?
C23B C22B H49B 111.2 . . ?
C21B C22B H49B 111.2 . . ?
C23B C22B H50B 111.2 . . ?
C21B C22B H50B 111.2 . . ?
H49B C22B H50B 109.1 . . ?
C22B C23B H51B 109.5 . . ?
C22B C23B H52B 109.5 . . ?
H51B C23B H52B 109.5 . . ?
C22B C23B H53B 109.5 . . ?
H51B C23B H53B 109.5 . . ?
H52B C23B H53B 109.5 . . ?
C21B C28B C27 111.3(11) . . ?
C21B C28B H45B 109.4 . . ?
C27 C28B H45B 109.4 . . ?
C21B C28B H46B 109.4 . . ?
C27 C28B H46B 109.4 . . ?
H45B C28B H46B 108.0 . . ?
O2 C27 N2 124.6(4) . . ?
O2 C27 C28B 115.0(7) . . ?
N2 C27 C28B 120.3(7) . . ?
O2 C27 C28 129.0(6) . . ?
N2 C27 C28 106.0(6) . . ?
N3 C31 H54 109.5 . . ?
N3 C31 H55 109.5 . . ?
H54 C31 H55 109.5 . . ?
N3 C31 H56 109.5 . . ?
H54 C31 H56 109.5 . . ?
H55 C31 H56 109.5 . . ?
N3 C32 H57 109.5 . . ?
N3 C32 H58 109.5 . . ?
H57 C32 H58 109.5 . . ?
N3 C32 H59 109.5 . . ?
H57 C32 H59 109.5 . . ?
H58 C32 H59 109.5 . . ?
N3 C33 H60 109.5 . . ?
N3 C33 H61 109.5 . . ?
H60 C33 H61 109.5 . . ?
N3 C33 H62 109.5 . . ?
H60 C33 H62 109.5 . . ?
H61 C33 H62 109.5 . . ?
N3 C34 H63 109.5 . . ?
N3 C34 H64 109.5 . . ?
H63 C34 H64 109.5 . . ?
N3 C34 H65 109.5 . . ?
H63 C34 H65 109.5 . . ?
H64 C34 H65 109.5 . . ?
O41 C41 C42 121.4(7) . . ?
O41 C41 H66 107.0 . . ?
C42 C41 H66 107.0 . . ?
O41 C41 H67 107.0 . . ?
C42 C41 H67 107.0 . . ?
H66 C41 H67 106.7 . . ?
O42 C42 C41 115.1(10) . . ?
O42 C42 H68 108.5 . . ?
C41 C42 H68 108.5 . . ?
O42 C42 H69 108.5 . . ?
C41 C42 H69 108.5 . . ?
H68 C42 H69 107.5 . . ?
O42 C43 C44 112.7(10) . . ?
O42 C43 H70 109.0 . . ?
C44 C43 H70 109.0 . . ?
O42 C43 H71 109.0 . . ?
C44 C43 H71 109.0 . . ?
H70 C43 H71 107.8 . . ?
O41 C44 C43 122.1(6) . . ?
O41 C44 H72 106.8 . . ?
C43 C44 H72 106.8 . . ?
O41 C44 H73 106.8 . . ?
C43 C44 H73 106.8 . . ?
H72 C44 H73 106.7 . . ?
C42B C41B O41 121.7(11) . . ?
C42B C41B H66B 106.9 . . ?
O41 C41B H66B 106.9 . . ?
C42B C41B H67B 106.9 . . ?
O41 C41B H67B 106.9 . . ?
H66B C41B H67B 106.7 . . ?
C41B C42B O42B 109.4(12) . . ?
C41B C42B H68B 109.8 . . ?
O42B C42B H68B 109.8 . . ?
C41B C42B H69B 109.8 . . ?
O42B C42B H69B 109.8 . . ?
H68B C42B H69B 108.2 . . ?
C44B C43B O42B 115.0(11) . . ?
C44B C43B H70B 108.5 . . ?
O42B C43B H70B 108.5 . . ?
C44B C43B H71B 108.5 . . ?
O42B C43B H71B 108.5 . . ?
H70B C43B H71B 107.5 . . ?
C43B C44B O41 113.4(8) . . ?
C43B C44B H72B 108.9 . . ?
O41 C44B H72B 108.9 . . ?
C43B C44B H73B 108.9 . . ?
O41 C44B H73B 108.9 . . ?
H72B C44B H73B 107.7 . . ?
C112 C111 C116 116.6(2) . . ?
C112 C111 C18 124.2(2) . . ?
C116 C111 C18 119.3(2) . . ?
C111 C112 C113 121.2(2) . . ?
C111 C112 H6 119.4 . . ?
C113 C112 H6 119.4 . . ?
C114 C113 C112 122.4(2) . . ?
C114 C113 H7 118.8 . . ?
C112 C113 H7 118.8 . . ?
C113 C114 C115 116.1(2) . . ?
C113 C114 C117 120.7(2) . . ?
C115 C114 C117 123.1(2) . . ?
C116 C115 C114 121.8(2) . . ?
C116 C115 H8 119.1 . . ?
C114 C115 H8 119.1 . . ?
C115 C116 C111 121.9(2) . . ?
C115 C116 H9 119.0 . . ?
C111 C116 H9 119.0 . . ?
C118 C117 C119 109.5(3) . . ?
C118 C117 C114 110.4(2) . . ?
C119 C117 C114 112.1(2) . . ?
C118 C117 C120 108.2(3) . . ?
C119 C117 C120 107.0(3) . . ?
C114 C117 C120 109.5(2) . . ?
C117 C118 H10 109.5 . . ?
C117 C118 H11 109.5 . . ?
H10 C118 H11 109.5 . . ?
C117 C118 H12 109.5 . . ?
H10 C118 H12 109.5 . . ?
H11 C118 H12 109.5 . . ?
C117 C119 H13 109.5 . . ?
C117 C119 H14 109.5 . . ?
H13 C119 H14 109.5 . . ?
C117 C119 H15 109.5 . . ?
H13 C119 H15 109.5 . . ?
H14 C119 H15 109.5 . . ?
C117 C120 H16 109.5 . . ?
C117 C120 H17 109.5 . . ?
H16 C120 H17 109.5 . . ?
C117 C120 H18 109.5 . . ?
H16 C120 H18 109.5 . . ?
H17 C120 H18 109.5 . . ?
C122 C121 C126 116.5(2) . . ?
C122 C121 C18 124.5(2) . . ?
C126 C121 C18 118.9(2) . . ?
C121 C122 C123 121.6(3) . . ?
C121 C122 H19 119.2 . . ?
C123 C122 H19 119.2 . . ?
C122 C123 C124 122.2(3) . . ?
C122 C123 H20 118.9 . . ?
C124 C123 H20 118.9 . . ?
C123 C124 C125 115.7(2) . . ?
C123 C124 C127 123.9(3) . . ?
C125 C124 C127 120.3(2) . . ?
C126 C125 C124 122.2(3) . . ?
C126 C125 H21 118.9 . . ?
C124 C125 H21 118.9 . . ?
C125 C126 C121 121.5(3) . . ?
C125 C126 H22 119.2 . . ?
C121 C126 H22 119.2 . . ?
C128 C127 C130 109.2(3) . . ?
C128 C127 C129 107.4(3) . . ?
C130 C127 C129 108.9(3) . . ?
C128 C127 C124 112.5(3) . . ?
C130 C127 C124 108.8(3) . . ?
C129 C127 C124 109.9(3) . . ?
C127 C128 H23 109.5 . . ?
C127 C128 H24 109.5 . . ?
H23 C128 H24 109.5 . . ?
C127 C128 H25 109.5 . . ?
H23 C128 H25 109.5 . . ?
H24 C128 H25 109.5 . . ?
C127 C129 H26 109.5 . . ?
C127 C129 H27 109.5 . . ?
H26 C129 H27 109.5 . . ?
C127 C129 H28 109.5 . . ?
H26 C129 H28 109.5 . . ?
H27 C129 H28 109.5 . . ?
C127 C130 H29 109.5 . . ?
C127 C130 H30 109.5 . . ?
H29 C130 H30 109.5 . . ?
C127 C130 H31 109.5 . . ?
H29 C130 H31 109.5 . . ?
H30 C130 H31 109.5 . . ?
C136 C131 C132 116.6(2) . . ?
C136 C131 C18 123.8(2) . . ?
C132 C131 C18 119.5(2) . . ?
C133 C132 C131 121.9(2) . . ?
C133 C132 H32 119.0 . . ?
C131 C132 H32 119.0 . . ?
C132 C133 C134 121.7(2) . . ?
C132 C133 H33 119.1 . . ?
C134 C133 H33 119.1 . . ?
C135 C134 C133 115.9(2) . . ?
C135 C134 C137 124.3(2) . . ?
C133 C134 C137 119.8(2) . . ?
C134 C135 C136 122.1(2) . . ?
C134 C135 H34 119.0 . . ?
C136 C135 H34 119.0 . . ?
C131 C136 C135 121.7(2) . . ?
C131 C136 H35 119.2 . . ?
C135 C136 H35 119.2 . . ?
C139 C137 C134 112.1(2) . . ?
C139 C137 C140 109.2(2) . . ?
C134 C137 C140 109.5(2) . . ?
C139 C137 C138 108.4(3) . . ?
C134 C137 C138 109.8(2) . . ?
C140 C137 C138 107.8(3) . . ?
C137 C138 H36 109.5 . . ?
C137 C138 H37 109.5 . . ?
H36 C138 H37 109.5 . . ?
C137 C138 H38 109.5 . . ?
H36 C138 H38 109.5 . . ?
H37 C138 H38 109.5 . . ?
C137 C139 H39 109.5 . . ?
C137 C139 H40 109.5 . . ?
H39 C139 H40 109.5 . . ?
C137 C139 H41 109.5 . . ?
H39 C139 H41 109.5 . . ?
H40 C139 H41 109.5 . . ?
C137 C140 H42 109.5 . . ?
C137 C140 H43 109.5 . . ?
H42 C140 H43 109.5 . . ?
C137 C140 H44 109.5 . . ?
H42 C140 H44 109.5 . . ?
H43 C140 H44 109.5 . . ?
C17 N1 C12 128.7(2) . . ?
C17 N1 H1 121(2) . . ?
C12 N1 H1 110(2) . . ?
C27 N2 C16 129.4(3) . . ?
C27 N2 H2 117(3) . . ?
C16 N2 H2 114(3) . . ?
C31 N3 C33 110.7(4) . . ?
C31 N3 C34 109.0(3) . . ?
C33 N3 C34 110.6(4) . . ?
C31 N3 C32 108.3(4) . . ?
C33 N3 C32 108.5(4) . . ?
C34 N3 C32 109.7(4) . . ?
C41B O41 C44B 113.2(5) . . ?
C41 O41 C44 113.2(5) . . ?
C43 O42 C42 111.6(13) . . ?
C42B O42B C43B 106.6(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
O11 C1 C11 C12 -11.8(5) . . . . ?
O12 C1 C11 C12 167.6(3) . . . . ?
O11 C1 C11 C16 170.0(3) . . . . ?
O12 C1 C11 C16 -10.6(5) . . . . ?
C16 C11 C12 C13 2.0(4) . . . . ?
C1 C11 C12 C13 -176.3(3) . . . . ?
C16 C11 C12 N1 -176.3(3) . . . . ?
C1 C11 C12 N1 5.3(4) . . . . ?
C11 C12 C13 C14 -0.5(5) . . . . ?
N1 C12 C13 C14 177.8(3) . . . . ?
C12 C13 C14 C15 -1.0(5) . . . . ?
C13 C14 C15 C16 0.9(6) . . . . ?
C14 C15 C16 N2 -179.6(3) . . . . ?
C14 C15 C16 C11 0.8(5) . . . . ?
C12 C11 C16 C15 -2.2(5) . . . . ?
C1 C11 C16 C15 176.1(3) . . . . ?
C12 C11 C16 N2 178.1(3) . . . . ?
C1 C11 C16 N2 -3.5(5) . . . . ?
O1 C17 C18 C111 -137.5(3) . . . . ?
N1 C17 C18 C111 42.6(3) . . . . ?
O1 C17 C18 C121 101.2(3) . . . . ?
N1 C17 C18 C121 -78.6(3) . . . . ?
O1 C17 C18 C131 -16.6(4) . . . . ?
N1 C17 C18 C131 163.5(2) . . . . ?
C28 C21 C22 C23 -73.6(16) . . . . ?
C22 C21 C28 C27 178.3(7) . . . . ?
C28B C21B C22B C23B -43(3) . . . . ?
C22B C21B C28B C27 -177.7(14) . . . . ?
C21B C28B C27 O2 124.8(13) . . . . ?
C21B C28B C27 N2 -52.1(18) . . . . ?
C21 C28 C27 O2 66.7(12) . . . . ?
C21 C28 C27 N2 -119.8(10) . . . . ?
O41 C41 C42 O42 31.6(19) . . . . ?
O42 C43 C44 O41 -43.0(15) . . . . ?
O41 C41B C42B O42B -48(2) . . . . ?
O42B C43B C44B O41 49.9(17) . . . . ?
C121 C18 C111 C112 -8.3(3) . . . . ?
C131 C18 C111 C112 112.3(3) . . . . ?
C17 C18 C111 C112 -129.4(3) . . . . ?
C121 C18 C111 C116 173.4(2) . . . . ?
C131 C18 C111 C116 -66.0(3) . . . . ?
C17 C18 C111 C116 52.3(3) . . . . ?
C116 C111 C112 C113 0.9(4) . . . . ?
C18 C111 C112 C113 -177.5(2) . . . . ?
C111 C112 C113 C114 0.1(4) . . . . ?
C112 C113 C114 C115 -0.8(4) . . . . ?
C112 C113 C114 C117 178.3(2) . . . . ?
C113 C114 C115 C116 0.4(4) . . . . ?
C117 C114 C115 C116 -178.7(3) . . . . ?
C114 C115 C116 C111 0.6(4) . . . . ?
C112 C111 C116 C115 -1.2(4) . . . . ?
C18 C111 C116 C115 177.2(2) . . . . ?
C113 C114 C117 C118 -55.5(4) . . . . ?
C115 C114 C117 C118 123.6(3) . . . . ?
C113 C114 C117 C119 -177.9(3) . . . . ?
C115 C114 C117 C119 1.2(4) . . . . ?
C113 C114 C117 C120 63.5(3) . . . . ?
C115 C114 C117 C120 -117.4(3) . . . . ?
C111 C18 C121 C122 -100.3(3) . . . . ?
C131 C18 C121 C122 137.1(3) . . . . ?
C17 C18 C121 C122 19.6(3) . . . . ?
C111 C18 C121 C126 76.8(3) . . . . ?
C131 C18 C121 C126 -45.8(3) . . . . ?
C17 C18 C121 C126 -163.3(2) . . . . ?
C126 C121 C122 C123 -3.2(4) . . . . ?
C18 C121 C122 C123 174.0(3) . . . . ?
C121 C122 C123 C124 -0.2(5) . . . . ?
C122 C123 C124 C125 3.0(4) . . . . ?
C122 C123 C124 C127 -177.5(3) . . . . ?
C123 C124 C125 C126 -2.5(4) . . . . ?
C127 C124 C125 C126 178.0(3) . . . . ?
C124 C125 C126 C121 -0.8(4) . . . . ?
C122 C121 C126 C125 3.6(4) . . . . ?
C18 C121 C126 C125 -173.7(2) . . . . ?
C123 C124 C127 C128 0.3(4) . . . . ?
C125 C124 C127 C128 179.7(3) . . . . ?
C123 C124 C127 C130 121.5(4) . . . . ?
C125 C124 C127 C130 -59.1(4) . . . . ?
C123 C124 C127 C129 -119.3(3) . . . . ?
C125 C124 C127 C129 60.1(4) . . . . ?
C111 C18 C131 C136 -3.9(3) . . . . ?
C121 C18 C131 C136 118.1(3) . . . . ?
C17 C18 C131 C136 -122.6(3) . . . . ?
C111 C18 C131 C132 178.4(2) . . . . ?
C121 C18 C131 C132 -59.6(3) . . . . ?
C17 C18 C131 C132 59.7(3) . . . . ?
C136 C131 C132 C133 2.9(4) . . . . ?
C18 C131 C132 C133 -179.3(2) . . . . ?
C131 C132 C133 C134 -1.1(4) . . . . ?
C132 C133 C134 C135 -1.4(4) . . . . ?
C132 C133 C134 C137 177.8(2) . . . . ?
C133 C134 C135 C136 2.2(4) . . . . ?
C137 C134 C135 C136 -177.0(2) . . . . ?
C132 C131 C136 C135 -2.2(4) . . . . ?
C18 C131 C136 C135 -179.9(2) . . . . ?
C134 C135 C136 C131 -0.4(4) . . . . ?
C135 C134 C137 C139 2.8(4) . . . . ?
C133 C134 C137 C139 -176.4(3) . . . . ?
C135 C134 C137 C140 124.1(3) . . . . ?
C133 C134 C137 C140 -55.1(3) . . . . ?
C135 C134 C137 C138 -117.7(3) . . . . ?
C133 C134 C137 C138 63.1(3) . . . . ?
O1 C17 N1 C12 0.0(5) . . . . ?
C18 C17 N1 C12 179.9(2) . . . . ?
C13 C12 N1 C17 13.8(4) . . . . ?
C11 C12 N1 C17 -167.8(3) . . . . ?
O2 C27 N2 C16 -6.7(8) . . . . ?
C28B C27 N2 C16 169.9(9) . . . . ?
C28 C27 N2 C16 179.5(6) . . . . ?
C15 C16 N2 C27 15.7(6) . . . . ?
C11 C16 N2 C27 -164.6(4) . . . . ?
C42B C41B O41 C44B 34.9(16) . . . . ?
C42 C41 O41 C44 -21.3(14) . . . . ?
C43B C44B O41 C41B -33.2(12) . . . . ?
C43 C44 O41 C41 27.4(12) . . . . ?
C44 C43 O42 C42 49.0(18) . . . . ?
C41 C42 O42 C43 -44.5(19) . . . . ?
C41B C42B O42B C43B 56(2) . . . . ?
C44B C43B O42B C42B -61.6(19) . . . . ?

_refine_diff_density_max         0.467
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.064

_shelxl_version_number           2014/6
####################################################################### 
# 
# 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/access/V1 
# 
# Audit and citation data items may have 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_L2H-1/2(dioxane)
_database_code_depnum_ccdc_archive 'CCDC 1042061'
_audit_update_record             
;
2015-01-05 deposited with the CCDC.
2015-03-18 downloaded from the CCDC.
;
_audit_creation_date             2014-10-09
_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C41 H49 N O4'
_chemical_formula_sum            'C41 H49 N O4'
_chemical_formula_weight         619.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.7369(14)
_cell_length_b                   12.6605(17)
_cell_length_c                   12.8455(17)
_cell_angle_alpha                73.348(5)
_cell_angle_beta                 71.463(5)
_cell_angle_gamma                83.617(6)
_cell_volume                     1733.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    200
_cell_measurement_reflns_used    4978
_cell_measurement_theta_min      3.00
_cell_measurement_theta_max      27.43

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_F_000             668
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.075
_shelx_estimated_absorpt_T_min   0.991
_shelx_estimated_absorpt_T_max   0.996
_exptl_absorpt_correction_type   none
_diffrn_ambient_temperature      200
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   
;
 MicroMax-007HF microfocus rotating anode X-ray generator
;
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            13072
_diffrn_reflns_av_unetI/netI     0.0894
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.995
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.969
_reflns_number_total             6072
_reflns_number_gt                3408
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'RAPID AUTO (Rigaku, 2006)'
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2006)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2006)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_refine_special_details          
;
Two t-Bu groups (C118-C120, C138-C140) and the dioxane molecule were 
disordered, which were separated into two parts and the occupancies were 
refined. These t-Bu groups were restrained by SADI to prevent to avoid the 
distortion during the refinements. The disordered dioxane molecule was 
restrained by DIFX and SIMU instructions to keep the similarity of the two 
parts. Unusual displacements of anisotropic thermal factors were restrained by 
ISOR and DELU.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0740P)²+0.0185P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6072
_refine_ls_number_parameters     505
_refine_ls_number_restraints     137
_refine_ls_R_factor_all          0.1258
_refine_ls_R_factor_gt           0.0649
_refine_ls_wR_factor_ref         0.1634
_refine_ls_wR_factor_gt          0.1394
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6703(2) 0.4673(2) -0.0223(2) 0.0416(7) Uani 1 1 d . . . . .
C11 C 0.8011(2) 0.4467(2) -0.0459(2) 0.0385(7) Uani 1 1 d . . . . .
C12 C 0.8518(2) 0.3677(2) 0.0306(2) 0.0360(6) Uani 1 1 d . . . . .
C13 C 0.9768(2) 0.3541(2) 0.0008(2) 0.0435(7) Uani 1 1 d . . . . .
H3 H 1.0124 0.3020 0.0516 0.052 Uiso 1 1 calc R U . . .
C14 C 1.0488(2) 0.4153(3) -0.1015(2) 0.0482(8) Uani 1 1 d . . . . .
H4 H 1.1335 0.4040 -0.1205 0.058 Uiso 1 1 calc R U . . .
C15 C 1.0005(2) 0.4926(3) -0.1766(2) 0.0529(8) Uani 1 1 d . . . . .
H5 H 1.0510 0.5353 -0.2463 0.063 Uiso 1 1 calc R U . . .
C16 C 0.8773(2) 0.5068(2) -0.1488(2) 0.0481(8) Uani 1 1 d . . . . .
H6 H 0.8434 0.5589 -0.2010 0.058 Uiso 1 1 calc R U . . .
C17 C 0.8096(2) 0.2325(2) 0.2210(2) 0.0394(7) Uani 1 1 d . . . . .
C18 C 0.7085(2) 0.1606(2) 0.3194(2) 0.0352(6) Uani 1 1 d . . . . .
C21 C 0.9319(6) -0.0809(6) 0.0794(7) 0.088(3) Uani 0.626(8) 1 d D U P A 1
H64 H 0.8997 -0.1507 0.0812 0.106 Uiso 0.626(8) 1 calc R U P A 1
H65 H 0.9108 -0.0774 0.1594 0.106 Uiso 0.626(8) 1 calc R U P A 1
C22 C 1.0627(6) -0.0896(6) 0.0370(9) 0.087(3) Uani 0.626(8) 1 d D U P A 1
H66 H 1.0923 -0.1204 0.1040 0.105 Uiso 0.626(8) 1 calc R U P A 1
H67 H 1.0826 -0.1448 -0.0076 0.105 Uiso 0.626(8) 1 calc R U P A 1
C21B C 0.9930(13) 0.0185(14) 0.0994(13) 0.144(6) Uani 0.374(8) 1 d D U P A 2
H64B H 1.0653 0.0637 0.0567 0.173 Uiso 0.374(8) 1 calc R U P A 2
H65B H 0.9655 0.0205 0.1801 0.173 Uiso 0.374(8) 1 calc R U P A 2
C22B C 1.0076(17) -0.0880(12) 0.0864(13) 0.101(4) Uani 0.374(8) 1 d D U P A 2
H66B H 0.9324 -0.1185 0.0889 0.121 Uiso 0.374(8) 1 calc R U P A 2
H67B H 1.0458 -0.1398 0.1401 0.121 Uiso 0.374(8) 1 calc R U P A 2
C111 C 0.6000(2) 0.1534(2) 0.2788(2) 0.0354(6) Uani 1 1 d . . . . .
C112 C 0.4829(2) 0.1802(2) 0.3348(2) 0.0420(7) Uani 1 1 d . . . . .
H7 H 0.4675 0.2084 0.3992 0.050 Uiso 1 1 calc R U . . .
C113 C 0.3874(2) 0.1662(2) 0.2972(2) 0.0441(7) Uani 1 1 d . . . . .
H8 H 0.3081 0.1843 0.3376 0.053 Uiso 1 1 calc R U . . .
C114 C 0.4045(2) 0.1269(2) 0.2036(2) 0.0397(7) Uani 1 1 d . . . . .
C115 C 0.5226(2) 0.1027(2) 0.1457(2) 0.0427(7) Uani 1 1 d . . . . .
H9 H 0.5380 0.0767 0.0800 0.051 Uiso 1 1 calc R U . . .
C116 C 0.6183(2) 0.1160(2) 0.1826(2) 0.0420(7) Uani 1 1 d . . . . .
H10 H 0.6977 0.0991 0.1413 0.050 Uiso 1 1 calc R U . . .
C117 C 0.2992(2) 0.1086(2) 0.1642(2) 0.0440(7) Uani 1 1 d D . . . .
C118 C 0.3182(5) 0.1777(6) 0.0398(5) 0.067(2) Uani 0.549(6) 1 d D . P B 1
H11 H 0.3219 0.2559 0.0353 0.080 Uiso 0.549(6) 1 calc R U P B 1
H12 H 0.3936 0.1543 -0.0091 0.080 Uiso 0.549(6) 1 calc R U P B 1
H13 H 0.2511 0.1668 0.0144 0.080 Uiso 0.549(6) 1 calc R U P B 1
C119 C 0.1774(4) 0.1452(6) 0.2361(5) 0.063(2) Uani 0.549(6) 1 d D . P B 1
H14 H 0.1799 0.2232 0.2326 0.076 Uiso 0.549(6) 1 calc R U P B 1
H15 H 0.1137 0.1346 0.2060 0.076 Uiso 0.549(6) 1 calc R U P B 1
H16 H 0.1609 0.1009 0.3154 0.076 Uiso 0.549(6) 1 calc R U P B 1
C120 C 0.2936(5) -0.0107(5) 0.1706(6) 0.068(2) Uani 0.549(6) 1 d D . P B 1
H17 H 0.2263 -0.0215 0.1454 0.082 Uiso 0.549(6) 1 calc R U P B 1
H18 H 0.3689 -0.0338 0.1212 0.082 Uiso 0.549(6) 1 calc R U P B 1
H19 H 0.2820 -0.0550 0.2493 0.082 Uiso 0.549(6) 1 calc R U P B 1
C121 C 0.6719(2) 0.2148(2) 0.4192(2) 0.0358(6) Uani 1 1 d . . . . .
C122 C 0.6893(2) 0.3243(2) 0.4052(2) 0.0470(7) Uani 1 1 d . . . . .
H20 H 0.7296 0.3687 0.3317 0.056 Uiso 1 1 calc R U . . .
C123 C 0.6493(2) 0.3713(3) 0.4963(3) 0.0501(8) Uani 1 1 d . . . . .
H21 H 0.6641 0.4469 0.4835 0.060 Uiso 1 1 calc R U . . .
C124 C 0.5884(2) 0.3110(2) 0.6057(2) 0.0448(7) Uani 1 1 d . . . . .
C125 C 0.5721(2) 0.2008(2) 0.6184(2) 0.0458(7) Uani 1 1 d . . . . .
H22 H 0.5308 0.1566 0.6917 0.055 Uiso 1 1 calc R U . . .
C126 C 0.6135(2) 0.1525(2) 0.5289(2) 0.0419(7) Uani 1 1 d . . . . .
H23 H 0.6020 0.0761 0.5423 0.050 Uiso 1 1 calc R U . . .
C127 C 0.5390(3) 0.3621(3) 0.7057(3) 0.0534(8) Uani 1 1 d . . . . .
C128 C 0.5697(3) 0.4839(3) 0.6736(3) 0.0728(10) Uani 1 1 d . . . . .
H24 H 0.5361 0.5128 0.7405 0.087 Uiso 1 1 calc R U . . .
H25 H 0.6572 0.4914 0.6465 0.087 Uiso 1 1 calc R U . . .
H26 H 0.5354 0.5255 0.6131 0.087 Uiso 1 1 calc R U . . .
C129 C 0.5907(3) 0.2997(3) 0.8028(3) 0.0692(10) Uani 1 1 d . . . . .
H27 H 0.5587 0.3328 0.8669 0.083 Uiso 1 1 calc R U . . .
H28 H 0.5678 0.2222 0.8277 0.083 Uiso 1 1 calc R U . . .
H29 H 0.6785 0.3041 0.7758 0.083 Uiso 1 1 calc R U . . .
C130 C 0.4015(3) 0.3536(3) 0.7485(3) 0.0715(10) Uani 1 1 d . . . . .
H30 H 0.3692 0.3864 0.8129 0.086 Uiso 1 1 calc R U . . .
H31 H 0.3680 0.3932 0.6869 0.086 Uiso 1 1 calc R U . . .
H32 H 0.3796 0.2759 0.7732 0.086 Uiso 1 1 calc R U . . .
C131 C 0.7636(2) 0.0445(2) 0.3573(2) 0.0355(6) Uani 1 1 d . . . . .
C132 C 0.7157(2) -0.0512(2) 0.3582(2) 0.0429(7) Uani 1 1 d . . . . .
H33 H 0.6439 -0.0465 0.3378 0.051 Uiso 1 1 calc R U . . .
C133 C 0.7700(2) -0.1534(2) 0.3881(2) 0.0467(7) Uani 1 1 d . . . . .
H34 H 0.7349 -0.2168 0.3865 0.056 Uiso 1 1 calc R U . . .
C134 C 0.8737(2) -0.1666(2) 0.4203(2) 0.0391(7) Uani 1 1 d . . . . .
C135 C 0.9173(2) -0.0713(2) 0.4260(2) 0.0457(7) Uani 1 1 d . . . . .
H35 H 0.9864 -0.0765 0.4506 0.055 Uiso 1 1 calc R U . . .
C136 C 0.8630(2) 0.0309(2) 0.3969(2) 0.0415(7) Uani 1 1 d . . . . .
H36 H 0.8944 0.0935 0.4042 0.050 Uiso 1 1 calc R U . . .
C137 C 0.9389(2) -0.2783(2) 0.4458(2) 0.0513(8) Uani 1 1 d D U . . .
C138 C 1.0171(10) -0.2984(11) 0.3361(7) 0.114(5) Uani 0.557(9) 1 d D U P C 1
H37 H 1.0710 -0.2363 0.2939 0.136 Uiso 0.557(9) 1 calc R U P C 1
H38 H 1.0650 -0.3664 0.3518 0.136 Uiso 0.557(9) 1 calc R U P C 1
H39 H 0.9670 -0.3059 0.2906 0.136 Uiso 0.557(9) 1 calc R U P C 1
C139 C 0.8530(6) -0.3686(6) 0.5170(10) 0.104(4) Uani 0.557(9) 1 d D U P C 1
H40 H 0.8046 -0.3502 0.5874 0.124 Uiso 0.557(9) 1 calc R U P C 1
H41 H 0.8000 -0.3773 0.4746 0.124 Uiso 0.557(9) 1 calc R U P C 1
H42 H 0.8980 -0.4378 0.5358 0.124 Uiso 0.557(9) 1 calc R U P C 1
C140 C 1.0269(8) -0.2770(6) 0.5171(7) 0.075(3) Uani 0.557(9) 1 d D U P C 1
H43 H 0.9803 -0.2639 0.5907 0.090 Uiso 0.557(9) 1 calc R U P C 1
H44 H 1.0700 -0.3481 0.5298 0.090 Uiso 0.557(9) 1 calc R U P C 1
H45 H 1.0849 -0.2180 0.4749 0.090 Uiso 0.557(9) 1 calc R U P C 1
C148 C 0.2406(7) 0.2179(6) 0.1254(8) 0.081(3) Uani 0.451(6) 1 d D . P B 2
H46 H 0.2992 0.2656 0.0616 0.097 Uiso 0.451(6) 1 calc R U P B 2
H47 H 0.1729 0.2069 0.1007 0.097 Uiso 0.451(6) 1 calc R U P B 2
H48 H 0.2113 0.2526 0.1884 0.097 Uiso 0.451(6) 1 calc R U P B 2
C149 C 0.2090(6) 0.0326(7) 0.2640(5) 0.071(3) Uani 0.451(6) 1 d D . P B 2
H49 H 0.2485 -0.0385 0.2886 0.085 Uiso 0.451(6) 1 calc R U P B 2
H50 H 0.1796 0.0667 0.3276 0.085 Uiso 0.451(6) 1 calc R U P B 2
H51 H 0.1412 0.0209 0.2399 0.085 Uiso 0.451(6) 1 calc R U P B 2
C150 C 0.3395(6) 0.0518(6) 0.0674(6) 0.061(3) Uani 0.451(6) 1 d D . P B 2
H52 H 0.3778 -0.0197 0.0928 0.073 Uiso 0.451(6) 1 calc R U P B 2
H53 H 0.2694 0.0404 0.0464 0.073 Uiso 0.451(6) 1 calc R U P B 2
H54 H 0.3970 0.0982 0.0013 0.073 Uiso 0.451(6) 1 calc R U P B 2
C168 C 0.8745(8) -0.3679(7) 0.4202(11) 0.076(3) Uani 0.443(9) 1 d D U P C 2
H55 H 0.8773 -0.3455 0.3398 0.091 Uiso 0.443(9) 1 calc R U P C 2
H56 H 0.9160 -0.4395 0.4367 0.091 Uiso 0.443(9) 1 calc R U P C 2
H57 H 0.7906 -0.3740 0.4682 0.091 Uiso 0.443(9) 1 calc R U P C 2
C169 C 0.9314(10) -0.3171(7) 0.5676(6) 0.073(4) Uani 0.443(9) 1 d D . P C 2
H58 H 0.8470 -0.3172 0.6141 0.087 Uiso 0.443(9) 1 calc R U P C 2
H59 H 0.9656 -0.3921 0.5837 0.087 Uiso 0.443(9) 1 calc R U P C 2
H60 H 0.9765 -0.2679 0.5859 0.087 Uiso 0.443(9) 1 calc R U P C 2
C170 C 1.0660(8) -0.2757(12) 0.3684(10) 0.109(6) Uani 0.443(9) 1 d D . P C 2
H61 H 1.0660 -0.2495 0.2889 0.131 Uiso 0.443(9) 1 calc R U P C 2
H62 H 1.1129 -0.2259 0.3841 0.131 Uiso 0.443(9) 1 calc R U P C 2
H63 H 1.1020 -0.3501 0.3819 0.131 Uiso 0.443(9) 1 calc R U P C 2
N1 N 0.77646(18) 0.30277(18) 0.13326(18) 0.0401(6) Uani 1 1 d . . . . .
H1 H 0.696(2) 0.313(2) 0.137(2) 0.048 Uiso 1 1 d . U . . .
O1 O 0.91135(16) 0.22753(19) 0.22665(17) 0.0656(7) Uani 1 1 d . . . . .
O11 O 0.64168(18) 0.55024(17) -0.09940(18) 0.0612(7) Uani 1 1 d . . . . .
H2 H 0.556(3) 0.569(3) -0.076(2) 0.073 Uiso 1 1 d . U . . .
O12 O 0.59377(15) 0.41406(16) 0.05953(16) 0.0509(6) Uani 1 1 d . . . . .
O21 O 0.8735(5) 0.0000(6) 0.0271(6) 0.0827(18) Uani 0.626(8) 1 d D U P A 1
O21B O 0.8986(11) 0.0458(13) 0.0454(12) 0.113(4) Uani 0.374(8) 1 d D U 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
C1 O12 1.223(3) . ?
C1 O11 1.316(3) . ?
C1 C11 1.475(4) . ?
C11 C16 1.396(4) . ?
C11 C12 1.413(3) . ?
C12 C13 1.397(3) . ?
C12 N1 1.413(3) . ?
C13 C14 1.377(4) . ?
C13 H3 0.9500 . ?
C14 C15 1.376(4) . ?
C14 H4 0.9500 . ?
C15 C16 1.378(4) . ?
C15 H5 0.9500 . ?
C16 H6 0.9500 . ?
C17 O1 1.213(3) . ?
C17 N1 1.356(3) . ?
C17 C18 1.568(3) . ?
C18 C111 1.542(3) . ?
C18 C121 1.546(4) . ?
C18 C131 1.548(4) . ?
C21 O21 1.308(8) . ?
C21 C22 1.460(8) . ?
C21 H64 0.9900 . ?
C21 H65 0.9900 . ?
C22 O21 1.337(9) 2_755 ?
C22 H66 0.9900 . ?
C22 H67 0.9900 . ?
C21B C22B 1.391(15) . ?
C21B O21B 1.447(13) . ?
C21B H64B 0.9900 . ?
C21B H65B 0.9900 . ?
C22B O21B 1.671(17) 2_755 ?
C22B H66B 0.9900 . ?
C22B H67B 0.9900 . ?
C111 C112 1.388(3) . ?
C111 C116 1.394(4) . ?
C112 C113 1.400(3) . ?
C112 H7 0.9500 . ?
C113 C114 1.379(4) . ?
C113 H8 0.9500 . ?
C114 C115 1.396(4) . ?
C114 C117 1.537(3) . ?
C115 C116 1.393(3) . ?
C115 H9 0.9500 . ?
C116 H10 0.9500 . ?
C117 C120 1.497(6) . ?
C117 C148 1.500(7) . ?
C117 C149 1.532(6) . ?
C117 C150 1.533(7) . ?
C117 C119 1.540(6) . ?
C117 C118 1.544(5) . ?
C118 H11 0.9800 . ?
C118 H12 0.9800 . ?
C118 H13 0.9800 . ?
C119 H14 0.9800 . ?
C119 H15 0.9800 . ?
C119 H16 0.9800 . ?
C120 H17 0.9800 . ?
C120 H18 0.9800 . ?
C120 H19 0.9800 . ?
C121 C122 1.375(4) . ?
C121 C126 1.395(3) . ?
C122 C123 1.390(4) . ?
C122 H20 0.9500 . ?
C123 C124 1.391(4) . ?
C123 H21 0.9500 . ?
C124 C125 1.385(4) . ?
C124 C127 1.525(4) . ?
C125 C126 1.383(4) . ?
C125 H22 0.9500 . ?
C126 H23 0.9500 . ?
C127 C128 1.530(4) . ?
C127 C129 1.535(4) . ?
C127 C130 1.536(4) . ?
C128 H24 0.9800 . ?
C128 H25 0.9800 . ?
C128 H26 0.9800 . ?
C129 H27 0.9800 . ?
C129 H28 0.9800 . ?
C129 H29 0.9800 . ?
C130 H30 0.9800 . ?
C130 H31 0.9800 . ?
C130 H32 0.9800 . ?
C131 C132 1.387(4) . ?
C131 C136 1.390(3) . ?
C132 C133 1.385(4) . ?
C132 H33 0.9500 . ?
C133 C134 1.384(3) . ?
C133 H34 0.9500 . ?
C134 C135 1.391(4) . ?
C134 C137 1.531(4) . ?
C135 C136 1.382(4) . ?
C135 H35 0.9500 . ?
C136 H36 0.9500 . ?
C137 C169 1.476(7) . ?
C137 C138 1.492(8) . ?
C137 C139 1.494(6) . ?
C137 C170 1.505(8) . ?
C137 C140 1.589(6) . ?
C137 C168 1.590(7) . ?
C138 H37 0.9800 . ?
C138 H38 0.9800 . ?
C138 H39 0.9800 . ?
C139 H40 0.9800 . ?
C139 H41 0.9800 . ?
C139 H42 0.9800 . ?
C140 H43 0.9800 . ?
C140 H44 0.9800 . ?
C140 H45 0.9800 . ?
C148 H46 0.9800 . ?
C148 H47 0.9800 . ?
C148 H48 0.9800 . ?
C149 H49 0.9800 . ?
C149 H50 0.9800 . ?
C149 H51 0.9800 . ?
C150 H52 0.9800 . ?
C150 H53 0.9800 . ?
C150 H54 0.9800 . ?
C168 H55 0.9800 . ?
C168 H56 0.9800 . ?
C168 H57 0.9800 . ?
C169 H58 0.9800 . ?
C169 H59 0.9800 . ?
C169 H60 0.9800 . ?
C170 H61 0.9800 . ?
C170 H62 0.9800 . ?
C170 H63 0.9800 . ?
N1 H1 0.92(3) . ?
O11 H2 0.98(3) . ?
O21 C22 1.337(9) 2_755 ?
O21B C22B 1.671(17) 2_755 ?

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
O12 C1 O11 121.8(2) . . ?
O12 C1 C11 124.9(2) . . ?
O11 C1 C11 113.3(2) . . ?
C16 C11 C12 118.9(2) . . ?
C16 C11 C1 118.4(2) . . ?
C12 C11 C1 122.6(2) . . ?
C13 C12 C11 118.5(2) . . ?
C13 C12 N1 121.4(2) . . ?
C11 C12 N1 120.0(2) . . ?
C14 C13 C12 120.8(3) . . ?
C14 C13 H3 119.6 . . ?
C12 C13 H3 119.6 . . ?
C15 C14 C13 121.3(3) . . ?
C15 C14 H4 119.4 . . ?
C13 C14 H4 119.4 . . ?
C14 C15 C16 118.7(2) . . ?
C14 C15 H5 120.6 . . ?
C16 C15 H5 120.6 . . ?
C15 C16 C11 121.8(3) . . ?
C15 C16 H6 119.1 . . ?
C11 C16 H6 119.1 . . ?
O1 C17 N1 122.3(2) . . ?
O1 C17 C18 120.6(2) . . ?
N1 C17 C18 117.0(2) . . ?
C111 C18 C121 111.1(2) . . ?
C111 C18 C131 110.6(2) . . ?
C121 C18 C131 109.3(2) . . ?
C111 C18 C17 110.95(19) . . ?
C121 C18 C17 107.2(2) . . ?
C131 C18 C17 107.6(2) . . ?
O21 C21 C22 120.3(6) . . ?
O21 C21 H64 107.3 . . ?
C22 C21 H64 107.3 . . ?
O21 C21 H65 107.3 . . ?
C22 C21 H65 107.3 . . ?
H64 C21 H65 106.9 . . ?
O21 C22 C21 119.9(6) 2_755 . ?
O21 C22 H66 107.3 2_755 . ?
C21 C22 H66 107.3 . . ?
O21 C22 H67 107.3 2_755 . ?
C21 C22 H67 107.3 . . ?
H66 C22 H67 106.9 . . ?
C22B C21B O21B 92.7(12) . . ?
C22B C21B H64B 113.2 . . ?
O21B C21B H64B 113.2 . . ?
C22B C21B H65B 113.2 . . ?
O21B C21B H65B 113.2 . . ?
H64B C21B H65B 110.5 . . ?
C21B C22B O21B 91.8(11) . 2_755 ?
C21B C22B H66B 113.3 . . ?
O21B C22B H66B 113.3 2_755 . ?
C21B C22B H67B 113.3 . . ?
O21B C22B H67B 113.3 2_755 . ?
H66B C22B H67B 110.6 . . ?
C112 C111 C116 117.5(2) . . ?
C112 C111 C18 123.4(3) . . ?
C116 C111 C18 119.1(2) . . ?
C111 C112 C113 120.5(3) . . ?
C111 C112 H7 119.7 . . ?
C113 C112 H7 119.7 . . ?
C114 C113 C112 122.3(2) . . ?
C114 C113 H8 118.9 . . ?
C112 C113 H8 118.9 . . ?
C113 C114 C115 117.0(2) . . ?
C113 C114 C117 122.2(2) . . ?
C115 C114 C117 120.7(3) . . ?
C116 C115 C114 121.2(3) . . ?
C116 C115 H9 119.4 . . ?
C114 C115 H9 119.4 . . ?
C115 C116 C111 121.4(2) . . ?
C115 C116 H10 119.3 . . ?
C111 C116 H10 119.3 . . ?
C148 C117 C149 110.3(5) . . ?
C148 C117 C150 109.4(5) . . ?
C149 C117 C150 106.8(4) . . ?
C120 C117 C114 110.1(3) . . ?
C148 C117 C114 108.9(3) . . ?
C149 C117 C114 108.9(3) . . ?
C150 C117 C114 112.4(3) . . ?
C120 C117 C119 108.7(4) . . ?
C114 C117 C119 112.5(3) . . ?
C120 C117 C118 109.2(4) . . ?
C114 C117 C118 109.0(3) . . ?
C119 C117 C118 107.2(4) . . ?
C117 C118 H11 109.5 . . ?
C117 C118 H12 109.5 . . ?
H11 C118 H12 109.5 . . ?
C117 C118 H13 109.5 . . ?
H11 C118 H13 109.5 . . ?
H12 C118 H13 109.5 . . ?
C117 C119 H14 109.5 . . ?
C117 C119 H15 109.5 . . ?
H14 C119 H15 109.5 . . ?
C117 C119 H16 109.5 . . ?
H14 C119 H16 109.5 . . ?
H15 C119 H16 109.5 . . ?
C117 C120 H17 109.5 . . ?
C117 C120 H18 109.5 . . ?
H17 C120 H18 109.5 . . ?
C117 C120 H19 109.5 . . ?
H17 C120 H19 109.5 . . ?
H18 C120 H19 109.5 . . ?
C122 C121 C126 117.3(3) . . ?
C122 C121 C18 123.1(2) . . ?
C126 C121 C18 119.5(2) . . ?
C121 C122 C123 121.4(3) . . ?
C121 C122 H20 119.3 . . ?
C123 C122 H20 119.3 . . ?
C122 C123 C124 122.0(3) . . ?
C122 C123 H21 119.0 . . ?
C124 C123 H21 119.0 . . ?
C125 C124 C123 115.8(3) . . ?
C125 C124 C127 121.3(3) . . ?
C123 C124 C127 122.9(3) . . ?
C126 C125 C124 122.8(3) . . ?
C126 C125 H22 118.6 . . ?
C124 C125 H22 118.6 . . ?
C125 C126 C121 120.7(3) . . ?
C125 C126 H23 119.7 . . ?
C121 C126 H23 119.7 . . ?
C124 C127 C128 112.7(3) . . ?
C124 C127 C129 109.8(3) . . ?
C128 C127 C129 108.3(3) . . ?
C124 C127 C130 109.1(2) . . ?
C128 C127 C130 107.9(3) . . ?
C129 C127 C130 109.1(3) . . ?
C127 C128 H24 109.5 . . ?
C127 C128 H25 109.5 . . ?
H24 C128 H25 109.5 . . ?
C127 C128 H26 109.5 . . ?
H24 C128 H26 109.5 . . ?
H25 C128 H26 109.5 . . ?
C127 C129 H27 109.5 . . ?
C127 C129 H28 109.5 . . ?
H27 C129 H28 109.5 . . ?
C127 C129 H29 109.5 . . ?
H27 C129 H29 109.5 . . ?
H28 C129 H29 109.5 . . ?
C127 C130 H30 109.5 . . ?
C127 C130 H31 109.5 . . ?
H30 C130 H31 109.5 . . ?
C127 C130 H32 109.5 . . ?
H30 C130 H32 109.5 . . ?
H31 C130 H32 109.5 . . ?
C132 C131 C136 116.2(2) . . ?
C132 C131 C18 123.0(2) . . ?
C136 C131 C18 120.7(2) . . ?
C133 C132 C131 121.5(2) . . ?
C133 C132 H33 119.2 . . ?
C131 C132 H33 119.2 . . ?
C134 C133 C132 122.3(3) . . ?
C134 C133 H34 118.8 . . ?
C132 C133 H34 118.8 . . ?
C133 C134 C135 115.9(2) . . ?
C133 C134 C137 122.5(3) . . ?
C135 C134 C137 121.6(2) . . ?
C136 C135 C134 122.0(2) . . ?
C136 C135 H35 119.0 . . ?
C134 C135 H35 119.0 . . ?
C135 C136 C131 121.8(3) . . ?
C135 C136 H36 119.1 . . ?
C131 C136 H36 119.1 . . ?
C138 C137 C139 113.8(6) . . ?
C169 C137 C170 112.8(6) . . ?
C169 C137 C134 110.8(4) . . ?
C138 C137 C134 108.8(5) . . ?
C139 C137 C134 111.7(4) . . ?
C170 C137 C134 111.8(6) . . ?
C138 C137 C140 105.7(5) . . ?
C139 C137 C140 105.8(4) . . ?
C134 C137 C140 110.9(3) . . ?
C169 C137 C168 106.5(5) . . ?
C170 C137 C168 105.1(6) . . ?
C134 C137 C168 109.4(4) . . ?
C137 C138 H37 109.5 . . ?
C137 C138 H38 109.5 . . ?
H37 C138 H38 109.5 . . ?
C137 C138 H39 109.5 . . ?
H37 C138 H39 109.5 . . ?
H38 C138 H39 109.5 . . ?
C137 C139 H40 109.5 . . ?
C137 C139 H41 109.5 . . ?
H40 C139 H41 109.5 . . ?
C137 C139 H42 109.5 . . ?
H40 C139 H42 109.5 . . ?
H41 C139 H42 109.5 . . ?
C137 C140 H43 109.5 . . ?
C137 C140 H44 109.5 . . ?
H43 C140 H44 109.5 . . ?
C137 C140 H45 109.5 . . ?
H43 C140 H45 109.5 . . ?
H44 C140 H45 109.5 . . ?
C117 C148 H46 109.5 . . ?
C117 C148 H47 109.5 . . ?
H46 C148 H47 109.5 . . ?
C117 C148 H48 109.5 . . ?
H46 C148 H48 109.5 . . ?
H47 C148 H48 109.5 . . ?
C117 C149 H49 109.5 . . ?
C117 C149 H50 109.5 . . ?
H49 C149 H50 109.5 . . ?
C117 C149 H51 109.5 . . ?
H49 C149 H51 109.5 . . ?
H50 C149 H51 109.5 . . ?
C117 C150 H52 109.5 . . ?
C117 C150 H53 109.5 . . ?
H52 C150 H53 109.5 . . ?
C117 C150 H54 109.5 . . ?
H52 C150 H54 109.5 . . ?
H53 C150 H54 109.5 . . ?
C137 C168 H55 109.5 . . ?
C137 C168 H56 109.5 . . ?
H55 C168 H56 109.5 . . ?
C137 C168 H57 109.5 . . ?
H55 C168 H57 109.5 . . ?
H56 C168 H57 109.5 . . ?
C137 C169 H58 109.5 . . ?
C137 C169 H59 109.5 . . ?
H58 C169 H59 109.5 . . ?
C137 C169 H60 109.5 . . ?
H58 C169 H60 109.5 . . ?
H59 C169 H60 109.5 . . ?
C137 C170 H61 109.5 . . ?
C137 C170 H62 109.5 . . ?
H61 C170 H62 109.5 . . ?
C137 C170 H63 109.5 . . ?
H61 C170 H63 109.5 . . ?
H62 C170 H63 109.5 . . ?
C17 N1 C12 127.6(2) . . ?
C17 N1 H1 120.0(16) . . ?
C12 N1 H1 112.4(16) . . ?
C1 O11 H2 111.1(18) . . ?
C21 O21 C22 115.8(6) . 2_755 ?
C21B O21B C22B 94.6(11) . 2_755 ?

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
O12 C1 C11 C16 173.5(3) . . . . ?
O11 C1 C11 C16 -6.3(4) . . . . ?
O12 C1 C11 C12 -5.6(5) . . . . ?
O11 C1 C11 C12 174.6(3) . . . . ?
C16 C11 C12 C13 0.9(4) . . . . ?
C1 C11 C12 C13 180.0(3) . . . . ?
C16 C11 C12 N1 -177.5(2) . . . . ?
C1 C11 C12 N1 1.6(4) . . . . ?
C11 C12 C13 C14 -0.7(4) . . . . ?
N1 C12 C13 C14 177.7(3) . . . . ?
C12 C13 C14 C15 0.8(5) . . . . ?
C13 C14 C15 C16 -1.1(5) . . . . ?
C14 C15 C16 C11 1.3(5) . . . . ?
C12 C11 C16 C15 -1.2(4) . . . . ?
C1 C11 C16 C15 179.6(3) . . . . ?
O1 C17 C18 C111 -162.8(3) . . . . ?
N1 C17 C18 C111 19.9(4) . . . . ?
O1 C17 C18 C121 75.7(3) . . . . ?
N1 C17 C18 C121 -101.6(3) . . . . ?
O1 C17 C18 C131 -41.7(4) . . . . ?
N1 C17 C18 C131 141.0(2) . . . . ?
O21 C21 C22 O21 23.3(17) . . . 2_755 ?
O21B C21B C22B O21B 85.3(12) . . . 2_755 ?
C121 C18 C111 C112 -7.2(3) . . . . ?
C131 C18 C111 C112 114.4(3) . . . . ?
C17 C18 C111 C112 -126.4(3) . . . . ?
C121 C18 C111 C116 174.3(2) . . . . ?
C131 C18 C111 C116 -64.2(3) . . . . ?
C17 C18 C111 C116 55.1(3) . . . . ?
C116 C111 C112 C113 2.1(4) . . . . ?
C18 C111 C112 C113 -176.5(2) . . . . ?
C111 C112 C113 C114 -0.8(4) . . . . ?
C112 C113 C114 C115 -0.9(4) . . . . ?
C112 C113 C114 C117 178.3(2) . . . . ?
C113 C114 C115 C116 1.1(4) . . . . ?
C117 C114 C115 C116 -178.1(2) . . . . ?
C114 C115 C116 C111 0.3(4) . . . . ?
C112 C111 C116 C115 -1.9(4) . . . . ?
C18 C111 C116 C115 176.8(2) . . . . ?
C113 C114 C117 C120 -118.0(4) . . . . ?
C115 C114 C117 C120 61.1(4) . . . . ?
C113 C114 C117 C148 65.4(5) . . . . ?
C115 C114 C117 C148 -115.5(5) . . . . ?
C113 C114 C117 C149 -55.0(5) . . . . ?
C115 C114 C117 C149 124.1(5) . . . . ?
C113 C114 C117 C150 -173.2(4) . . . . ?
C115 C114 C117 C150 6.0(5) . . . . ?
C113 C114 C117 C119 3.4(4) . . . . ?
C115 C114 C117 C119 -177.5(4) . . . . ?
C113 C114 C117 C118 122.2(4) . . . . ?
C115 C114 C117 C118 -58.6(4) . . . . ?
C111 C18 C121 C122 -98.2(3) . . . . ?
C131 C18 C121 C122 139.5(2) . . . . ?
C17 C18 C121 C122 23.2(3) . . . . ?
C111 C18 C121 C126 78.9(3) . . . . ?
C131 C18 C121 C126 -43.4(3) . . . . ?
C17 C18 C121 C126 -159.7(2) . . . . ?
C126 C121 C122 C123 -0.7(4) . . . . ?
C18 C121 C122 C123 176.6(2) . . . . ?
C121 C122 C123 C124 -0.9(4) . . . . ?
C122 C123 C124 C125 1.2(4) . . . . ?
C122 C123 C124 C127 -177.3(2) . . . . ?
C123 C124 C125 C126 0.1(4) . . . . ?
C127 C124 C125 C126 178.6(2) . . . . ?
C124 C125 C126 C121 -1.7(4) . . . . ?
C122 C121 C126 C125 1.9(4) . . . . ?
C18 C121 C126 C125 -175.4(2) . . . . ?
C125 C124 C127 C128 178.7(3) . . . . ?
C123 C124 C127 C128 -3.0(4) . . . . ?
C125 C124 C127 C129 57.9(3) . . . . ?
C123 C124 C127 C129 -123.7(3) . . . . ?
C125 C124 C127 C130 -61.5(4) . . . . ?
C123 C124 C127 C130 116.8(3) . . . . ?
C111 C18 C131 C132 -2.7(3) . . . . ?
C121 C18 C131 C132 119.9(3) . . . . ?
C17 C18 C131 C132 -124.0(3) . . . . ?
C111 C18 C131 C136 179.8(2) . . . . ?
C121 C18 C131 C136 -57.6(3) . . . . ?
C17 C18 C131 C136 58.5(3) . . . . ?
C136 C131 C132 C133 -5.1(4) . . . . ?
C18 C131 C132 C133 177.3(3) . . . . ?
C131 C132 C133 C134 0.9(4) . . . . ?
C132 C133 C134 C135 2.9(4) . . . . ?
C132 C133 C134 C137 -175.8(3) . . . . ?
C133 C134 C135 C136 -2.5(4) . . . . ?
C137 C134 C135 C136 176.3(3) . . . . ?
C134 C135 C136 C131 -1.8(4) . . . . ?
C132 C131 C136 C135 5.5(4) . . . . ?
C18 C131 C136 C135 -176.8(2) . . . . ?
C133 C134 C137 C169 -112.9(6) . . . . ?
C135 C134 C137 C169 68.4(6) . . . . ?
C133 C134 C137 C138 82.4(6) . . . . ?
C135 C134 C137 C138 -96.3(6) . . . . ?
C133 C134 C137 C139 -44.0(6) . . . . ?
C135 C134 C137 C139 137.3(6) . . . . ?
C133 C134 C137 C170 120.3(7) . . . . ?
C135 C134 C137 C170 -58.3(7) . . . . ?
C133 C134 C137 C140 -161.8(4) . . . . ?
C135 C134 C137 C140 19.6(5) . . . . ?
C133 C134 C137 C168 4.2(6) . . . . ?
C135 C134 C137 C168 -174.4(5) . . . . ?
O1 C17 N1 C12 9.3(5) . . . . ?
C18 C17 N1 C12 -173.4(3) . . . . ?
C13 C12 N1 C17 9.4(4) . . . . ?
C11 C12 N1 C17 -172.2(3) . . . . ?
C22 C21 O21 C22 -22.4(16) . . . 2_755 ?
C22B C21B O21B C22B -88.0(11) . . . 2_755 ?

_refine_diff_density_max         0.379
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.051

_shelxl_version_number           2014/6
####################################################################### 
# 
# 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/access/V1 
# 
# Audit and citation data items may have 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_Ca2L24-4(1,4-dioxane)-4H2O
_database_code_depnum_ccdc_archive 'CCDC 1042062'
_audit_update_record             
;
2015-01-05 deposited with the CCDC.
2015-03-18 downloaded from the CCDC.
;
_audit_creation_date             2014-09-04
_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        
; 
 [{[(t-BuC6H4)3CCONH](n-BuCONH)C6H3COO}4Ca2(H2O)5(dioxane)]-4(dioxane)-4(H2O)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C196 H270 Ca2 N8 O35'
_chemical_formula_sum            'C196 H270 Ca2 N8 O35'
_chemical_formula_weight         3378.34

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'
Ca Ca 0.2262 0.3064 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.0688(18)
_cell_length_b                   11.3006(12)
_cell_length_c                   50.441(5)
_cell_angle_alpha                90
_cell_angle_beta                 108.006(6)
_cell_angle_gamma                90
_cell_volume                     9795.1(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    200
_cell_measurement_reflns_used    9679
_cell_measurement_theta_min      3.04
_cell_measurement_theta_max      27.48

_exptl_crystal_description       platelet
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_F_000             3644
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.129
_shelx_estimated_absorpt_T_min   0.975
_shelx_estimated_absorpt_T_max   0.997
_exptl_absorpt_correction_type   none
_diffrn_ambient_temperature      200
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   
;
 MicroMax-007HF microfocus rotating anode X-ray generator
;
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            73841
_diffrn_reflns_av_unetI/netI     0.2513
_diffrn_reflns_av_R_equivalents  0.2746
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_theta_min         3.044
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.970
_reflns_number_total             17222
_reflns_number_gt                5008
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'RAPID AUTO (Rigaku, 2006)'
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2006)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_refine_special_details          
;
This crystal has crystallographic inversion center at the midpoint between two 
Ca atoms of the dinuclear complex. The real structure is dinucler Ca complex 
containing two non-equivalent Ca ions although the space group is not Pc. Two 
Ca ions, Ca1 and Ca2, are 0.5 occupancy. Two water molecules (O5, O6), dioxane 
molecule (O51), two carboxylate groups (O11, O12, and O21), amide group (O3) 
are coordinated to Ca1 atom. Water molecule (O31) is interacted with O6 (H2O). 
To Ca2 atom, three water molecules (O7, O8, O9) are coordinated. Two 
carboxylate groups (O11, O12, O21) and amide group (O3) are also coordinated 
to Ca2 similar to the situation of Ca1. One dioxane (O71, O72 C71-C74) is near 
to O8 instead of O31 and O6 neighboring Ca1. A water molecule (O32) is present 
instead of the dioxane (O61, O62, C61-C64). The occupancy must be 0.5, 
therefore, fixed. Two sets of the surrounding of Ca ions are refined using 
PART. The dioxane molecules and n-Bu group were restrained by DFIX instruction.
 Unusual displacements of anisotropic thermal factors were restrained by ISOR 
and DELU.  
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         17222
_refine_ls_number_parameters     1207
_refine_ls_number_restraints     223
_refine_ls_R_factor_all          0.3361
_refine_ls_R_factor_gt           0.1481
_refine_ls_wR_factor_ref         0.4705
_refine_ls_wR_factor_gt          0.3610
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Ca1 Ca 0.1921(2) 0.4740(4) 0.57243(11) 0.0807(14) Uani 0.5 1 d . . P A 1
Ca2 Ca 0.1633(3) 0.5289(5) 0.57925(11) 0.0878(15) Uani 0.5 1 d . . P A 2
O1 O -0.1394(4) 0.1692(5) 0.59951(14) 0.099(2) Uani 1 1 d . . . . .
O2 O 0.5972(4) 0.3601(5) 0.68142(15) 0.105(2) Uani 1 1 d . . . . .
O3 O 0.0955(5) 0.6301(7) 0.54496(17) 0.133(3) Uani 1 1 d . . . . .
O4 O 0.2617(9) -0.0470(15) 0.5933(3) 0.251(7) Uani 1 1 d . U . . .
O5 O 0.2893(6) 0.6152(12) 0.5699(3) 0.100(4) Uani 0.5 1 d . . P A 1
O6 O 0.2615(8) 0.3863(16) 0.5436(3) 0.110(5) Uani 0.5 1 d . . P A 1
O7 O 0.2610(7) 0.6709(12) 0.5931(4) 0.122(6) Uani 0.5 1 d . . P A 2
O8 O 0.2502(9) 0.4896(19) 0.5508(4) 0.134(6) Uani 0.5 1 d . . P A 2
O9 O 0.1305(16) 0.590(3) 0.6198(9) 0.24(2) Uani 0.5 1 d . . P A 2
O11 O 0.0979(4) 0.3437(7) 0.54450(15) 0.115(2) Uani 1 1 d . . . . .
O12 O 0.0599(4) 0.4052(6) 0.57974(16) 0.103(2) Uani 1 1 d . . . . .
O21 O 0.2594(4) 0.3702(9) 0.60587(17) 0.161(4) Uani 1 1 d . . . . .
O22 O 0.3675(4) 0.4615(9) 0.60610(19) 0.163(4) Uani 1 1 d . . . . .
O31 O 0.3326(16) 0.027(3) 0.5214(13) 0.31(3) Uani 0.5 1 d . . P B 1
O32 O 0.1199(15) 0.781(2) 0.6530(4) 0.197(10) Uani 0.5 1 d . . P C 2
O41 O 0.3045(10) 0.8533(15) 0.5569(6) 0.393(13) Uani 1 1 d . . . . .
O51 O 0.1942(10) 0.5748(14) 0.6143(4) 0.128(6) Uani 0.5 1 d D U P A 1
O52 O 0.2062(13) 0.8023(15) 0.6347(5) 0.191(8) Uani 0.5 1 d D U P A 1
O61 O 0.0695(8) 0.840(2) 0.6655(4) 0.193(10) Uani 0.5 1 d D . P D 1
O62 O 0.1507(7) 0.9440(14) 0.7059(3) 0.115(5) Uani 0.5 1 d D . P D 1
O71 O 0.2825(13) 0.203(2) 0.5363(4) 0.225(12) Uani 0.5 1 d D U P E 2
O72 O 0.3225(18) 0.046(3) 0.4991(5) 0.189(13) Uani 0.5 1 d D U P E 2
O81 O 0.6528(8) 0.2965(11) 0.5821(4) 0.227(7) Uani 1 1 d D U . . .
O82 O 0.5919(7) 0.0790(10) 0.5706(3) 0.213(5) Uani 1 1 d D . . . .
N1 N -0.0648(4) 0.3013(6) 0.5851(2) 0.090(2) Uani 1 1 d . . . . .
H1 H -0.0270 0.3530 0.5914 0.108 Uiso 1 1 calc R U . . .
N2 N 0.4907(4) 0.3913(6) 0.64506(16) 0.087(2) Uani 1 1 d . . . . .
H2 H 0.4641 0.4470 0.6340 0.105 Uiso 1 1 calc R U . . .
N3 N -0.0093(4) 0.3197(6) 0.4969(2) 0.092(2) Uani 1 1 d . . . . .
H3 H 0.0408 0.3127 0.5057 0.110 Uiso 1 1 calc R U . . .
N4 N 0.2678(7) 0.1431(12) 0.6068(2) 0.186(5) Uani 1 1 d . U . . .
H4 H 0.2447 0.2121 0.6061 0.223 Uiso 1 1 calc R U . . .
C1 C 0.0459(6) 0.3547(10) 0.5564(3) 0.096(3) Uani 1 1 d . . . . .
C2 C 0.3343(6) 0.3710(14) 0.6110(2) 0.119(4) Uani 1 1 d . . . . .
C11 C -0.0348(5) 0.3087(7) 0.5411(2) 0.079(3) Uani 1 1 d . . . . .
C12 C -0.0862(5) 0.2763(7) 0.5564(2) 0.078(3) Uani 1 1 d . . . . .
C13 C -0.1592(5) 0.2316(7) 0.5431(2) 0.081(3) Uani 1 1 d . . . . .
H5 H -0.1921 0.2098 0.5538 0.097 Uiso 1 1 calc R U . . .
C14 C -0.1848(6) 0.2180(9) 0.5149(3) 0.101(3) Uani 1 1 d . . . . .
H6 H -0.2357 0.1891 0.5058 0.121 Uiso 1 1 calc R U . . .
C15 C -0.1345(5) 0.2477(8) 0.4993(2) 0.092(3) Uani 1 1 d . . . . .
H7 H -0.1513 0.2370 0.4797 0.110 Uiso 1 1 calc R U . . .
C16 C -0.0617(5) 0.2918(8) 0.5122(2) 0.077(2) Uani 1 1 d . . . . .
C17 C -0.0973(5) 0.2527(8) 0.6049(2) 0.084(3) Uani 1 1 d . . . . .
C18 C -0.0735(5) 0.3202(7) 0.6335(2) 0.076(2) Uani 1 1 d . . . . .
C21 C 0.3821(7) 0.2655(11) 0.6250(2) 0.108(3) Uani 1 1 d . . . . .
C22 C 0.4584(6) 0.2766(10) 0.6410(2) 0.091(3) Uani 1 1 d . . . . .
C23 C 0.5014(7) 0.1785(10) 0.6537(3) 0.136(5) Uani 1 1 d . . . . .
H8 H 0.5534 0.1866 0.6656 0.163 Uiso 1 1 calc R U . . .
C24 C 0.4654(10) 0.0681(11) 0.6485(4) 0.162(6) Uani 1 1 d . . . . .
H9 H 0.4966 0.0015 0.6563 0.194 Uiso 1 1 calc R U . . .
C25 C 0.3946(11) 0.0471(16) 0.6342(4) 0.160(6) Uani 1 1 d . U . . .
H10 H 0.3727 -0.0300 0.6323 0.192 Uiso 1 1 calc R U . . .
C26 C 0.3536(8) 0.1427(15) 0.6220(3) 0.139(5) Uani 1 1 d . U . . .
C27 C 0.5580(5) 0.4251(7) 0.6642(2) 0.073(2) Uani 1 1 d . . . . .
C28 C 0.5792(4) 0.5590(7) 0.6636(2) 0.074(2) Uani 1 1 d . . . . .
C31 C -0.1182(5) 0.5976(8) 0.5217(2) 0.096(3) Uani 1 1 d . . . . .
H13 H -0.1389 0.6619 0.5081 0.116 Uiso 1 1 calc R U . . .
H14 H -0.1126 0.5261 0.5111 0.116 Uiso 1 1 calc R U . . .
C32 C -0.1761(6) 0.5721(9) 0.5372(2) 0.106(3) Uani 1 1 d . . . . .
H15 H -0.1529 0.5114 0.5515 0.128 Uiso 1 1 calc R U . . .
H16 H -0.1819 0.6452 0.5472 0.128 Uiso 1 1 calc R U . . .
C33 C -0.2552(6) 0.5313(9) 0.5211(3) 0.122(4) Uani 1 1 d . . . . .
H19 H -0.2860 0.5185 0.5338 0.146 Uiso 1 1 calc R U . . .
H18 H -0.2806 0.5914 0.5073 0.146 Uiso 1 1 calc R U . . .
H17 H -0.2515 0.4570 0.5116 0.146 Uiso 1 1 calc R U . . .
C37 C 0.0297(7) 0.6442(9) 0.5299(3) 0.098(3) Uani 1 1 d . . . . .
C38 C -0.0382(6) 0.6335(9) 0.5410(2) 0.110(3) Uani 1 1 d . . . . .
H11 H -0.0443 0.7109 0.5493 0.132 Uiso 1 1 calc R U . . .
H12 H -0.0236 0.5755 0.5565 0.132 Uiso 1 1 calc R U . . .
C41 C 0.0950(8) -0.002(3) 0.5614(5) 0.43(2) Uani 1 1 d D U . . .
H22 H 0.1210 -0.0801 0.5635 0.511 Uiso 1 1 calc R U . . .
H23 H 0.0978 0.0357 0.5440 0.511 Uiso 1 1 calc R U . . .
C42 C 0.0118(7) -0.0146(14) 0.5611(4) 0.222(10) Uani 1 1 d D U . . .
H24 H -0.0072 0.0582 0.5679 0.266 Uiso 1 1 calc R U . . .
H25 H 0.0051 -0.0828 0.5725 0.266 Uiso 1 1 calc R U . . .
C43 C -0.0288(11) -0.035(2) 0.5304(4) 0.321(13) Uani 1 1 d D U . . .
H26 H -0.0848 -0.0448 0.5273 0.385 Uiso 1 1 calc R U . . .
H28 H -0.0201 0.0333 0.5198 0.385 Uiso 1 1 calc R U . . .
H27 H -0.0079 -0.1064 0.5244 0.385 Uiso 1 1 calc R U . . .
C47 C 0.2191(9) 0.050(2) 0.5937(5) 0.244(9) Uani 1 1 d D U . . .
C48 C 0.1316(8) 0.0745(15) 0.5860(3) 0.224(7) Uani 1 1 d D U . . .
H20 H 0.1120 0.0539 0.6016 0.269 Uiso 1 1 calc R U . . .
H21 H 0.1203 0.1589 0.5812 0.269 Uiso 1 1 calc R U . . .
C51 C 0.2671(13) 0.618(2) 0.6318(6) 0.196(13) Uani 0.5 1 d D U P A 1
H107 H 0.3094 0.5806 0.6260 0.235 Uiso 0.5 1 calc R U P A 1
H108 H 0.2737 0.5931 0.6512 0.235 Uiso 0.5 1 calc R U P A 1
C52 C 0.2746(12) 0.7496(19) 0.6308(6) 0.128(8) Uani 0.5 1 d D U P A 1
H110 H 0.3216 0.7762 0.6457 0.153 Uiso 0.5 1 calc R U P A 1
H109 H 0.2798 0.7741 0.6126 0.153 Uiso 0.5 1 calc R U P A 1
C53 C 0.1436(15) 0.749(3) 0.6129(6) 0.180(13) Uani 0.5 1 d D U P A 1
H111 H 0.1552 0.7658 0.5953 0.216 Uiso 0.5 1 calc R U P A 1
H112 H 0.0965 0.7952 0.6120 0.216 Uiso 0.5 1 calc R U P A 1
C54 C 0.1193(18) 0.622(3) 0.6111(12) 0.17(2) Uani 0.5 1 d D U P A 1
H114 H 0.0989 0.5984 0.6265 0.209 Uiso 0.5 1 calc R U P A 1
H113 H 0.0811 0.6016 0.5929 0.209 Uiso 0.5 1 calc R U P A 1
C61 C 0.1303(12) 0.7657(18) 0.6827(5) 0.126(10) Uani 0.5 1 d D U P D 1
H115 H 0.1779 0.7674 0.6769 0.151 Uiso 0.5 1 calc R U P D 1
H116 H 0.1130 0.6830 0.6834 0.151 Uiso 0.5 1 calc R U P D 1
C62 C 0.1399(11) 0.8285(19) 0.7085(4) 0.132(9) Uani 0.5 1 d D U P D 1
H118 H 0.0932 0.8163 0.7144 0.158 Uiso 0.5 1 calc R U P D 1
H117 H 0.1852 0.7955 0.7231 0.158 Uiso 0.5 1 calc R U P D 1
C63 C 0.0927(13) 0.995(2) 0.6847(5) 0.143(10) Uani 0.5 1 d D . P D 1
H119 H 0.0998 1.0822 0.6852 0.172 Uiso 0.5 1 calc R U P D 1
H120 H 0.0415 0.9781 0.6872 0.172 Uiso 0.5 1 calc R U P D 1
C64 C 0.0946(16) 0.9500(15) 0.6587(5) 0.124(9) Uani 0.5 1 d D . P D 1
H122 H 0.0571 0.9885 0.6424 0.148 Uiso 0.5 1 calc R U P D 1
H121 H 0.1474 0.9483 0.6567 0.148 Uiso 0.5 1 calc R U P D 1
C71 C 0.3607(12) 0.156(3) 0.5469(5) 0.193(13) Uani 0.5 1 d D U P E 2
H123 H 0.3637 0.0937 0.5610 0.231 Uiso 0.5 1 calc R U P E 2
H124 H 0.3986 0.2190 0.5553 0.231 Uiso 0.5 1 calc R U P E 2
C72 C 0.3755(10) 0.105(2) 0.5213(6) 0.112(8) Uani 0.5 1 d D U P E 2
H126 H 0.3956 0.1715 0.5128 0.135 Uiso 0.5 1 calc R U P E 2
H125 H 0.4196 0.0494 0.5285 0.135 Uiso 0.5 1 calc R U P E 2
C73 C 0.2466(15) 0.0835(19) 0.4954(6) 0.137(10) Uani 0.5 1 d D U P E 2
H127 H 0.2099 0.0205 0.4858 0.165 Uiso 0.5 1 calc R U P E 2
H128 H 0.2356 0.1547 0.4833 0.165 Uiso 0.5 1 calc R U P E 2
C74 C 0.2342(12) 0.111(2) 0.5222(7) 0.145(13) Uani 0.5 1 d D U P E 2
H130 H 0.1792 0.1339 0.5188 0.175 Uiso 0.5 1 calc R U P E 2
H129 H 0.2446 0.0395 0.5340 0.175 Uiso 0.5 1 calc R U P E 2
C81 C 0.6338(12) 0.2416(18) 0.6027(4) 0.233(11) Uani 1 1 d D U . . .
H132 H 0.5890 0.2837 0.6057 0.279 Uiso 1 1 calc R U . . .
H131 H 0.6781 0.2489 0.6200 0.279 Uiso 1 1 calc R U . . .
C82 C 0.6140(15) 0.1182(18) 0.5981(4) 0.267(11) Uani 1 1 d D U . . .
H133 H 0.6594 0.0709 0.6089 0.320 Uiso 1 1 calc R U . . .
H134 H 0.5709 0.1012 0.6058 0.320 Uiso 1 1 calc R U . . .
C83 C 0.6306(17) 0.160(2) 0.5555(5) 0.309(14) Uani 1 1 d D U . . .
H135 H 0.6134 0.1303 0.5361 0.371 Uiso 1 1 calc R U . . .
H136 H 0.6865 0.1393 0.5630 0.371 Uiso 1 1 calc R U . . .
C84 C 0.630(2) 0.291(2) 0.5526(5) 0.37(2) Uani 1 1 d D U . . .
H137 H 0.6691 0.3226 0.5444 0.445 Uiso 1 1 calc R U . . .
H138 H 0.5777 0.3252 0.5433 0.445 Uiso 1 1 calc R U . . .
C111 C 0.0145(5) 0.3152(7) 0.6488(2) 0.073(2) Uani 1 1 d . . . . .
C112 C 0.0404(5) 0.3587(7) 0.6758(2) 0.085(3) Uani 1 1 d . . . . .
H29 H 0.0030 0.3893 0.6837 0.102 Uiso 1 1 calc R U . . .
C113 C 0.1178(5) 0.3598(8) 0.6918(2) 0.086(3) Uani 1 1 d . . . . .
H30 H 0.1321 0.3910 0.7102 0.103 Uiso 1 1 calc R U . . .
C114 C 0.1741(5) 0.3165(9) 0.6815(2) 0.086(3) Uani 1 1 d . . . . .
C115 C 0.1498(6) 0.2691(9) 0.6553(3) 0.104(3) Uani 1 1 d . . . . .
H31 H 0.1871 0.2352 0.6477 0.125 Uiso 1 1 calc R U . . .
C116 C 0.0711(6) 0.2696(8) 0.6393(2) 0.090(3) Uani 1 1 d . . . . .
H32 H 0.0567 0.2367 0.6211 0.108 Uiso 1 1 calc R U . . .
C117 C 0.2603(5) 0.3142(9) 0.6986(2) 0.098(3) Uani 1 1 d D . . . .
C118 C 0.3135(6) 0.2765(18) 0.6835(3) 0.212(9) Uani 1 1 d . . . . .
H33 H 0.3044 0.3245 0.6666 0.255 Uiso 1 1 calc R U . . .
H34 H 0.3674 0.2870 0.6954 0.255 Uiso 1 1 calc R U . . .
H35 H 0.3043 0.1929 0.6783 0.255 Uiso 1 1 calc R U . . .
C119 C 0.2705(6) 0.2440(12) 0.7252(3) 0.140(5) Uani 1 1 d . . . . .
H36 H 0.2337 0.2727 0.7345 0.168 Uiso 1 1 calc R U . . .
H38 H 0.2607 0.1600 0.7207 0.168 Uiso 1 1 calc R U . . .
H37 H 0.3238 0.2541 0.7377 0.168 Uiso 1 1 calc R U . . .
C120 C 0.2843(7) 0.4398(11) 0.7089(4) 0.212(9) Uani 1 1 d D . . . .
H39 H 0.2501 0.4689 0.7193 0.255 Uiso 1 1 calc R U . . .
H40 H 0.3382 0.4394 0.7212 0.255 Uiso 1 1 calc R U . . .
H41 H 0.2799 0.4915 0.6929 0.255 Uiso 1 1 calc R U . . .
C121 C -0.1015(5) 0.4494(7) 0.6257(2) 0.077(2) Uani 1 1 d . . . . .
C122 C -0.0552(5) 0.5474(8) 0.6327(2) 0.084(3) Uani 1 1 d . . . . .
H42 H -0.0021 0.5375 0.6433 0.101 Uiso 1 1 calc R U . . .
C123 C -0.0827(5) 0.6600(8) 0.6249(2) 0.090(3) Uani 1 1 d . . . . .
H43 H -0.0480 0.7255 0.6290 0.108 Uiso 1 1 calc R U . . .
C124 C -0.1619(5) 0.6780(7) 0.61087(19) 0.077(2) Uani 1 1 d . . . . .
C125 C -0.2082(5) 0.5778(8) 0.60290(18) 0.077(2) Uani 1 1 d . . . . .
H44 H -0.2611 0.5862 0.5919 0.093 Uiso 1 1 calc R U . . .
C126 C -0.1790(5) 0.4688(7) 0.61061(19) 0.081(3) Uani 1 1 d . . . . .
H45 H -0.2129 0.4026 0.6055 0.097 Uiso 1 1 calc R U . . .
C127 C -0.1913(6) 0.8042(7) 0.6028(2) 0.085(3) Uani 1 1 d . . . . .
C128 C -0.1432(7) 0.8698(10) 0.5882(3) 0.154(5) Uani 1 1 d . . . . .
H46 H -0.1442 0.8273 0.5712 0.185 Uiso 1 1 calc R U . . .
H48 H -0.1646 0.9494 0.5834 0.185 Uiso 1 1 calc R U . . .
H47 H -0.0895 0.8756 0.6005 0.185 Uiso 1 1 calc R U . . .
C129 C -0.1880(8) 0.8701(9) 0.6276(3) 0.156(5) Uani 1 1 d . . . . .
H51 H -0.1345 0.8697 0.6403 0.187 Uiso 1 1 calc R U . . .
H50 H -0.2044 0.9518 0.6225 0.187 Uiso 1 1 calc R U . . .
H49 H -0.2227 0.8336 0.6368 0.187 Uiso 1 1 calc R U . . .
C130 C -0.2731(7) 0.8067(9) 0.5841(3) 0.193(8) Uani 1 1 d . . . . .
H53 H -0.2768 0.7623 0.5670 0.232 Uiso 1 1 calc R U . . .
H52 H -0.3072 0.7706 0.5936 0.232 Uiso 1 1 calc R U . . .
H54 H -0.2890 0.8889 0.5793 0.232 Uiso 1 1 calc R U . . .
C131 C -0.1175(4) 0.2610(7) 0.65199(19) 0.070(2) Uani 1 1 d . . . . .
C132 C -0.0984(5) 0.1448(7) 0.6603(2) 0.091(3) Uani 1 1 d . . . . .
H55 H -0.0609 0.1043 0.6540 0.109 Uiso 1 1 calc R U . . .
C133 C -0.1326(5) 0.0875(8) 0.6774(2) 0.082(3) Uani 1 1 d . . . . .
H56 H -0.1183 0.0078 0.6825 0.099 Uiso 1 1 calc R U . . .
C134 C -0.1867(4) 0.1406(7) 0.68758(17) 0.065(2) Uani 1 1 d . . . . .
C135 C -0.2039(5) 0.2582(8) 0.6791(2) 0.081(3) Uani 1 1 d . . . . .
H57 H -0.2409 0.2999 0.6854 0.097 Uiso 1 1 calc R U . . .
C136 C -0.1692(4) 0.3158(7) 0.66195(19) 0.073(2) Uani 1 1 d . . . . .
H58 H -0.1822 0.3961 0.6571 0.087 Uiso 1 1 calc R U . . .
C137 C -0.2238(5) 0.0790(8) 0.7057(2) 0.086(3) Uani 1 1 d . . . . .
C138 C -0.1791(9) -0.0206(16) 0.7210(4) 0.256(11) Uani 1 1 d . U . . .
H59 H -0.1716 -0.0793 0.7077 0.308 Uiso 1 1 calc R U . . .
H60 H -0.1283 0.0075 0.7328 0.308 Uiso 1 1 calc R U . . .
H61 H -0.2073 -0.0568 0.7326 0.308 Uiso 1 1 calc R U . . .
C139 C -0.2266(15) 0.1506(14) 0.7293(4) 0.293(14) Uani 1 1 d . U . . .
H62 H -0.2556 0.2236 0.7225 0.352 Uiso 1 1 calc R U . . .
H63 H -0.2525 0.1062 0.7405 0.352 Uiso 1 1 calc R U . . .
H64 H -0.1735 0.1705 0.7407 0.352 Uiso 1 1 calc R U . . .
C140 C -0.3020(8) 0.0397(18) 0.6895(3) 0.238(10) Uani 1 1 d . U . . .
H67 H -0.2989 -0.0084 0.6737 0.286 Uiso 1 1 calc R U . . .
H65 H -0.3244 -0.0076 0.7014 0.286 Uiso 1 1 calc R U . . .
H66 H -0.3351 0.1089 0.6825 0.286 Uiso 1 1 calc R U . . .
C211 C 0.5572(4) 0.6006(7) 0.6331(2) 0.074(2) Uani 1 1 d . . . . .
C212 C 0.5852(5) 0.5354(9) 0.6144(2) 0.093(3) Uani 1 1 d . . . . .
H68 H 0.6187 0.4696 0.6208 0.112 Uiso 1 1 calc R U . . .
C213 C 0.5629(6) 0.5690(10) 0.5859(2) 0.095(3) Uani 1 1 d . . . . .
H69 H 0.5829 0.5256 0.5735 0.114 Uiso 1 1 calc R U . . .
C214 C 0.5142(6) 0.6603(11) 0.5757(3) 0.101(3) Uani 1 1 d . . . . .
C215 C 0.4852(6) 0.7220(11) 0.5946(3) 0.115(4) Uani 1 1 d . . . . .
H70 H 0.4494 0.7849 0.5880 0.137 Uiso 1 1 calc R U . . .
C216 C 0.5076(5) 0.6932(9) 0.6221(2) 0.096(3) Uani 1 1 d . . . . .
H71 H 0.4881 0.7390 0.6343 0.115 Uiso 1 1 calc R U . . .
C217 C 0.4880(9) 0.6937(14) 0.5444(3) 0.154(5) Uani 1 1 d . . . . .
C218 C 0.4096(10) 0.665(3) 0.5306(3) 0.358(18) Uani 1 1 d . U . . .
H72 H 0.4000 0.5825 0.5343 0.430 Uiso 1 1 calc R U . . .
H74 H 0.3757 0.7168 0.5374 0.430 Uiso 1 1 calc R U . . .
H73 H 0.3986 0.6769 0.5105 0.430 Uiso 1 1 calc R U . . .
C219 C 0.5432(14) 0.6224(17) 0.5293(3) 0.264(11) Uani 1 1 d . U . . .
H76 H 0.5980 0.6415 0.5388 0.316 Uiso 1 1 calc R U . . .
H75 H 0.5352 0.5370 0.5305 0.316 Uiso 1 1 calc R U . . .
H77 H 0.5295 0.6461 0.5097 0.316 Uiso 1 1 calc R U . . .
C220 C 0.5094(12) 0.8164(15) 0.5404(3) 0.239(9) Uani 1 1 d . U . . .
H78 H 0.5645 0.8290 0.5506 0.287 Uiso 1 1 calc R U . . .
H80 H 0.5004 0.8309 0.5205 0.287 Uiso 1 1 calc R U . . .
H79 H 0.4776 0.8709 0.5474 0.287 Uiso 1 1 calc R U . . .
C221 C 0.5356(4) 0.6326(7) 0.67995(18) 0.071(2) Uani 1 1 d . . . . .
C222 C 0.5633(5) 0.7458(9) 0.6900(2) 0.101(3) Uani 1 1 d . . . . .
H81 H 0.6082 0.7758 0.6863 0.121 Uiso 1 1 calc R U . . .
C223 C 0.5286(5) 0.8122(8) 0.7044(2) 0.095(3) Uani 1 1 d . . . . .
H82 H 0.5492 0.8886 0.7102 0.114 Uiso 1 1 calc R U . . .
C224 C 0.4654(5) 0.7765(8) 0.7114(2) 0.081(3) Uani 1 1 d . . . . .
C225 C 0.4403(5) 0.6659(9) 0.7016(2) 0.099(3) Uani 1 1 d . . . . .
H83 H 0.3959 0.6361 0.7057 0.119 Uiso 1 1 calc R U . . .
C226 C 0.4723(4) 0.5960(8) 0.6868(2) 0.080(3) Uani 1 1 d . . . . .
H84 H 0.4506 0.5201 0.6810 0.096 Uiso 1 1 calc R U . . .
C227 C 0.4288(5) 0.8490(10) 0.7283(3) 0.112(3) Uani 1 1 d . U . . .
C228 C 0.4585(10) 0.9774(13) 0.7334(4) 0.226(8) Uani 1 1 d . U . . .
H86 H 0.5155 0.9778 0.7392 0.271 Uiso 1 1 calc R U . . .
H85 H 0.4381 1.0231 0.7162 0.271 Uiso 1 1 calc R U . . .
H87 H 0.4407 1.0130 0.7481 0.271 Uiso 1 1 calc R U . . .
C229 C 0.3481(7) 0.8518(18) 0.7202(4) 0.296(10) Uani 1 1 d . U . . .
H88 H 0.3281 0.8823 0.7012 0.356 Uiso 1 1 calc R U . . .
H90 H 0.3281 0.7716 0.7209 0.356 Uiso 1 1 calc R U . . .
H89 H 0.3311 0.9034 0.7329 0.356 Uiso 1 1 calc R U . . .
C230 C 0.4512(14) 0.8034(19) 0.7562(4) 0.274(9) Uani 1 1 d . U . . .
H92 H 0.5080 0.7986 0.7635 0.329 Uiso 1 1 calc R U . . .
H91 H 0.4319 0.8560 0.7680 0.329 Uiso 1 1 calc R U . . .
H93 H 0.4289 0.7243 0.7561 0.329 Uiso 1 1 calc R U . . .
C231 C 0.6673(4) 0.5730(7) 0.6788(2) 0.071(2) Uani 1 1 d . . . . .
C232 C 0.7207(4) 0.6124(7) 0.66665(19) 0.072(2) Uani 1 1 d . . . . .
H94 H 0.7032 0.6316 0.6474 0.086 Uiso 1 1 calc R U . . .
C233 C 0.8002(5) 0.6258(7) 0.6813(2) 0.076(2) Uani 1 1 d . . . . .
H95 H 0.8350 0.6574 0.6723 0.091 Uiso 1 1 calc R U . . .
C234 C 0.8268(4) 0.5917(7) 0.7091(2) 0.080(3) Uani 1 1 d . . . . .
C235 C 0.7742(4) 0.5535(7) 0.72138(19) 0.078(3) Uani 1 1 d . . . . .
H96 H 0.7917 0.5329 0.7406 0.094 Uiso 1 1 calc R U . . .
C236 C 0.6964(5) 0.5439(7) 0.7068(2) 0.082(3) Uani 1 1 d . . . . .
H97 H 0.6615 0.5165 0.7163 0.099 Uiso 1 1 calc R U . . .
C237 C 0.9135(5) 0.5962(8) 0.7264(2) 0.087(3) Uani 1 1 d . . . . .
C238 C 0.9617(5) 0.6474(10) 0.7092(2) 0.121(4) Uani 1 1 d . . . . .
H99 H 0.9554 0.5982 0.6927 0.145 Uiso 1 1 calc R U . . .
H98 H 0.9441 0.7281 0.7035 0.145 Uiso 1 1 calc R U . . .
H100 H 1.0167 0.6488 0.7205 0.145 Uiso 1 1 calc R U . . .
C239 C 0.9240(5) 0.6743(9) 0.7523(2) 0.111(4) Uani 1 1 d . . . . .
H103 H 0.8931 0.6419 0.7635 0.133 Uiso 1 1 calc R U . . .
H102 H 0.9790 0.6757 0.7634 0.133 Uiso 1 1 calc R U . . .
H101 H 0.9065 0.7549 0.7464 0.133 Uiso 1 1 calc R U . . .
C240 C 0.9409(5) 0.4671(8) 0.7352(2) 0.105(3) Uani 1 1 d . . . . .
H105 H 0.9099 0.4340 0.7463 0.126 Uiso 1 1 calc R U . . .
H104 H 0.9342 0.4185 0.7186 0.126 Uiso 1 1 calc R U . . .
H106 H 0.9960 0.4678 0.7464 0.126 Uiso 1 1 calc R U . . .


_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
Ca1 O21 2.105(10) . ?
Ca1 O11 2.359(8) . ?
Ca1 O51 2.389(18) . ?
Ca1 O5 2.406(12) . ?
Ca1 O6 2.407(17) . ?
Ca1 O3 2.566(10) . ?
Ca1 O12 2.644(8) . ?
Ca1 C1 2.851(10) . ?
Ca1 C2 2.940(13) . ?
Ca1 O22 3.101(8) . ?
Ca1 C54 3.15(4) . ?
Ca2 O3 2.119(10) . ?
Ca2 O7 2.327(12) . ?
Ca2 O12 2.340(7) . ?
Ca2 O9 2.40(3) . ?
Ca2 O8 2.474(17) . ?
Ca2 O21 2.568(11) . ?
Ca2 O11 2.751(9) . ?
Ca2 C1 2.862(11) . ?
Ca2 C37 3.162(14) . ?
O1 C17 1.189(9) . ?
O2 C27 1.191(9) . ?
O3 C37 1.207(12) . ?
O4 C47 1.35(2) . ?
O11 C1 1.267(11) . ?
O12 C1 1.263(12) . ?
O21 C2 1.297(12) . ?
O22 C2 1.248(13) . ?
O51 C54 1.42(2) . ?
O51 C51 1.424(18) . ?
O52 C52 1.439(16) . ?
O52 C53 1.445(17) . ?
O61 C64 1.403(16) . ?
O61 C61 1.439(16) . ?
O62 C62 1.332(15) . ?
O62 C63 1.373(15) . ?
O71 C74 1.403(18) . ?
O71 C71 1.449(17) . ?
O72 C73 1.390(18) . ?
O72 C72 1.396(19) . ?
O81 C81 1.342(16) . ?
O81 C84 1.419(17) . ?
O82 C82 1.393(14) . ?
O82 C83 1.493(15) . ?
N1 C12 1.405(11) . ?
N1 C17 1.419(11) . ?
N1 H1 0.8800 . ?
N2 C27 1.352(10) . ?
N2 C22 1.411(11) . ?
N2 H2 0.8800 . ?
N3 C37 1.352(12) 3_566 ?
N3 C16 1.430(11) . ?
N3 H3 0.8800 . ?
N4 C47 1.40(2) . ?
N4 C26 1.501(17) . ?
N4 H4 0.8800 . ?
C1 C11 1.516(12) . ?
C2 C21 1.513(16) . ?
C11 C16 1.400(12) . ?
C11 C12 1.425(12) . ?
C12 C13 1.377(11) . ?
C13 C14 1.364(12) . ?
C13 H5 0.9500 . ?
C14 C15 1.412(13) . ?
C14 H6 0.9500 . ?
C15 C16 1.369(11) . ?
C15 H7 0.9500 . ?
C17 C18 1.569(12) . ?
C18 C111 1.539(11) . ?
C18 C131 1.552(11) . ?
C18 C121 1.556(11) . ?
C21 C22 1.371(13) . ?
C21 C26 1.472(17) . ?
C22 C23 1.392(14) . ?
C23 C24 1.394(15) . ?
C23 H8 0.9500 . ?
C24 C25 1.282(18) . ?
C24 H9 0.9500 . ?
C25 C26 1.346(19) . ?
C25 H10 0.9500 . ?
C27 C28 1.564(11) . ?
C28 C211 1.535(12) . ?
C28 C231 1.547(11) . ?
C28 C221 1.550(11) . ?
C31 C32 1.517(12) . ?
C31 C38 1.529(12) . ?
C31 H13 0.9900 . ?
C31 H14 0.9900 . ?
C32 C33 1.482(12) . ?
C32 H15 0.9900 . ?
C32 H16 0.9900 . ?
C33 H19 0.9800 . ?
C33 H18 0.9800 . ?
C33 H17 0.9800 . ?
C37 N3 1.351(12) 3_566 ?
C37 C38 1.501(14) . ?
C38 H11 0.9900 . ?
C38 H12 0.9900 . ?
C41 C48 1.486(9) . ?
C41 C42 1.506(9) . ?
C41 H22 0.9900 . ?
C41 H23 0.9900 . ?
C42 C43 1.513(10) . ?
C42 H24 0.9900 . ?
C42 H25 0.9900 . ?
C43 H26 0.9800 . ?
C43 H28 0.9800 . ?
C43 H27 0.9800 . ?
C47 C48 1.530(10) . ?
C48 H20 0.9900 . ?
C48 H21 0.9900 . ?
C51 C52 1.501(17) . ?
C51 H107 0.9900 . ?
C51 H108 0.9900 . ?
C52 H110 0.9900 . ?
C52 H109 0.9900 . ?
C53 C54 1.50(2) . ?
C53 H111 0.9900 . ?
C53 H112 0.9900 . ?
C54 H114 0.9900 . ?
C54 H113 0.9900 . ?
C61 C62 1.443(18) . ?
C61 H115 0.9900 . ?
C61 H116 0.9900 . ?
C62 H118 0.9900 . ?
C62 H117 0.9900 . ?
C63 C64 1.421(18) . ?
C63 H119 0.9900 . ?
C63 H120 0.9900 . ?
C64 H122 0.9900 . ?
C64 H121 0.9900 . ?
C71 C72 1.510(18) . ?
C71 H123 0.9900 . ?
C71 H124 0.9900 . ?
C72 H126 0.9900 . ?
C72 H125 0.9900 . ?
C73 C74 1.470(18) . ?
C73 H127 0.9900 . ?
C73 H128 0.9900 . ?
C74 H130 0.9900 . ?
C74 H129 0.9900 . ?
C81 C82 1.441(16) . ?
C81 H132 0.9900 . ?
C81 H131 0.9900 . ?
C82 H133 0.9900 . ?
C82 H134 0.9900 . ?
C83 C84 1.495(18) . ?
C83 H135 0.9900 . ?
C83 H136 0.9900 . ?
C84 H137 0.9900 . ?
C84 H138 0.9900 . ?
C111 C116 1.358(11) . ?
C111 C112 1.385(12) . ?
C112 C113 1.382(11) . ?
C112 H29 0.9500 . ?
C113 C114 1.367(12) . ?
C113 H30 0.9500 . ?
C114 C115 1.369(13) . ?
C114 C117 1.530(13) . ?
C115 C116 1.401(13) . ?
C115 H31 0.9500 . ?
C116 H32 0.9500 . ?
C117 C118 1.465(14) . ?
C117 C119 1.519(14) . ?
C117 C120 1.527(13) . ?
C118 H33 0.9800 . ?
C118 H34 0.9800 . ?
C118 H35 0.9800 . ?
C119 H36 0.9800 . ?
C119 H38 0.9800 . ?
C119 H37 0.9800 . ?
C120 H39 0.9800 . ?
C120 H40 0.9800 . ?
C120 H41 0.9800 . ?
C121 C122 1.367(11) . ?
C121 C126 1.388(11) . ?
C122 C123 1.380(11) . ?
C122 H42 0.9500 . ?
C123 C124 1.401(11) . ?
C123 H43 0.9500 . ?
C124 C125 1.391(10) . ?
C124 C127 1.532(11) . ?
C125 C126 1.349(11) . ?
C125 H44 0.9500 . ?
C126 H45 0.9500 . ?
C127 C129 1.438(14) . ?
C127 C130 1.487(13) . ?
C127 C128 1.497(13) . ?
C128 H46 0.9800 . ?
C128 H48 0.9800 . ?
C128 H47 0.9800 . ?
C129 H51 0.9800 . ?
C129 H50 0.9800 . ?
C129 H49 0.9800 . ?
C130 H53 0.9800 . ?
C130 H52 0.9800 . ?
C130 H54 0.9800 . ?
C131 C136 1.341(10) . ?
C131 C132 1.389(11) . ?
C132 C133 1.370(11) . ?
C132 H55 0.9500 . ?
C133 C134 1.375(11) . ?
C133 H56 0.9500 . ?
C134 C135 1.402(11) . ?
C134 C137 1.464(12) . ?
C135 C136 1.376(11) . ?
C135 H57 0.9500 . ?
C136 H58 0.9500 . ?
C137 C139 1.452(17) . ?
C137 C138 1.459(13) . ?
C137 C140 1.466(15) . ?
C138 H59 0.9800 . ?
C138 H60 0.9800 . ?
C138 H61 0.9800 . ?
C139 H62 0.9800 . ?
C139 H63 0.9800 . ?
C139 H64 0.9800 . ?
C140 H67 0.9800 . ?
C140 H65 0.9800 . ?
C140 H66 0.9800 . ?
C211 C216 1.378(11) . ?
C211 C212 1.410(12) . ?
C212 C213 1.420(13) . ?
C212 H68 0.9500 . ?
C213 C214 1.350(13) . ?
C213 H69 0.9500 . ?
C214 C215 1.405(15) . ?
C214 C217 1.547(17) . ?
C215 C216 1.362(14) . ?
C215 H70 0.9500 . ?
C216 H71 0.9500 . ?
C217 C218 1.408(18) . ?
C217 C220 1.471(18) . ?
C217 C219 1.64(2) . ?
C218 H72 0.9800 . ?
C218 H74 0.9800 . ?
C218 H73 0.9800 . ?
C219 H76 0.9800 . ?
C219 H75 0.9800 . ?
C219 H77 0.9800 . ?
C220 H78 0.9800 . ?
C220 H80 0.9800 . ?
C220 H79 0.9800 . ?
C221 C226 1.358(10) . ?
C221 C222 1.409(12) . ?
C222 C223 1.330(12) . ?
C222 H81 0.9500 . ?
C223 C224 1.357(11) . ?
C223 H82 0.9500 . ?
C224 C225 1.369(12) . ?
C224 C227 1.478(12) . ?
C225 C226 1.335(11) . ?
C225 H83 0.9500 . ?
C226 H84 0.9500 . ?
C227 C229 1.387(14) . ?
C227 C230 1.43(2) . ?
C227 C228 1.541(16) . ?
C228 H86 0.9800 . ?
C228 H85 0.9800 . ?
C228 H87 0.9800 . ?
C229 H88 0.9800 . ?
C229 H90 0.9800 . ?
C229 H89 0.9800 . ?
C230 H92 0.9800 . ?
C230 H91 0.9800 . ?
C230 H93 0.9800 . ?
C231 C232 1.367(10) . ?
C231 C236 1.388(12) . ?
C232 C233 1.405(11) . ?
C232 H94 0.9500 . ?
C233 C234 1.390(12) . ?
C233 H95 0.9500 . ?
C234 C235 1.356(11) . ?
C234 C237 1.540(11) . ?
C235 C236 1.375(11) . ?
C235 H96 0.9500 . ?
C236 H97 0.9500 . ?
C237 C238 1.519(13) . ?
C237 C239 1.539(13) . ?
C237 C240 1.561(12) . ?
C238 H99 0.9800 . ?
C238 H98 0.9800 . ?
C238 H100 0.9800 . ?
C239 H103 0.9800 . ?
C239 H102 0.9800 . ?
C239 H101 0.9800 . ?
C240 H105 0.9800 . ?
C240 H104 0.9800 . ?
C240 H106 0.9800 . ?

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
O21 Ca1 O11 105.2(3) . . ?
O21 Ca1 O51 73.2(5) . . ?
O11 Ca1 O51 129.5(5) . . ?
O21 Ca1 O5 99.3(4) . . ?
O11 Ca1 O5 141.8(5) . . ?
O51 Ca1 O5 85.3(6) . . ?
O21 Ca1 O6 88.6(5) . . ?
O11 Ca1 O6 78.3(4) . . ?
O51 Ca1 O6 149.5(6) . . ?
O5 Ca1 O6 73.5(5) . . ?
O21 Ca1 O3 160.7(4) . . ?
O11 Ca1 O3 82.0(3) . . ?
O51 Ca1 O3 88.4(5) . . ?
O5 Ca1 O3 84.3(4) . . ?
O6 Ca1 O3 110.5(5) . . ?
O21 Ca1 O12 92.7(3) . . ?
O11 Ca1 O12 52.0(2) . . ?
O51 Ca1 O12 77.6(5) . . ?
O5 Ca1 O12 155.3(4) . . ?
O6 Ca1 O12 128.7(4) . . ?
O3 Ca1 O12 77.5(2) . . ?
O21 Ca1 C1 102.7(3) . . ?
O11 Ca1 C1 26.0(3) . . ?
O51 Ca1 C1 103.7(5) . . ?
O5 Ca1 C1 157.8(4) . . ?
O6 Ca1 C1 104.1(5) . . ?
O3 Ca1 C1 75.8(3) . . ?
O12 Ca1 C1 26.2(3) . . ?
O21 Ca1 C2 23.0(3) . . ?
O11 Ca1 C2 118.0(4) . . ?
O51 Ca1 C2 80.4(5) . . ?
O5 Ca1 C2 78.2(4) . . ?
O6 Ca1 C2 74.0(4) . . ?
O3 Ca1 C2 159.8(4) . . ?
O12 Ca1 C2 115.7(3) . . ?
C1 Ca1 C2 123.0(4) . . ?
O21 Ca1 O22 45.3(3) . . ?
O11 Ca1 O22 136.5(3) . . ?
O51 Ca1 O22 78.7(5) . . ?
O5 Ca1 O22 54.6(3) . . ?
O6 Ca1 O22 71.2(4) . . ?
O3 Ca1 O22 137.4(3) . . ?
O12 Ca1 O22 136.4(3) . . ?
C1 Ca1 O22 146.5(3) . . ?
C2 Ca1 O22 23.6(3) . . ?
O21 Ca1 C54 92.7(9) . . ?
O11 Ca1 C54 109.8(7) . . ?
O51 Ca1 C54 25.2(8) . . ?
O5 Ca1 C54 97.6(7) . . ?
O6 Ca1 C54 171.1(7) . . ?
O3 Ca1 C54 68.0(9) . . ?
O12 Ca1 C54 60.1(6) . . ?
C1 Ca1 C54 84.2(7) . . ?
C2 Ca1 C54 104.3(9) . . ?
O22 Ca1 C54 103.7(8) . . ?
O3 Ca2 O7 93.8(4) . . ?
O3 Ca2 O12 93.9(3) . . ?
O7 Ca2 O12 160.6(6) . . ?
O3 Ca2 O9 107.9(12) . . ?
O7 Ca2 O9 84.8(8) . . ?
O12 Ca2 O9 75.9(6) . . ?
O3 Ca2 O8 86.2(5) . . ?
O7 Ca2 O8 74.9(6) . . ?
O12 Ca2 O8 123.4(5) . . ?
O9 Ca2 O8 156.1(8) . . ?
O3 Ca2 O21 158.5(4) . . ?
O7 Ca2 O21 89.8(4) . . ?
O12 Ca2 O21 89.4(3) . . ?
O9 Ca2 O21 93.5(12) . . ?
O8 Ca2 O21 74.3(5) . . ?
O3 Ca2 O11 82.2(3) . . ?
O7 Ca2 O11 148.4(6) . . ?
O12 Ca2 O11 50.6(2) . . ?
O9 Ca2 O11 126.3(6) . . ?
O8 Ca2 O11 73.6(5) . . ?
O21 Ca2 O11 83.7(3) . . ?
O3 Ca2 C1 82.7(3) . . ?
O7 Ca2 C1 173.7(6) . . ?
O12 Ca2 C1 25.7(3) . . ?
O9 Ca2 C1 101.3(6) . . ?
O8 Ca2 C1 99.6(5) . . ?
O21 Ca2 C1 91.6(3) . . ?
O11 Ca2 C1 26.0(3) . . ?
O3 Ca2 C37 13.5(3) . . ?
O7 Ca2 C37 106.0(4) . . ?
O12 Ca2 C37 80.6(3) . . ?
O9 Ca2 C37 102.8(11) . . ?
O8 Ca2 C37 94.9(5) . . ?
O21 Ca2 C37 158.1(3) . . ?
O11 Ca2 C37 74.9(3) . . ?
C1 Ca2 C37 71.1(3) . . ?
C37 O3 Ca2 142.4(7) . . ?
C37 O3 Ca1 143.5(7) . . ?
C1 O11 Ca1 99.2(7) . . ?
C1 O11 Ca2 81.9(7) . . ?
C1 O12 Ca2 100.9(6) . . ?
C1 O12 Ca1 86.0(6) . . ?
C2 O21 Ca1 117.7(8) . . ?
C2 O21 Ca2 126.5(9) . . ?
C2 O22 Ca1 70.9(7) . . ?
C54 O51 C51 128(3) . . ?
C54 O51 Ca1 109(2) . . ?
C51 O51 Ca1 117.9(18) . . ?
C52 O52 C53 103(2) . . ?
C64 O61 C61 114.8(16) . . ?
C62 O62 C63 112.9(14) . . ?
C74 O71 C71 107.1(17) . . ?
C73 O72 C72 112(2) . . ?
C81 O81 C84 137(2) . . ?
C82 O82 C83 106.2(13) . . ?
C12 N1 C17 127.3(7) . . ?
C12 N1 H1 116.4 . . ?
C17 N1 H1 116.4 . . ?
C27 N2 C22 127.2(8) . . ?
C27 N2 H2 116.4 . . ?
C22 N2 H2 116.4 . . ?
C37 N3 C16 126.0(9) 3_566 . ?
C37 N3 H3 117.0 3_566 . ?
C16 N3 H3 117.0 . . ?
C47 N4 C26 129.8(15) . . ?
C47 N4 H4 115.1 . . ?
C26 N4 H4 115.1 . . ?
O12 C1 O11 121.5(9) . . ?
O12 C1 C11 120.8(10) . . ?
O11 C1 C11 117.7(11) . . ?
O12 C1 Ca1 67.7(5) . . ?
O11 C1 Ca1 54.8(5) . . ?
C11 C1 Ca1 165.6(7) . . ?
O12 C1 Ca2 53.4(5) . . ?
O11 C1 Ca2 72.1(5) . . ?
C11 C1 Ca2 156.6(7) . . ?
O22 C2 O21 120.1(13) . . ?
O22 C2 C21 119.9(10) . . ?
O21 C2 C21 119.8(12) . . ?
O22 C2 Ca1 85.4(8) . . ?
O21 C2 Ca1 39.4(6) . . ?
C21 C2 Ca1 151.2(8) . . ?
C16 C11 C12 117.0(8) . . ?
C16 C11 C1 123.0(9) . . ?
C12 C11 C1 120.0(10) . . ?
C13 C12 N1 119.5(9) . . ?
C13 C12 C11 121.1(10) . . ?
N1 C12 C11 119.1(8) . . ?
C14 C13 C12 121.0(10) . . ?
C14 C13 H5 119.5 . . ?
C12 C13 H5 119.5 . . ?
C13 C14 C15 118.9(9) . . ?
C13 C14 H6 120.5 . . ?
C15 C14 H6 120.5 . . ?
C16 C15 C14 120.8(10) . . ?
C16 C15 H7 119.6 . . ?
C14 C15 H7 119.6 . . ?
C15 C16 C11 121.2(9) . . ?
C15 C16 N3 121.5(10) . . ?
C11 C16 N3 117.3(8) . . ?
O1 C17 N1 121.4(9) . . ?
O1 C17 C18 124.8(9) . . ?
N1 C17 C18 113.8(7) . . ?
C111 C18 C131 108.9(7) . . ?
C111 C18 C121 111.5(6) . . ?
C131 C18 C121 111.6(7) . . ?
C111 C18 C17 113.1(7) . . ?
C131 C18 C17 107.3(7) . . ?
C121 C18 C17 104.4(7) . . ?
C22 C21 C26 113.8(12) . . ?
C22 C21 C2 121.9(10) . . ?
C26 C21 C2 124.3(11) . . ?
C21 C22 C23 121.0(11) . . ?
C21 C22 N2 117.8(10) . . ?
C23 C22 N2 121.1(9) . . ?
C22 C23 C24 117.6(12) . . ?
C22 C23 H8 121.2 . . ?
C24 C23 H8 121.2 . . ?
C25 C24 C23 126.7(16) . . ?
C25 C24 H9 116.6 . . ?
C23 C24 H9 116.6 . . ?
C24 C25 C26 114.9(16) . . ?
C24 C25 H10 122.5 . . ?
C26 C25 H10 122.5 . . ?
C25 C26 C21 125.7(14) . . ?
C25 C26 N4 124.8(15) . . ?
C21 C26 N4 108.9(14) . . ?
O2 C27 N2 123.2(8) . . ?
O2 C27 C28 121.2(8) . . ?
N2 C27 C28 115.5(8) . . ?
C211 C28 C231 112.0(7) . . ?
C211 C28 C221 110.6(7) . . ?
C231 C28 C221 107.1(7) . . ?
C211 C28 C27 109.1(7) . . ?
C231 C28 C27 108.1(7) . . ?
C221 C28 C27 110.0(7) . . ?
C32 C31 C38 112.8(9) . . ?
C32 C31 H13 109.0 . . ?
C38 C31 H13 109.0 . . ?
C32 C31 H14 109.0 . . ?
C38 C31 H14 109.0 . . ?
H13 C31 H14 107.8 . . ?
C33 C32 C31 118.5(10) . . ?
C33 C32 H15 107.7 . . ?
C31 C32 H15 107.7 . . ?
C33 C32 H16 107.7 . . ?
C31 C32 H16 107.7 . . ?
H15 C32 H16 107.1 . . ?
C32 C33 H19 109.5 . . ?
C32 C33 H18 109.5 . . ?
H19 C33 H18 109.5 . . ?
C32 C33 H17 109.5 . . ?
H19 C33 H17 109.5 . . ?
H18 C33 H17 109.5 . . ?
O3 C37 N3 125.4(11) . 3_566 ?
O3 C37 C38 121.1(11) . . ?
N3 C37 C38 113.3(10) 3_566 . ?
O3 C37 Ca2 24.1(5) . . ?
N3 C37 Ca2 144.8(8) 3_566 . ?
C38 C37 Ca2 100.8(7) . . ?
C37 C38 C31 120.3(9) . . ?
C37 C38 H11 107.2 . . ?
C31 C38 H11 107.2 . . ?
C37 C38 H12 107.2 . . ?
C31 C38 H12 107.2 . . ?
H11 C38 H12 106.9 . . ?
C48 C41 C42 104.4(10) . . ?
C48 C41 H22 110.9 . . ?
C42 C41 H22 110.9 . . ?
C48 C41 H23 110.9 . . ?
C42 C41 H23 110.9 . . ?
H22 C41 H23 108.9 . . ?
C41 C42 C43 101.0(11) . . ?
C41 C42 H24 111.6 . . ?
C43 C42 H24 111.6 . . ?
C41 C42 H25 111.6 . . ?
C43 C42 H25 111.6 . . ?
H24 C42 H25 109.4 . . ?
C42 C43 H26 109.5 . . ?
C42 C43 H28 109.5 . . ?
H26 C43 H28 109.5 . . ?
C42 C43 H27 109.5 . . ?
H26 C43 H27 109.5 . . ?
H28 C43 H27 109.5 . . ?
O4 C47 N4 109.9(14) . . ?
O4 C47 C48 133.7(19) . . ?
N4 C47 C48 116.0(17) . . ?
C41 C48 C47 105.5(12) . . ?
C41 C48 H20 110.6 . . ?
C47 C48 H20 110.6 . . ?
C41 C48 H21 110.6 . . ?
C47 C48 H21 110.6 . . ?
H20 C48 H21 108.8 . . ?
O51 C51 C52 113.2(19) . . ?
O51 C51 H107 108.9 . . ?
C52 C51 H107 108.9 . . ?
O51 C51 H108 108.9 . . ?
C52 C51 H108 108.9 . . ?
H107 C51 H108 107.8 . . ?
O52 C52 C51 108.5(18) . . ?
O52 C52 H110 110.0 . . ?
C51 C52 H110 110.0 . . ?
O52 C52 H109 110.0 . . ?
C51 C52 H109 110.0 . . ?
H110 C52 H109 108.4 . . ?
O52 C53 C54 126(3) . . ?
O52 C53 H111 105.7 . . ?
C54 C53 H111 105.7 . . ?
O52 C53 H112 105.7 . . ?
C54 C53 H112 105.7 . . ?
H111 C53 H112 106.2 . . ?
O51 C54 C53 96(2) . . ?
O51 C54 Ca1 45.8(18) . . ?
C53 C54 Ca1 112(2) . . ?
O51 C54 H114 112.6 . . ?
C53 C54 H114 112.6 . . ?
Ca1 C54 H114 132.0 . . ?
O51 C54 H113 112.6 . . ?
C53 C54 H113 112.6 . . ?
Ca1 C54 H113 66.8 . . ?
H114 C54 H113 110.1 . . ?
O61 C61 C62 96.6(15) . . ?
O61 C61 H115 112.4 . . ?
C62 C61 H115 112.4 . . ?
O61 C61 H116 112.4 . . ?
C62 C61 H116 112.4 . . ?
H115 C61 H116 110.0 . . ?
O62 C62 C61 112.1(17) . . ?
O62 C62 H118 109.2 . . ?
C61 C62 H118 109.2 . . ?
O62 C62 H117 109.2 . . ?
C61 C62 H117 109.2 . . ?
H118 C62 H117 107.9 . . ?
O62 C63 C64 110(2) . . ?
O62 C63 H119 109.7 . . ?
C64 C63 H119 109.7 . . ?
O62 C63 H120 109.7 . . ?
C64 C63 H120 109.7 . . ?
H119 C63 H120 108.2 . . ?
O61 C64 C63 90(2) . . ?
O61 C64 H122 113.7 . . ?
C63 C64 H122 113.7 . . ?
O61 C64 H121 113.7 . . ?
C63 C64 H121 113.7 . . ?
H122 C64 H121 111.0 . . ?
O71 C71 C72 103.6(16) . . ?
O71 C71 H123 111.0 . . ?
C72 C71 H123 111.0 . . ?
O71 C71 H124 111.0 . . ?
C72 C71 H124 111.0 . . ?
H123 C71 H124 109.0 . . ?
O72 C72 C71 127(2) . . ?
O72 C72 H126 105.4 . . ?
C71 C72 H126 105.4 . . ?
O72 C72 H125 105.4 . . ?
C71 C72 H125 105.4 . . ?
H126 C72 H125 106.0 . . ?
O72 C73 C74 111(2) . . ?
O72 C73 H127 109.4 . . ?
C74 C73 H127 109.4 . . ?
O72 C73 H128 109.4 . . ?
C74 C73 H128 109.4 . . ?
H127 C73 H128 108.0 . . ?
O71 C74 C73 112(2) . . ?
O71 C74 H130 109.2 . . ?
C73 C74 H130 109.2 . . ?
O71 C74 H129 109.2 . . ?
C73 C74 H129 109.2 . . ?
H130 C74 H129 107.9 . . ?
O81 C81 C82 115.7(15) . . ?
O81 C81 H132 108.4 . . ?
C82 C81 H132 108.4 . . ?
O81 C81 H131 108.4 . . ?
C82 C81 H131 108.4 . . ?
H132 C81 H131 107.4 . . ?
O82 C82 C81 116.6(14) . . ?
O82 C82 H133 108.1 . . ?
C81 C82 H133 108.1 . . ?
O82 C82 H134 108.1 . . ?
C81 C82 H134 108.1 . . ?
H133 C82 H134 107.3 . . ?
O82 C83 C84 132(2) . . ?
O82 C83 H135 104.3 . . ?
C84 C83 H135 104.3 . . ?
O82 C83 H136 104.3 . . ?
C84 C83 H136 104.3 . . ?
H135 C83 H136 105.6 . . ?
O81 C84 C83 86.9(19) . . ?
O81 C84 H137 114.2 . . ?
C83 C84 H137 114.2 . . ?
O81 C84 H138 114.2 . . ?
C83 C84 H138 114.2 . . ?
H137 C84 H138 111.3 . . ?
C116 C111 C112 114.8(9) . . ?
C116 C111 C18 127.5(9) . . ?
C112 C111 C18 117.6(8) . . ?
C113 C112 C111 123.5(9) . . ?
C113 C112 H29 118.2 . . ?
C111 C112 H29 118.2 . . ?
C114 C113 C112 120.7(10) . . ?
C114 C113 H30 119.7 . . ?
C112 C113 H30 119.7 . . ?
C113 C114 C115 117.1(9) . . ?
C113 C114 C117 122.5(10) . . ?
C115 C114 C117 120.3(10) . . ?
C114 C115 C116 121.2(10) . . ?
C114 C115 H31 119.4 . . ?
C116 C115 H31 119.4 . . ?
C111 C116 C115 122.7(10) . . ?
C111 C116 H32 118.7 . . ?
C115 C116 H32 118.7 . . ?
C118 C117 C119 112.9(11) . . ?
C118 C117 C120 106.5(11) . . ?
C119 C117 C120 103.9(11) . . ?
C118 C117 C114 115.3(10) . . ?
C119 C117 C114 109.4(8) . . ?
C120 C117 C114 107.9(9) . . ?
C117 C118 H33 109.5 . . ?
C117 C118 H34 109.5 . . ?
H33 C118 H34 109.5 . . ?
C117 C118 H35 109.5 . . ?
H33 C118 H35 109.5 . . ?
H34 C118 H35 109.5 . . ?
C117 C119 H36 109.5 . . ?
C117 C119 H38 109.5 . . ?
H36 C119 H38 109.5 . . ?
C117 C119 H37 109.5 . . ?
H36 C119 H37 109.5 . . ?
H38 C119 H37 109.5 . . ?
C117 C120 H39 109.5 . . ?
C117 C120 H40 109.5 . . ?
H39 C120 H40 109.5 . . ?
C117 C120 H41 109.5 . . ?
H39 C120 H41 109.5 . . ?
H40 C120 H41 109.5 . . ?
C122 C121 C126 116.6(8) . . ?
C122 C121 C18 124.7(8) . . ?
C126 C121 C18 118.8(7) . . ?
C121 C122 C123 122.3(8) . . ?
C121 C122 H42 118.8 . . ?
C123 C122 H42 118.8 . . ?
C122 C123 C124 120.0(8) . . ?
C122 C123 H43 120.0 . . ?
C124 C123 H43 120.0 . . ?
C125 C124 C123 117.2(7) . . ?
C125 C124 C127 123.6(8) . . ?
C123 C124 C127 119.0(8) . . ?
C126 C125 C124 120.9(8) . . ?
C126 C125 H44 119.5 . . ?
C124 C125 H44 119.5 . . ?
C125 C126 C121 122.7(8) . . ?
C125 C126 H45 118.7 . . ?
C121 C126 H45 118.7 . . ?
C129 C127 C130 108.0(10) . . ?
C129 C127 C128 107.2(9) . . ?
C130 C127 C128 106.9(11) . . ?
C129 C127 C124 109.5(9) . . ?
C130 C127 C124 112.4(8) . . ?
C128 C127 C124 112.6(8) . . ?
C127 C128 H46 109.5 . . ?
C127 C128 H48 109.5 . . ?
H46 C128 H48 109.5 . . ?
C127 C128 H47 109.5 . . ?
H46 C128 H47 109.5 . . ?
H48 C128 H47 109.5 . . ?
C127 C129 H51 109.5 . . ?
C127 C129 H50 109.5 . . ?
H51 C129 H50 109.5 . . ?
C127 C129 H49 109.5 . . ?
H51 C129 H49 109.5 . . ?
H50 C129 H49 109.5 . . ?
C127 C130 H53 109.5 . . ?
C127 C130 H52 109.5 . . ?
H53 C130 H52 109.5 . . ?
C127 C130 H54 109.5 . . ?
H53 C130 H54 109.5 . . ?
H52 C130 H54 109.5 . . ?
C136 C131 C132 117.4(8) . . ?
C136 C131 C18 124.9(8) . . ?
C132 C131 C18 117.6(8) . . ?
C133 C132 C131 121.3(9) . . ?
C133 C132 H55 119.4 . . ?
C131 C132 H55 119.4 . . ?
C132 C133 C134 122.7(8) . . ?
C132 C133 H56 118.7 . . ?
C134 C133 H56 118.7 . . ?
C133 C134 C135 114.5(8) . . ?
C133 C134 C137 122.7(8) . . ?
C135 C134 C137 122.8(8) . . ?
C136 C135 C134 122.7(8) . . ?
C136 C135 H57 118.7 . . ?
C134 C135 H57 118.7 . . ?
C131 C136 C135 121.4(8) . . ?
C131 C136 H58 119.3 . . ?
C135 C136 H58 119.3 . . ?
C139 C137 C138 98.7(14) . . ?
C139 C137 C134 112.6(9) . . ?
C138 C137 C134 114.2(8) . . ?
C139 C137 C140 110.7(14) . . ?
C138 C137 C140 110.0(13) . . ?
C134 C137 C140 110.1(10) . . ?
C137 C138 H59 109.5 . . ?
C137 C138 H60 109.5 . . ?
H59 C138 H60 109.5 . . ?
C137 C138 H61 109.5 . . ?
H59 C138 H61 109.5 . . ?
H60 C138 H61 109.5 . . ?
C137 C139 H62 109.5 . . ?
C137 C139 H63 109.5 . . ?
H62 C139 H63 109.5 . . ?
C137 C139 H64 109.5 . . ?
H62 C139 H64 109.5 . . ?
H63 C139 H64 109.5 . . ?
C137 C140 H67 109.5 . . ?
C137 C140 H65 109.5 . . ?
H67 C140 H65 109.5 . . ?
C137 C140 H66 109.5 . . ?
H67 C140 H66 109.5 . . ?
H65 C140 H66 109.5 . . ?
C216 C211 C212 116.8(9) . . ?
C216 C211 C28 124.8(9) . . ?
C212 C211 C28 118.3(8) . . ?
C211 C212 C213 119.4(9) . . ?
C211 C212 H68 120.3 . . ?
C213 C212 H68 120.3 . . ?
C214 C213 C212 122.5(11) . . ?
C214 C213 H69 118.8 . . ?
C212 C213 H69 118.8 . . ?
C213 C214 C215 117.2(11) . . ?
C213 C214 C217 122.2(14) . . ?
C215 C214 C217 120.6(13) . . ?
C216 C215 C214 121.2(11) . . ?
C216 C215 H70 119.4 . . ?
C214 C215 H70 119.4 . . ?
C215 C216 C211 122.9(11) . . ?
C215 C216 H71 118.6 . . ?
C211 C216 H71 118.6 . . ?
C218 C217 C220 114.5(16) . . ?
C218 C217 C214 113.1(14) . . ?
C220 C217 C214 111.1(11) . . ?
C218 C217 C219 108.8(17) . . ?
C220 C217 C219 100.0(15) . . ?
C214 C217 C219 108.3(12) . . ?
C217 C218 H72 109.5 . . ?
C217 C218 H74 109.5 . . ?
H72 C218 H74 109.5 . . ?
C217 C218 H73 109.5 . . ?
H72 C218 H73 109.5 . . ?
H74 C218 H73 109.5 . . ?
C217 C219 H76 109.5 . . ?
C217 C219 H75 109.5 . . ?
H76 C219 H75 109.5 . . ?
C217 C219 H77 109.5 . . ?
H76 C219 H77 109.5 . . ?
H75 C219 H77 109.5 . . ?
C217 C220 H78 109.5 . . ?
C217 C220 H80 109.5 . . ?
H78 C220 H80 109.5 . . ?
C217 C220 H79 109.5 . . ?
H78 C220 H79 109.5 . . ?
H80 C220 H79 109.5 . . ?
C226 C221 C222 114.8(8) . . ?
C226 C221 C28 125.4(8) . . ?
C222 C221 C28 119.7(8) . . ?
C223 C222 C221 122.2(8) . . ?
C223 C222 H81 118.9 . . ?
C221 C222 H81 118.9 . . ?
C222 C223 C224 123.5(9) . . ?
C222 C223 H82 118.2 . . ?
C224 C223 H82 118.2 . . ?
C223 C224 C225 112.8(8) . . ?
C223 C224 C227 123.3(9) . . ?
C225 C224 C227 123.9(9) . . ?
C226 C225 C224 126.2(9) . . ?
C226 C225 H83 116.9 . . ?
C224 C225 H83 116.9 . . ?
C225 C226 C221 120.4(9) . . ?
C225 C226 H84 119.8 . . ?
C221 C226 H84 119.8 . . ?
C229 C227 C230 104.5(15) . . ?
C229 C227 C224 117.3(11) . . ?
C230 C227 C224 109.0(11) . . ?
C229 C227 C228 107.9(12) . . ?
C230 C227 C228 101.4(14) . . ?
C224 C227 C228 115.0(9) . . ?
C227 C228 H86 109.5 . . ?
C227 C228 H85 109.5 . . ?
H86 C228 H85 109.5 . . ?
C227 C228 H87 109.5 . . ?
H86 C228 H87 109.5 . . ?
H85 C228 H87 109.5 . . ?
C227 C229 H88 109.5 . . ?
C227 C229 H90 109.5 . . ?
H88 C229 H90 109.5 . . ?
C227 C229 H89 109.5 . . ?
H88 C229 H89 109.5 . . ?
H90 C229 H89 109.5 . . ?
C227 C230 H92 109.5 . . ?
C227 C230 H91 109.5 . . ?
H92 C230 H91 109.5 . . ?
C227 C230 H93 109.5 . . ?
H92 C230 H93 109.5 . . ?
H91 C230 H93 109.5 . . ?
C232 C231 C236 116.0(8) . . ?
C232 C231 C28 124.8(9) . . ?
C236 C231 C28 119.3(8) . . ?
C231 C232 C233 123.3(9) . . ?
C231 C232 H94 118.4 . . ?
C233 C232 H94 118.4 . . ?
C234 C233 C232 118.5(9) . . ?
C234 C233 H95 120.7 . . ?
C232 C233 H95 120.7 . . ?
C235 C234 C233 118.5(8) . . ?
C235 C234 C237 119.0(10) . . ?
C233 C234 C237 122.4(9) . . ?
C234 C235 C236 121.8(9) . . ?
C234 C235 H96 119.1 . . ?
C236 C235 H96 119.1 . . ?
C235 C236 C231 121.8(9) . . ?
C235 C236 H97 119.1 . . ?
C231 C236 H97 119.1 . . ?
C238 C237 C239 108.9(8) . . ?
C238 C237 C234 110.6(9) . . ?
C239 C237 C234 109.6(7) . . ?
C238 C237 C240 109.4(8) . . ?
C239 C237 C240 110.3(9) . . ?
C234 C237 C240 108.0(7) . . ?
C237 C238 H99 109.5 . . ?
C237 C238 H98 109.5 . . ?
H99 C238 H98 109.5 . . ?
C237 C238 H100 109.5 . . ?
H99 C238 H100 109.5 . . ?
H98 C238 H100 109.5 . . ?
C237 C239 H103 109.5 . . ?
C237 C239 H102 109.5 . . ?
H103 C239 H102 109.5 . . ?
C237 C239 H101 109.5 . . ?
H103 C239 H101 109.5 . . ?
H102 C239 H101 109.5 . . ?
C237 C240 H105 109.5 . . ?
C237 C240 H104 109.5 . . ?
H105 C240 H104 109.5 . . ?
C237 C240 H106 109.5 . . ?
H105 C240 H106 109.5 . . ?
H104 C240 H106 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
Ca2 O12 C1 O11 25.3(12) . . . . ?
Ca1 O12 C1 O11 11.0(10) . . . . ?
Ca2 O12 C1 C11 -152.7(8) . . . . ?
Ca1 O12 C1 C11 -167.0(9) . . . . ?
Ca1 O11 C1 O12 -12.5(11) . . . . ?
Ca2 O11 C1 O12 -21.2(10) . . . . ?
Ca1 O11 C1 C11 165.6(7) . . . . ?
Ca2 O11 C1 C11 156.9(9) . . . . ?
Ca1 O22 C2 O21 -19.4(9) . . . . ?
Ca1 O22 C2 C21 165.5(12) . . . . ?
Ca1 O21 C2 O22 31.5(15) . . . . ?
Ca2 O21 C2 O22 9.8(17) . . . . ?
Ca1 O21 C2 C21 -153.4(8) . . . . ?
Ca2 O21 C2 C21 -175.1(7) . . . . ?
O12 C1 C11 C16 156.4(9) . . . . ?
O11 C1 C11 C16 -21.7(14) . . . . ?
Ca1 C1 C11 C16 33(4) . . . . ?
Ca2 C1 C11 C16 88(2) . . . . ?
O12 C1 C11 C12 -26.0(14) . . . . ?
O11 C1 C11 C12 155.9(9) . . . . ?
Ca1 C1 C11 C12 -149(3) . . . . ?
Ca2 C1 C11 C12 -94(2) . . . . ?
C17 N1 C12 C13 22.5(13) . . . . ?
C17 N1 C12 C11 -163.6(8) . . . . ?
C16 C11 C12 C13 -0.6(13) . . . . ?
C1 C11 C12 C13 -178.4(8) . . . . ?
C16 C11 C12 N1 -174.4(8) . . . . ?
C1 C11 C12 N1 7.8(13) . . . . ?
N1 C12 C13 C14 173.0(9) . . . . ?
C11 C12 C13 C14 -0.7(13) . . . . ?
C12 C13 C14 C15 1.7(14) . . . . ?
C13 C14 C15 C16 -1.4(15) . . . . ?
C14 C15 C16 C11 0.1(14) . . . . ?
C14 C15 C16 N3 178.5(8) . . . . ?
C12 C11 C16 C15 0.9(13) . . . . ?
C1 C11 C16 C15 178.6(9) . . . . ?
C12 C11 C16 N3 -177.6(7) . . . . ?
C1 C11 C16 N3 0.1(13) . . . . ?
C37 N3 C16 C15 30.0(14) 3_566 . . . ?
C37 N3 C16 C11 -151.5(9) 3_566 . . . ?
C12 N1 C17 O1 12.2(14) . . . . ?
C12 N1 C17 C18 -166.8(8) . . . . ?
O1 C17 C18 C111 117.7(9) . . . . ?
N1 C17 C18 C111 -63.3(9) . . . . ?
O1 C17 C18 C131 -2.4(11) . . . . ?
N1 C17 C18 C131 176.6(7) . . . . ?
O1 C17 C18 C121 -121.0(9) . . . . ?
N1 C17 C18 C121 58.0(9) . . . . ?
O22 C2 C21 C22 22.8(17) . . . . ?
O21 C2 C21 C22 -152.3(11) . . . . ?
Ca1 C2 C21 C22 171.6(12) . . . . ?
O22 C2 C21 C26 -154.5(12) . . . . ?
O21 C2 C21 C26 30.4(18) . . . . ?
Ca1 C2 C21 C26 -6(2) . . . . ?
C26 C21 C22 C23 -2.5(16) . . . . ?
C2 C21 C22 C23 179.9(11) . . . . ?
C26 C21 C22 N2 -179.8(9) . . . . ?
C2 C21 C22 N2 2.6(15) . . . . ?
C27 N2 C22 C21 165.7(9) . . . . ?
C27 N2 C22 C23 -11.6(15) . . . . ?
C21 C22 C23 C24 3.2(18) . . . . ?
N2 C22 C23 C24 -179.6(11) . . . . ?
C22 C23 C24 C25 -4(3) . . . . ?
C23 C24 C25 C26 4(3) . . . . ?
C24 C25 C26 C21 -3(3) . . . . ?
C24 C25 C26 N4 -173.1(14) . . . . ?
C22 C21 C26 C25 3(2) . . . . ?
C2 C21 C26 C25 -179.9(15) . . . . ?
C22 C21 C26 N4 173.9(10) . . . . ?
C2 C21 C26 N4 -8.6(16) . . . . ?
C47 N4 C26 C25 -25(3) . . . . ?
C47 N4 C26 C21 163.7(16) . . . . ?
C22 N2 C27 O2 -4.5(15) . . . . ?
C22 N2 C27 C28 179.5(8) . . . . ?
O2 C27 C28 C211 145.1(9) . . . . ?
N2 C27 C28 C211 -38.9(10) . . . . ?
O2 C27 C28 C231 23.1(12) . . . . ?
N2 C27 C28 C231 -160.8(8) . . . . ?
O2 C27 C28 C221 -93.5(10) . . . . ?
N2 C27 C28 C221 82.5(9) . . . . ?
C38 C31 C32 C33 -177.5(9) . . . . ?
Ca2 O3 C37 N3 -150.2(10) . . . 3_566 ?
Ca1 O3 C37 N3 -116.0(12) . . . 3_566 ?
Ca2 O3 C37 C38 35.9(19) . . . . ?
Ca1 O3 C37 C38 70.2(17) . . . . ?
O3 C37 C38 C31 -153.1(10) . . . . ?
N3 C37 C38 C31 32.3(13) 3_566 . . . ?
Ca2 C37 C38 C31 -139.0(8) . . . . ?
C32 C31 C38 C37 170.7(9) . . . . ?
C48 C41 C42 C43 153(2) . . . . ?
C26 N4 C47 O4 -7(3) . . . . ?
C26 N4 C47 C48 166.6(14) . . . . ?
C42 C41 C48 C47 158.5(19) . . . . ?
O4 C47 C48 C41 -36(4) . . . . ?
N4 C47 C48 C41 152(2) . . . . ?
C54 O51 C51 C52 -44(4) . . . . ?
Ca1 O51 C51 C52 107(2) . . . . ?
C53 O52 C52 C51 -56(3) . . . . ?
O51 C51 C52 O52 49(3) . . . . ?
C52 O52 C53 C54 68(4) . . . . ?
C51 O51 C54 C53 38(5) . . . . ?
Ca1 O51 C54 C53 -115(3) . . . . ?
C51 O51 C54 Ca1 153(3) . . . . ?
O52 C53 C54 O51 -53(5) . . . . ?
O52 C53 C54 Ca1 -97(4) . . . . ?
C64 O61 C61 C62 76(2) . . . . ?
C63 O62 C62 C61 55(2) . . . . ?
O61 C61 C62 O62 -52(2) . . . . ?
C62 O62 C63 C64 -66(2) . . . . ?
C61 O61 C64 C63 -83(2) . . . . ?
O62 C63 C64 O61 69(2) . . . . ?
C74 O71 C71 C72 54(3) . . . . ?
C73 O72 C72 C71 28(4) . . . . ?
O71 C71 C72 O72 -38(4) . . . . ?
C72 O72 C73 C74 -35(3) . . . . ?
C71 O71 C74 C73 -73(3) . . . . ?
O72 C73 C74 O71 61(3) . . . . ?
C84 O81 C81 C82 35(4) . . . . ?
C83 O82 C82 C81 27(3) . . . . ?
O81 C81 C82 O82 -20(3) . . . . ?
C82 O82 C83 C84 -55(4) . . . . ?
C81 O81 C84 C83 -43(4) . . . . ?
O82 C83 C84 O81 53(4) . . . . ?
C131 C18 C111 C116 125.3(9) . . . . ?
C121 C18 C111 C116 -111.1(10) . . . . ?
C17 C18 C111 C116 6.2(12) . . . . ?
C131 C18 C111 C112 -52.7(9) . . . . ?
C121 C18 C111 C112 70.9(10) . . . . ?
C17 C18 C111 C112 -171.9(7) . . . . ?
C116 C111 C112 C113 1.9(13) . . . . ?
C18 C111 C112 C113 -179.8(8) . . . . ?
C111 C112 C113 C114 -0.1(14) . . . . ?
C112 C113 C114 C115 -2.2(14) . . . . ?
C112 C113 C114 C117 -179.0(9) . . . . ?
C113 C114 C115 C116 2.6(15) . . . . ?
C117 C114 C115 C116 179.5(9) . . . . ?
C112 C111 C116 C115 -1.5(13) . . . . ?
C18 C111 C116 C115 -179.6(8) . . . . ?
C114 C115 C116 C111 -0.8(15) . . . . ?
C113 C114 C117 C118 -173.8(12) . . . . ?
C115 C114 C117 C118 9.4(16) . . . . ?
C113 C114 C117 C119 57.6(13) . . . . ?
C115 C114 C117 C119 -119.2(11) . . . . ?
C113 C114 C117 C120 -54.9(13) . . . . ?
C115 C114 C117 C120 128.3(11) . . . . ?
C111 C18 C121 C122 -3.1(13) . . . . ?
C131 C18 C121 C122 119.0(9) . . . . ?
C17 C18 C121 C122 -125.5(9) . . . . ?
C111 C18 C121 C126 177.2(9) . . . . ?
C131 C18 C121 C126 -60.8(11) . . . . ?
C17 C18 C121 C126 54.8(10) . . . . ?
C126 C121 C122 C123 -1.3(14) . . . . ?
C18 C121 C122 C123 179.0(9) . . . . ?
C121 C122 C123 C124 4.5(15) . . . . ?
C122 C123 C124 C125 -6.6(14) . . . . ?
C122 C123 C124 C127 179.0(9) . . . . ?
C123 C124 C125 C126 5.8(14) . . . . ?
C127 C124 C125 C126 179.9(9) . . . . ?
C124 C125 C126 C121 -2.8(15) . . . . ?
C122 C121 C126 C125 0.4(14) . . . . ?
C18 C121 C126 C125 -179.8(8) . . . . ?
C125 C124 C127 C129 116.3(11) . . . . ?
C123 C124 C127 C129 -69.7(12) . . . . ?
C125 C124 C127 C130 -3.7(15) . . . . ?
C123 C124 C127 C130 170.3(11) . . . . ?
C125 C124 C127 C128 -124.6(11) . . . . ?
C123 C124 C127 C128 49.5(13) . . . . ?
C111 C18 C131 C136 118.8(9) . . . . ?
C121 C18 C131 C136 -4.8(12) . . . . ?
C17 C18 C131 C136 -118.5(9) . . . . ?
C111 C18 C131 C132 -56.9(10) . . . . ?
C121 C18 C131 C132 179.5(8) . . . . ?
C17 C18 C131 C132 65.8(9) . . . . ?
C136 C131 C132 C133 1.7(13) . . . . ?
C18 C131 C132 C133 177.7(8) . . . . ?
C131 C132 C133 C134 -0.6(15) . . . . ?
C132 C133 C134 C135 -0.2(13) . . . . ?
C132 C133 C134 C137 179.5(9) . . . . ?
C133 C134 C135 C136 0.0(12) . . . . ?
C137 C134 C135 C136 -179.7(8) . . . . ?
C132 C131 C136 C135 -1.9(12) . . . . ?
C18 C131 C136 C135 -177.7(8) . . . . ?
C134 C135 C136 C131 1.2(13) . . . . ?
C133 C134 C137 C139 135.0(14) . . . . ?
C135 C134 C137 C139 -45.3(16) . . . . ?
C133 C134 C137 C138 23.5(16) . . . . ?
C135 C134 C137 C138 -156.9(13) . . . . ?
C133 C134 C137 C140 -100.9(13) . . . . ?
C135 C134 C137 C140 78.8(13) . . . . ?
C231 C28 C211 C216 -117.3(9) . . . . ?
C221 C28 C211 C216 2.1(11) . . . . ?
C27 C28 C211 C216 123.1(8) . . . . ?
C231 C28 C211 C212 67.1(9) . . . . ?
C221 C28 C211 C212 -173.5(7) . . . . ?
C27 C28 C211 C212 -52.5(10) . . . . ?
C216 C211 C212 C213 1.3(12) . . . . ?
C28 C211 C212 C213 177.2(7) . . . . ?
C211 C212 C213 C214 -1.3(14) . . . . ?
C212 C213 C214 C215 -0.5(15) . . . . ?
C212 C213 C214 C217 -177.9(10) . . . . ?
C213 C214 C215 C216 2.3(16) . . . . ?
C217 C214 C215 C216 179.8(10) . . . . ?
C214 C215 C216 C211 -2.3(16) . . . . ?
C212 C211 C216 C215 0.4(13) . . . . ?
C28 C211 C216 C215 -175.2(9) . . . . ?
C213 C214 C217 C218 108.1(19) . . . . ?
C215 C214 C217 C218 -69(2) . . . . ?
C213 C214 C217 C220 -121.5(15) . . . . ?
C215 C214 C217 C220 61.1(18) . . . . ?
C213 C214 C217 C219 -12.6(17) . . . . ?
C215 C214 C217 C219 170.1(12) . . . . ?
C211 C28 C221 C226 102.6(10) . . . . ?
C231 C28 C221 C226 -135.1(9) . . . . ?
C27 C28 C221 C226 -17.9(12) . . . . ?
C211 C28 C221 C222 -80.1(10) . . . . ?
C231 C28 C221 C222 42.2(11) . . . . ?
C27 C28 C221 C222 159.4(8) . . . . ?
C226 C221 C222 C223 -1.5(14) . . . . ?
C28 C221 C222 C223 -179.2(9) . . . . ?
C221 C222 C223 C224 1.7(17) . . . . ?
C222 C223 C224 C225 -1.1(15) . . . . ?
C222 C223 C224 C227 177.8(11) . . . . ?
C223 C224 C225 C226 0.5(15) . . . . ?
C227 C224 C225 C226 -178.4(11) . . . . ?
C224 C225 C226 C221 -0.5(16) . . . . ?
C222 C221 C226 C225 0.9(13) . . . . ?
C28 C221 C226 C225 178.4(9) . . . . ?
C223 C224 C227 C229 138.6(15) . . . . ?
C225 C224 C227 C229 -43(2) . . . . ?
C223 C224 C227 C230 -103.0(15) . . . . ?
C225 C224 C227 C230 75.7(16) . . . . ?
C223 C224 C227 C228 10.0(17) . . . . ?
C225 C224 C227 C228 -171.2(12) . . . . ?
C211 C28 C231 C232 -2.9(11) . . . . ?
C221 C28 C231 C232 -124.3(9) . . . . ?
C27 C28 C231 C232 117.2(9) . . . . ?
C211 C28 C231 C236 177.4(8) . . . . ?
C221 C28 C231 C236 56.0(10) . . . . ?
C27 C28 C231 C236 -62.5(10) . . . . ?
C236 C231 C232 C233 -1.3(12) . . . . ?
C28 C231 C232 C233 179.0(7) . . . . ?
C231 C232 C233 C234 3.4(12) . . . . ?
C232 C233 C234 C235 -3.8(12) . . . . ?
C232 C233 C234 C237 176.4(7) . . . . ?
C233 C234 C235 C236 2.3(13) . . . . ?
C237 C234 C235 C236 -177.9(8) . . . . ?
C234 C235 C236 C231 -0.2(13) . . . . ?
C232 C231 C236 C235 -0.4(13) . . . . ?
C28 C231 C236 C235 179.4(8) . . . . ?
C235 C234 C237 C238 -177.0(8) . . . . ?
C233 C234 C237 C238 2.8(12) . . . . ?
C235 C234 C237 C239 -56.9(11) . . . . ?
C233 C234 C237 C239 122.9(10) . . . . ?
C235 C234 C237 C240 63.3(11) . . . . ?
C233 C234 C237 C240 -116.9(9) . . . . ?

_refine_diff_density_max         0.722
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.070

_shelxl_version_number           2014/6

# start Validation Reply Form
_vrf_RFACR01_Ca2L24-41,4-dioxane-4H2O 
;
PROBLEM: The value of the weighted R factor is > 0.45
RESPONSE: This crystal is thin and relatively low crystallinity. 
;
_vrf_RINTA01_Ca2L24-41,4-dioxane-4H2O 
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: This crystal is thin and relatively low crystallinity; therefore, 
the reflections were weak especially at high angle. The poor quality of the 
data was probably caused by the highly disordered structure with pseudo-
centrosymmetry, which resulted in large Rint and R values.
;
_vrf_PLAT020_Ca2L24-41,4-dioxane-4H2O 
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.275 Report
RESPONSE:This crystal is thin and relatively low crystallinity; therefore, 
the reflections were weak especially at high angle. The poor quality of the 
data was probably caused by the highly disordered structure with pseudo-
centrosymmetry, which resulted in large Rint and R values.
;
_vrf_PLAT026_Ca2L24-41,4-dioxane-4H2O 
;
PROBLEM: Ratio Observed / Unique Reflections too Low ....         29 %     
RESPONSE: The reflections were weak especially at high angle. At the higher 
angle, the reflections disappeared. Therefore, the number of the observed 
reflections is very low. 
;
_vrf_PLAT084_Ca2L24-41,4-dioxane-4H2O 
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.47 Report
RESPONSE: This crystal is thin and relatively low crystallinity; therefore, 
the reflections were weak especially at high angle. The poor quality of the 
data was probably caused by the highly disordered structure with pseudo-
centrosymmetry, which resulted in large Rint and R values.
;
_vrf_PLAT241_Ca2L24-41,4-dioxane-4H2O 
;
PROBLEM: High      Ueq as Compared to Neighbors for .....        C41 Check 
RESPONSE: C41 is the carbon atom of the n-Bu chain. The chain is disordered 
but could not be separated reasonably into two parts. The large Ueq indicates 
large thermal motion of the flexible alkyl chain. 
;
_vrf_PLAT242_Ca2L24-41,4-dioxane-4H2O 
;
PROBLEM: Low       Ueq as Compared to Neighbors for .....        C42 Check 
RESPONSE: The thermal motion of C41 is very large but that of C42 is normal.
;
_vrf_PLAT430_Ca2L24-41,4-dioxane-4H2O 
;
PROBLEM: Short Inter D...A Contact  O4     ..  O41     ..       2.47 Ang.  
RESPONSE: O41 is osygen atom of water molecule and forms hydrogen bond with 
amide carbonyl oxygen (O41H...O4=C47). The hydrogen atoms of the water could 
not be found in the differential Fourier map.
;
_chemical_properties_physical    Efflorescent
####################################################################### 
# 
# 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/access/V1 
# 
# Audit and citation data items may have 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_MgL12(EtOH)-4(EtOH)
_database_code_depnum_ccdc_archive 'CCDC 1042063'
_audit_update_record             
;
2015-01-05 deposited with the CCDC.
2015-03-18 downloaded from the CCDC.
;
_audit_creation_date             2014-11-01
_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        
; 
[{[(t-BuC6H4)3CCONH](n-BuCONH)C6H3COO}2Mg(EtOH)4]-4(EtOH)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C104 H154 Mg N4 O16'
_chemical_formula_sum            'C104 H154 Mg N4 O16'
_chemical_formula_weight         1740.61

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'
Mg Mg 0.0486 0.0363 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.1365(10)
_cell_length_b                   11.8861(4)
_cell_length_c                   31.198(2)
_cell_angle_alpha                90
_cell_angle_beta                 102.064(7)
_cell_angle_gamma                90
_cell_volume                     10203.1(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    200
_cell_measurement_reflns_used    23296
_cell_measurement_theta_min      3.13
_cell_measurement_theta_max      27.45

_exptl_crystal_description       column
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_F_000             3784
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.081
_shelx_estimated_absorpt_T_min   0.984
_shelx_estimated_absorpt_T_max   0.995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9841
_exptl_absorpt_correction_T_max  0.9952
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   
;
 MicroMax-007HF microfocus rotating anode X-ray generator
;
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            38531
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         3.129
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.969
_reflns_number_total             8961
_reflns_number_gt                6226
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'RAPID AUTO (Rigaku, 2006)'
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2006)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2006)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1058P)²+18.9055P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8961
_refine_ls_number_parameters     582
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0756
_refine_ls_wR_factor_ref         0.2164
_refine_ls_wR_factor_gt          0.1942
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Mg1 Mg 0.5000 0.31448(12) 0.2500 0.0347(3) Uani 1 2 d S T P . .
O1 O 0.56055(8) 0.33825(18) 0.47344(7) 0.0431(5) Uani 1 1 d . . . . .
O2 O 0.40144(10) 0.7606(2) 0.31891(8) 0.0604(7) Uani 1 1 d . . . . .
O3 O 0.57578(8) 0.3215(2) 0.26814(7) 0.0449(6) Uani 1 1 d . . . . .
H3 H 0.5839(13) 0.368(3) 0.2883(12) 0.054 Uiso 1 1 d . U . . .
O4 O 0.50469(9) 0.1899(2) 0.20474(8) 0.0517(6) Uani 1 1 d . . . . .
H4 H 0.5220(14) 0.193(3) 0.1865(13) 0.062 Uiso 1 1 d . U . . .
O5 O 0.43914(12) 0.1805(3) 0.35457(10) 0.0729(9) Uani 1 1 d . . . . .
H5 H 0.4310(18) 0.116(4) 0.3572(16) 0.087 Uiso 1 1 d . U . . .
O6 O 0.44302(14) 0.9522(3) 0.36383(12) 0.0884(11) Uani 1 1 d . . . . .
H6 H 0.430(2) 0.888(5) 0.3532(17) 0.106 Uiso 1 1 d . U . . .
O11 O 0.49856(8) 0.43242(18) 0.29763(6) 0.0406(5) Uani 1 1 d . . . . .
O12 O 0.57463(7) 0.46295(19) 0.33315(7) 0.0416(5) Uani 1 1 d . . . . .
N1 N 0.57987(9) 0.4491(2) 0.42079(8) 0.0330(6) Uani 1 1 d D . . . .
H1 H 0.5967(11) 0.453(3) 0.4022(10) 0.040 Uiso 1 1 d D U . . .
N2 N 0.44006(10) 0.5940(2) 0.31473(9) 0.0410(6) Uani 1 1 d D . . . .
H2 H 0.4479(12) 0.547(3) 0.2972(10) 0.041 Uiso 1 1 d D U . . .
C1 C 0.52981(11) 0.4693(2) 0.33017(9) 0.0344(7) Uani 1 1 d . . . . .
C11 C 0.51010(11) 0.5208(2) 0.36680(9) 0.0318(6) Uani 1 1 d . . . . .
C12 C 0.53431(11) 0.5056(2) 0.41072(9) 0.0332(7) Uani 1 1 d . . . . .
C13 C 0.51427(12) 0.5473(3) 0.44472(10) 0.0381(7) Uani 1 1 d . . . . .
H7 H 0.5310 0.5375 0.4742 0.046 Uiso 1 1 calc R U . . .
C14 C 0.47049(12) 0.6026(3) 0.43578(10) 0.0423(8) Uani 1 1 d . . . . .
H8 H 0.4570 0.6296 0.4593 0.051 Uiso 1 1 calc R U . . .
C15 C 0.44581(12) 0.6195(3) 0.39312(10) 0.0421(8) Uani 1 1 d . . . . .
H9 H 0.4156 0.6580 0.3874 0.050 Uiso 1 1 calc R U . . .
C16 C 0.46551(11) 0.5799(3) 0.35863(10) 0.0359(7) Uani 1 1 d . . . . .
C17 C 0.59034(10) 0.3692(2) 0.45249(9) 0.0322(7) Uani 1 1 d . . . . .
C18 C 0.64333(10) 0.3221(2) 0.46439(9) 0.0327(6) Uani 1 1 d . . . . .
C21 C 0.37375(16) 0.7703(4) 0.22506(14) 0.0686(11) Uani 1 1 d . . . . .
H12 H 0.3535 0.7533 0.1958 0.082 Uiso 1 1 calc R U . . .
H13 H 0.3544 0.8194 0.2406 0.082 Uiso 1 1 calc R U . . .
C22 C 0.41813(18) 0.8339(4) 0.21900(15) 0.0781(13) Uani 1 1 d . . . . .
H14 H 0.4370 0.8563 0.2482 0.094 Uiso 1 1 calc R U . . .
H15 H 0.4075 0.9037 0.2024 0.094 Uiso 1 1 calc R U . . .
C23 C 0.4514(2) 0.7687(5) 0.19516(18) 0.0973(17) Uani 1 1 d . . . . .
H16 H 0.4793 0.8157 0.1926 0.117 Uiso 1 1 calc R U . . .
H17 H 0.4629 0.7004 0.2117 0.117 Uiso 1 1 calc R U . . .
H18 H 0.4334 0.7479 0.1658 0.117 Uiso 1 1 calc R U . . .
C27 C 0.40936(12) 0.6786(3) 0.29776(11) 0.0436(8) Uani 1 1 d . . . . .
C28 C 0.38445(13) 0.6612(3) 0.25041(11) 0.0523(9) Uani 1 1 d . . . . .
H10 H 0.3536 0.6204 0.2493 0.063 Uiso 1 1 calc R U . . .
H11 H 0.4054 0.6136 0.2360 0.063 Uiso 1 1 calc R U . . .
C31 C 0.61359(14) 0.3194(4) 0.24383(12) 0.0590(10) Uani 1 1 d . . . . .
H19 H 0.6364 0.3822 0.2535 0.071 Uiso 1 1 calc R U . . .
H20 H 0.5993 0.3300 0.2123 0.071 Uiso 1 1 calc R U . . .
C32 C 0.64047(18) 0.2117(5) 0.25008(18) 0.0949(17) Uani 1 1 d . . . . .
H21 H 0.6661 0.2126 0.2331 0.114 Uiso 1 1 calc R U . . .
H22 H 0.6551 0.2017 0.2812 0.114 Uiso 1 1 calc R U . . .
H23 H 0.6180 0.1495 0.2401 0.114 Uiso 1 1 calc R U . . .
C41 C 0.47321(14) 0.0953(3) 0.19358(12) 0.0565(10) Uani 1 1 d . . . . .
H24 H 0.4567 0.0795 0.2180 0.068 Uiso 1 1 calc R U . . .
H25 H 0.4929 0.0285 0.1896 0.068 Uiso 1 1 calc R U . . .
C42 C 0.43587(18) 0.1142(4) 0.15276(14) 0.0769(13) Uani 1 1 d . . . . .
H26 H 0.4152 0.0474 0.1464 0.092 Uiso 1 1 calc R U . . .
H27 H 0.4159 0.1794 0.1567 0.092 Uiso 1 1 calc R U . . .
H28 H 0.4520 0.1283 0.1283 0.092 Uiso 1 1 calc R U . . .
C51 C 0.4570(3) 0.2398(7) 0.3934(2) 0.163(4) Uani 1 1 d D U . . .
H29 H 0.4865 0.1996 0.4087 0.195 Uiso 1 1 calc R U . . .
H30 H 0.4680 0.3140 0.3847 0.195 Uiso 1 1 calc R U . . .
C52 C 0.4290(3) 0.2601(8) 0.4241(3) 0.163(3) Uani 1 1 d D U . . .
H31 H 0.4481 0.3026 0.4487 0.195 Uiso 1 1 calc R U . . .
H32 H 0.4002 0.3037 0.4106 0.195 Uiso 1 1 calc R U . . .
H33 H 0.4188 0.1883 0.4348 0.195 Uiso 1 1 calc R U . . .
C61 C 0.47741(18) 0.9101(4) 0.39985(16) 0.0821(14) Uani 1 1 d . . . . .
H34 H 0.5062 0.9601 0.4056 0.099 Uiso 1 1 calc R U . . .
H35 H 0.4882 0.8346 0.3925 0.099 Uiso 1 1 calc R U . . .
C62 C 0.4572(3) 0.9026(5) 0.43927(18) 0.113(2) Uani 1 1 d . . . . .
H36 H 0.4820 0.8732 0.4635 0.136 Uiso 1 1 calc R U . . .
H37 H 0.4471 0.9776 0.4469 0.136 Uiso 1 1 calc R U . . .
H38 H 0.4291 0.8521 0.4338 0.136 Uiso 1 1 calc R U . . .
C111 C 0.67674(10) 0.3741(2) 0.43622(9) 0.0323(6) Uani 1 1 d . . . . .
C112 C 0.66808(11) 0.3541(3) 0.39108(10) 0.0366(7) Uani 1 1 d . . . . .
H39 H 0.6416 0.3070 0.3782 0.044 Uiso 1 1 calc R U . . .
C113 C 0.69669(11) 0.4004(3) 0.36463(10) 0.0405(7) Uani 1 1 d . . . . .
H40 H 0.6890 0.3856 0.3340 0.049 Uiso 1 1 calc R U . . .
C114 C 0.73643(11) 0.4681(3) 0.38168(11) 0.0416(8) Uani 1 1 d . . . . .
C115 C 0.74612(12) 0.4855(3) 0.42678(11) 0.0442(8) Uani 1 1 d . . . . .
H41 H 0.7736 0.5293 0.4398 0.053 Uiso 1 1 calc R U . . .
C116 C 0.71698(11) 0.4412(3) 0.45336(10) 0.0384(7) Uani 1 1 d . . . . .
H42 H 0.7245 0.4568 0.4839 0.046 Uiso 1 1 calc R U . . .
C117 C 0.76844(13) 0.5228(3) 0.35303(12) 0.0499(9) Uani 1 1 d . . . . .
C118 C 0.7553(2) 0.4839(6) 0.30555(17) 0.113(2) Uani 1 1 d . . . . .
H43 H 0.7588 0.4020 0.3043 0.135 Uiso 1 1 calc R U . . .
H44 H 0.7216 0.5049 0.2929 0.135 Uiso 1 1 calc R U . . .
H45 H 0.7770 0.5198 0.2889 0.135 Uiso 1 1 calc R U . . .
C119 C 0.7629(3) 0.6460(5) 0.3539(3) 0.154(3) Uani 1 1 d . U . . .
H46 H 0.7286 0.6659 0.3434 0.184 Uiso 1 1 calc R U . . .
H47 H 0.7740 0.6733 0.3840 0.184 Uiso 1 1 calc R U . . .
H48 H 0.7824 0.6808 0.3349 0.184 Uiso 1 1 calc R U . . .
C120 C 0.82081(18) 0.4857(6) 0.3689(2) 0.110(2) Uani 1 1 d . . . . .
H49 H 0.8227 0.4034 0.3678 0.132 Uiso 1 1 calc R U . . .
H50 H 0.8410 0.5186 0.3501 0.132 Uiso 1 1 calc R U . . .
H51 H 0.8325 0.5111 0.3992 0.132 Uiso 1 1 calc R U . . .
C121 C 0.64304(10) 0.1924(2) 0.45956(9) 0.0326(6) Uani 1 1 d . . . . .
C122 C 0.68248(11) 0.1370(3) 0.44950(10) 0.0412(8) Uani 1 1 d . . . . .
H52 H 0.7088 0.1800 0.4434 0.049 Uiso 1 1 calc R U . . .
C123 C 0.68493(12) 0.0203(3) 0.44799(11) 0.0430(8) Uani 1 1 d . . . . .
H53 H 0.7129 -0.0139 0.4410 0.052 Uiso 1 1 calc R U . . .
C124 C 0.64785(12) -0.0475(3) 0.45637(10) 0.0390(7) Uani 1 1 d . . . . .
C125 C 0.60853(13) 0.0085(3) 0.46704(12) 0.0497(9) Uani 1 1 d . . . . .
H54 H 0.5824 -0.0345 0.4734 0.060 Uiso 1 1 calc R U . . .
C126 C 0.60614(13) 0.1246(3) 0.46869(12) 0.0474(8) Uani 1 1 d . . . . .
H55 H 0.5785 0.1589 0.4763 0.057 Uiso 1 1 calc R U . . .
C127 C 0.65087(13) -0.1765(3) 0.45517(12) 0.0482(8) Uani 1 1 d . . . . .
C128 C 0.6784(3) -0.2175(4) 0.4213(2) 0.119(2) Uani 1 1 d . U . . .
H56 H 0.7101 -0.1799 0.4258 0.143 Uiso 1 1 calc R U . . .
H57 H 0.6833 -0.2990 0.4242 0.143 Uiso 1 1 calc R U . . .
H58 H 0.6597 -0.2001 0.3918 0.143 Uiso 1 1 calc R U . . .
C129 C 0.60225(18) -0.2331(4) 0.4487(2) 0.0964(17) Uani 1 1 d . . . . .
H59 H 0.5849 -0.2059 0.4708 0.116 Uiso 1 1 calc R U . . .
H60 H 0.5833 -0.2158 0.4194 0.116 Uiso 1 1 calc R U . . .
H61 H 0.6068 -0.3147 0.4518 0.116 Uiso 1 1 calc R U . . .
C130 C 0.6805(2) -0.2171(4) 0.49945(19) 0.111(2) Uani 1 1 d . . . . .
H62 H 0.7127 -0.1819 0.5050 0.133 Uiso 1 1 calc R U . . .
H63 H 0.6636 -0.1961 0.5228 0.133 Uiso 1 1 calc R U . . .
H64 H 0.6840 -0.2990 0.4989 0.133 Uiso 1 1 calc R U . . .
C131 C 0.66106(10) 0.3547(2) 0.51328(9) 0.0326(6) Uani 1 1 d . . . . .
C132 C 0.68489(11) 0.2799(3) 0.54431(9) 0.0376(7) Uani 1 1 d . . . . .
H65 H 0.6898 0.2047 0.5360 0.045 Uiso 1 1 calc R U . . .
C133 C 0.70182(12) 0.3127(3) 0.58749(10) 0.0406(7) Uani 1 1 d . . . . .
H66 H 0.7182 0.2589 0.6079 0.049 Uiso 1 1 calc R U . . .
C134 C 0.69580(11) 0.4212(3) 0.60210(10) 0.0363(7) Uani 1 1 d . . . . .
C135 C 0.67167(13) 0.4957(3) 0.57061(10) 0.0456(8) Uani 1 1 d . . . . .
H67 H 0.6667 0.5711 0.5788 0.055 Uiso 1 1 calc R U . . .
C136 C 0.65466(13) 0.4628(3) 0.52760(10) 0.0436(8) Uani 1 1 d . . . . .
H68 H 0.6380 0.5162 0.5072 0.052 Uiso 1 1 calc R U . . .
C137 C 0.71556(12) 0.4574(3) 0.64979(10) 0.0445(8) Uani 1 1 d . . . . .
C138 C 0.72249(17) 0.3557(4) 0.68083(12) 0.0695(12) Uani 1 1 d . . . . .
H69 H 0.6913 0.3171 0.6788 0.083 Uiso 1 1 calc R U . . .
H70 H 0.7460 0.3037 0.6725 0.083 Uiso 1 1 calc R U . . .
H71 H 0.7345 0.3814 0.7110 0.083 Uiso 1 1 calc R U . . .
C139 C 0.76382(17) 0.5161(5) 0.65322(15) 0.0903(17) Uani 1 1 d . . . . .
H72 H 0.7597 0.5812 0.6335 0.108 Uiso 1 1 calc R U . . .
H73 H 0.7758 0.5415 0.6834 0.108 Uiso 1 1 calc R U . . .
H74 H 0.7873 0.4638 0.6450 0.108 Uiso 1 1 calc R U . . .
C140 C 0.67935(16) 0.5362(4) 0.66590(13) 0.0678(11) Uani 1 1 d . . . . .
H75 H 0.6482 0.4975 0.6636 0.081 Uiso 1 1 calc R U . . .
H76 H 0.6923 0.5568 0.6965 0.081 Uiso 1 1 calc R U . . .
H77 H 0.6746 0.6043 0.6478 0.081 Uiso 1 1 calc R U . . .


_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
Mg1 O11 2.049(2) . ?
Mg1 O11 2.049(2) 2_655 ?
Mg1 O4 2.070(3) . ?
Mg1 O4 2.070(3) 2_655 ?
Mg1 O3 2.090(2) . ?
Mg1 O3 2.090(2) 2_655 ?
O1 C17 1.222(3) . ?
O2 C27 1.223(4) . ?
O3 C31 1.430(4) . ?
O3 H3 0.83(4) . ?
O4 C41 1.429(4) . ?
O4 H4 0.82(4) . ?
O5 C51 1.400(7) . ?
O5 H5 0.81(5) . ?
O6 C61 1.413(6) . ?
O6 H6 0.87(6) . ?
O11 C1 1.274(4) . ?
O12 C1 1.247(4) . ?
N1 C17 1.358(4) . ?
N1 C12 1.423(4) . ?
N1 H1 0.82(3) . ?
N2 C27 1.359(4) . ?
N2 C16 1.417(4) . ?
N2 H2 0.84(3) . ?
C1 C11 1.501(4) . ?
C11 C12 1.409(4) . ?
C11 C16 1.414(4) . ?
C12 C13 1.393(4) . ?
C13 C14 1.372(4) . ?
C13 H7 0.9500 . ?
C14 C15 1.381(4) . ?
C14 H8 0.9500 . ?
C15 C16 1.391(4) . ?
C15 H9 0.9500 . ?
C17 C18 1.564(4) . ?
C18 C111 1.544(4) . ?
C18 C121 1.549(4) . ?
C18 C131 1.551(4) . ?
C21 C22 1.505(6) . ?
C21 C28 1.516(5) . ?
C21 H12 0.9900 . ?
C21 H13 0.9900 . ?
C22 C23 1.524(7) . ?
C22 H14 0.9900 . ?
C22 H15 0.9900 . ?
C23 H16 0.9800 . ?
C23 H17 0.9800 . ?
C23 H18 0.9800 . ?
C27 C28 1.511(5) . ?
C28 H10 0.9900 . ?
C28 H11 0.9900 . ?
C31 C32 1.479(6) . ?
C31 H19 0.9900 . ?
C31 H20 0.9900 . ?
C32 H21 0.9800 . ?
C32 H22 0.9800 . ?
C32 H23 0.9800 . ?
C41 C42 1.489(5) . ?
C41 H24 0.9900 . ?
C41 H25 0.9900 . ?
C42 H26 0.9800 . ?
C42 H27 0.9800 . ?
C42 H28 0.9800 . ?
C51 C52 1.385(6) . ?
C51 H29 0.9900 . ?
C51 H30 0.9900 . ?
C52 H31 0.9800 . ?
C52 H32 0.9800 . ?
C52 H33 0.9800 . ?
C61 C62 1.461(7) . ?
C61 H34 0.9900 . ?
C61 H35 0.9900 . ?
C62 H36 0.9800 . ?
C62 H37 0.9800 . ?
C62 H38 0.9800 . ?
C111 C116 1.397(4) . ?
C111 C112 1.398(4) . ?
C112 C113 1.382(4) . ?
C112 H39 0.9500 . ?
C113 C114 1.390(5) . ?
C113 H40 0.9500 . ?
C114 C115 1.391(5) . ?
C114 C117 1.540(4) . ?
C115 C116 1.386(4) . ?
C115 H41 0.9500 . ?
C116 H42 0.9500 . ?
C117 C119 1.474(6) . ?
C117 C120 1.519(6) . ?
C117 C118 1.522(6) . ?
C118 H43 0.9800 . ?
C118 H44 0.9800 . ?
C118 H45 0.9800 . ?
C119 H46 0.9800 . ?
C119 H47 0.9800 . ?
C119 H48 0.9800 . ?
C120 H49 0.9800 . ?
C120 H50 0.9800 . ?
C120 H51 0.9800 . ?
C121 C122 1.382(4) . ?
C121 C126 1.390(4) . ?
C122 C123 1.389(4) . ?
C122 H52 0.9500 . ?
C123 C124 1.386(4) . ?
C123 H53 0.9500 . ?
C124 C125 1.390(5) . ?
C124 C127 1.537(4) . ?
C125 C126 1.383(5) . ?
C125 H54 0.9500 . ?
C126 H55 0.9500 . ?
C127 C129 1.500(6) . ?
C127 C128 1.517(6) . ?
C127 C130 1.534(6) . ?
C128 H56 0.9800 . ?
C128 H57 0.9800 . ?
C128 H58 0.9800 . ?
C129 H59 0.9800 . ?
C129 H60 0.9800 . ?
C129 H61 0.9800 . ?
C130 H62 0.9800 . ?
C130 H63 0.9800 . ?
C130 H64 0.9800 . ?
C131 C132 1.380(4) . ?
C131 C136 1.385(4) . ?
C132 C133 1.388(4) . ?
C132 H65 0.9500 . ?
C133 C134 1.389(4) . ?
C133 H66 0.9500 . ?
C134 C135 1.390(5) . ?
C134 C137 1.537(4) . ?
C135 C136 1.383(4) . ?
C135 H67 0.9500 . ?
C136 H68 0.9500 . ?
C137 C139 1.511(5) . ?
C137 C138 1.535(5) . ?
C137 C140 1.543(5) . ?
C138 H69 0.9800 . ?
C138 H70 0.9800 . ?
C138 H71 0.9800 . ?
C139 H72 0.9800 . ?
C139 H73 0.9800 . ?
C139 H74 0.9800 . ?
C140 H75 0.9800 . ?
C140 H76 0.9800 . ?
C140 H77 0.9800 . ?

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
O11 Mg1 O11 93.68(13) . 2_655 ?
O11 Mg1 O4 176.38(10) . . ?
O11 Mg1 O4 88.92(9) 2_655 . ?
O11 Mg1 O4 88.92(9) . 2_655 ?
O11 Mg1 O4 176.38(10) 2_655 2_655 ?
O4 Mg1 O4 88.59(15) . 2_655 ?
O11 Mg1 O3 87.12(9) . . ?
O11 Mg1 O3 89.73(9) 2_655 . ?
O4 Mg1 O3 90.38(10) . . ?
O4 Mg1 O3 92.92(10) 2_655 . ?
O11 Mg1 O3 89.73(9) . 2_655 ?
O11 Mg1 O3 87.12(9) 2_655 2_655 ?
O4 Mg1 O3 92.92(10) . 2_655 ?
O4 Mg1 O3 90.38(10) 2_655 2_655 ?
O3 Mg1 O3 175.39(16) . 2_655 ?
C31 O3 Mg1 133.3(2) . . ?
C31 O3 H3 107(3) . . ?
Mg1 O3 H3 110(3) . . ?
C41 O4 Mg1 127.2(2) . . ?
C41 O4 H4 107(3) . . ?
Mg1 O4 H4 125(3) . . ?
C51 O5 H5 117(4) . . ?
C61 O6 H6 99(4) . . ?
C1 O11 Mg1 134.28(19) . . ?
C17 N1 C12 122.6(2) . . ?
C17 N1 H1 119(2) . . ?
C12 N1 H1 116(2) . . ?
C27 N2 C16 128.0(3) . . ?
C27 N2 H2 118(2) . . ?
C16 N2 H2 114(2) . . ?
O12 C1 O11 123.9(3) . . ?
O12 C1 C11 119.8(3) . . ?
O11 C1 C11 116.3(3) . . ?
C12 C11 C16 118.0(3) . . ?
C12 C11 C1 120.5(3) . . ?
C16 C11 C1 121.4(3) . . ?
C13 C12 C11 120.3(3) . . ?
C13 C12 N1 119.3(3) . . ?
C11 C12 N1 120.4(2) . . ?
C14 C13 C12 120.3(3) . . ?
C14 C13 H7 119.8 . . ?
C12 C13 H7 119.8 . . ?
C13 C14 C15 121.0(3) . . ?
C13 C14 H8 119.5 . . ?
C15 C14 H8 119.5 . . ?
C14 C15 C16 119.7(3) . . ?
C14 C15 H9 120.2 . . ?
C16 C15 H9 120.2 . . ?
C15 C16 C11 120.7(3) . . ?
C15 C16 N2 120.3(3) . . ?
C11 C16 N2 118.9(3) . . ?
O1 C17 N1 122.1(3) . . ?
O1 C17 C18 119.4(3) . . ?
N1 C17 C18 118.3(2) . . ?
C111 C18 C121 109.6(2) . . ?
C111 C18 C131 110.5(2) . . ?
C121 C18 C131 109.8(2) . . ?
C111 C18 C17 112.6(2) . . ?
C121 C18 C17 110.4(2) . . ?
C131 C18 C17 103.8(2) . . ?
C22 C21 C28 114.6(3) . . ?
C22 C21 H12 108.6 . . ?
C28 C21 H12 108.6 . . ?
C22 C21 H13 108.6 . . ?
C28 C21 H13 108.6 . . ?
H12 C21 H13 107.6 . . ?
C21 C22 C23 114.6(4) . . ?
C21 C22 H14 108.6 . . ?
C23 C22 H14 108.6 . . ?
C21 C22 H15 108.6 . . ?
C23 C22 H15 108.6 . . ?
H14 C22 H15 107.6 . . ?
C22 C23 H16 109.5 . . ?
C22 C23 H17 109.5 . . ?
H16 C23 H17 109.5 . . ?
C22 C23 H18 109.5 . . ?
H16 C23 H18 109.5 . . ?
H17 C23 H18 109.5 . . ?
O2 C27 N2 123.5(3) . . ?
O2 C27 C28 122.5(3) . . ?
N2 C27 C28 114.0(3) . . ?
C27 C28 C21 113.2(3) . . ?
C27 C28 H10 108.9 . . ?
C21 C28 H10 108.9 . . ?
C27 C28 H11 108.9 . . ?
C21 C28 H11 108.9 . . ?
H10 C28 H11 107.8 . . ?
O3 C31 C32 111.2(4) . . ?
O3 C31 H19 109.4 . . ?
C32 C31 H19 109.4 . . ?
O3 C31 H20 109.4 . . ?
C32 C31 H20 109.4 . . ?
H19 C31 H20 108.0 . . ?
C31 C32 H21 109.5 . . ?
C31 C32 H22 109.5 . . ?
H21 C32 H22 109.5 . . ?
C31 C32 H23 109.5 . . ?
H21 C32 H23 109.5 . . ?
H22 C32 H23 109.5 . . ?
O4 C41 C42 112.4(3) . . ?
O4 C41 H24 109.1 . . ?
C42 C41 H24 109.1 . . ?
O4 C41 H25 109.1 . . ?
C42 C41 H25 109.1 . . ?
H24 C41 H25 107.9 . . ?
C41 C42 H26 109.5 . . ?
C41 C42 H27 109.5 . . ?
H26 C42 H27 109.5 . . ?
C41 C42 H28 109.5 . . ?
H26 C42 H28 109.5 . . ?
H27 C42 H28 109.5 . . ?
C52 C51 O5 122.1(7) . . ?
C52 C51 H29 106.8 . . ?
O5 C51 H29 106.8 . . ?
C52 C51 H30 106.8 . . ?
O5 C51 H30 106.8 . . ?
H29 C51 H30 106.6 . . ?
C51 C52 H31 109.5 . . ?
C51 C52 H32 109.5 . . ?
H31 C52 H32 109.5 . . ?
C51 C52 H33 109.5 . . ?
H31 C52 H33 109.5 . . ?
H32 C52 H33 109.5 . . ?
O6 C61 C62 111.7(5) . . ?
O6 C61 H34 109.3 . . ?
C62 C61 H34 109.3 . . ?
O6 C61 H35 109.3 . . ?
C62 C61 H35 109.3 . . ?
H34 C61 H35 107.9 . . ?
C61 C62 H36 109.5 . . ?
C61 C62 H37 109.5 . . ?
H36 C62 H37 109.5 . . ?
C61 C62 H38 109.5 . . ?
H36 C62 H38 109.5 . . ?
H37 C62 H38 109.5 . . ?
C116 C111 C112 116.1(3) . . ?
C116 C111 C18 123.5(3) . . ?
C112 C111 C18 120.4(3) . . ?
C113 C112 C111 122.2(3) . . ?
C113 C112 H39 118.9 . . ?
C111 C112 H39 118.9 . . ?
C112 C113 C114 121.6(3) . . ?
C112 C113 H40 119.2 . . ?
C114 C113 H40 119.2 . . ?
C113 C114 C115 116.4(3) . . ?
C113 C114 C117 122.9(3) . . ?
C115 C114 C117 120.6(3) . . ?
C116 C115 C114 122.2(3) . . ?
C116 C115 H41 118.9 . . ?
C114 C115 H41 118.9 . . ?
C115 C116 C111 121.4(3) . . ?
C115 C116 H42 119.3 . . ?
C111 C116 H42 119.3 . . ?
C119 C117 C120 112.4(5) . . ?
C119 C117 C118 108.4(5) . . ?
C120 C117 C118 104.6(4) . . ?
C119 C117 C114 109.4(3) . . ?
C120 C117 C114 109.5(3) . . ?
C118 C117 C114 112.6(3) . . ?
C117 C118 H43 109.5 . . ?
C117 C118 H44 109.5 . . ?
H43 C118 H44 109.5 . . ?
C117 C118 H45 109.5 . . ?
H43 C118 H45 109.5 . . ?
H44 C118 H45 109.5 . . ?
C117 C119 H46 109.5 . . ?
C117 C119 H47 109.5 . . ?
H46 C119 H47 109.5 . . ?
C117 C119 H48 109.5 . . ?
H46 C119 H48 109.5 . . ?
H47 C119 H48 109.5 . . ?
C117 C120 H49 109.5 . . ?
C117 C120 H50 109.5 . . ?
H49 C120 H50 109.5 . . ?
C117 C120 H51 109.5 . . ?
H49 C120 H51 109.5 . . ?
H50 C120 H51 109.5 . . ?
C122 C121 C126 116.1(3) . . ?
C122 C121 C18 120.5(3) . . ?
C126 C121 C18 123.1(3) . . ?
C121 C122 C123 122.1(3) . . ?
C121 C122 H52 119.0 . . ?
C123 C122 H52 119.0 . . ?
C124 C123 C122 122.0(3) . . ?
C124 C123 H53 119.0 . . ?
C122 C123 H53 119.0 . . ?
C123 C124 C125 115.8(3) . . ?
C123 C124 C127 121.9(3) . . ?
C125 C124 C127 122.3(3) . . ?
C126 C125 C124 122.3(3) . . ?
C126 C125 H54 118.9 . . ?
C124 C125 H54 118.9 . . ?
C125 C126 C121 121.8(3) . . ?
C125 C126 H55 119.1 . . ?
C121 C126 H55 119.1 . . ?
C129 C127 C128 110.3(4) . . ?
C129 C127 C130 106.7(4) . . ?
C128 C127 C130 105.5(5) . . ?
C129 C127 C124 113.4(3) . . ?
C128 C127 C124 112.1(3) . . ?
C130 C127 C124 108.3(3) . . ?
C127 C128 H56 109.5 . . ?
C127 C128 H57 109.5 . . ?
H56 C128 H57 109.5 . . ?
C127 C128 H58 109.5 . . ?
H56 C128 H58 109.5 . . ?
H57 C128 H58 109.5 . . ?
C127 C129 H59 109.5 . . ?
C127 C129 H60 109.5 . . ?
H59 C129 H60 109.5 . . ?
C127 C129 H61 109.5 . . ?
H59 C129 H61 109.5 . . ?
H60 C129 H61 109.5 . . ?
C127 C130 H62 109.5 . . ?
C127 C130 H63 109.5 . . ?
H62 C130 H63 109.5 . . ?
C127 C130 H64 109.5 . . ?
H62 C130 H64 109.5 . . ?
H63 C130 H64 109.5 . . ?
C132 C131 C136 116.6(3) . . ?
C132 C131 C18 122.5(3) . . ?
C136 C131 C18 120.8(3) . . ?
C131 C132 C133 121.2(3) . . ?
C131 C132 H65 119.4 . . ?
C133 C132 H65 119.4 . . ?
C132 C133 C134 122.6(3) . . ?
C132 C133 H66 118.7 . . ?
C134 C133 H66 118.7 . . ?
C133 C134 C135 115.7(3) . . ?
C133 C134 C137 122.2(3) . . ?
C135 C134 C137 122.0(3) . . ?
C136 C135 C134 121.6(3) . . ?
C136 C135 H67 119.2 . . ?
C134 C135 H67 119.2 . . ?
C135 C136 C131 122.2(3) . . ?
C135 C136 H68 118.9 . . ?
C131 C136 H68 118.9 . . ?
C139 C137 C138 109.0(4) . . ?
C139 C137 C134 109.6(3) . . ?
C138 C137 C134 111.3(3) . . ?
C139 C137 C140 109.9(4) . . ?
C138 C137 C140 106.1(3) . . ?
C134 C137 C140 110.8(3) . . ?
C137 C138 H69 109.5 . . ?
C137 C138 H70 109.5 . . ?
H69 C138 H70 109.5 . . ?
C137 C138 H71 109.5 . . ?
H69 C138 H71 109.5 . . ?
H70 C138 H71 109.5 . . ?
C137 C139 H72 109.5 . . ?
C137 C139 H73 109.5 . . ?
H72 C139 H73 109.5 . . ?
C137 C139 H74 109.5 . . ?
H72 C139 H74 109.5 . . ?
H73 C139 H74 109.5 . . ?
C137 C140 H75 109.5 . . ?
C137 C140 H76 109.5 . . ?
H75 C140 H76 109.5 . . ?
C137 C140 H77 109.5 . . ?
H75 C140 H77 109.5 . . ?
H76 C140 H77 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
Mg1 O11 C1 O12 22.5(5) . . . . ?
Mg1 O11 C1 C11 -156.3(2) . . . . ?
O12 C1 C11 C12 -35.6(4) . . . . ?
O11 C1 C11 C12 143.3(3) . . . . ?
O12 C1 C11 C16 148.3(3) . . . . ?
O11 C1 C11 C16 -32.8(4) . . . . ?
C16 C11 C12 C13 0.4(4) . . . . ?
C1 C11 C12 C13 -175.8(3) . . . . ?
C16 C11 C12 N1 -178.5(3) . . . . ?
C1 C11 C12 N1 5.2(4) . . . . ?
C17 N1 C12 C13 46.2(4) . . . . ?
C17 N1 C12 C11 -134.9(3) . . . . ?
C11 C12 C13 C14 0.7(5) . . . . ?
N1 C12 C13 C14 179.7(3) . . . . ?
C12 C13 C14 C15 -1.0(5) . . . . ?
C13 C14 C15 C16 0.1(5) . . . . ?
C14 C15 C16 C11 1.1(5) . . . . ?
C14 C15 C16 N2 178.4(3) . . . . ?
C12 C11 C16 C15 -1.3(4) . . . . ?
C1 C11 C16 C15 174.9(3) . . . . ?
C12 C11 C16 N2 -178.7(3) . . . . ?
C1 C11 C16 N2 -2.5(4) . . . . ?
C27 N2 C16 C15 30.8(5) . . . . ?
C27 N2 C16 C11 -151.8(3) . . . . ?
C12 N1 C17 O1 2.4(4) . . . . ?
C12 N1 C17 C18 -173.4(2) . . . . ?
O1 C17 C18 C111 -177.3(3) . . . . ?
N1 C17 C18 C111 -1.4(4) . . . . ?
O1 C17 C18 C121 59.9(3) . . . . ?
N1 C17 C18 C121 -124.2(3) . . . . ?
O1 C17 C18 C131 -57.7(3) . . . . ?
N1 C17 C18 C131 118.2(3) . . . . ?
C28 C21 C22 C23 58.8(5) . . . . ?
C16 N2 C27 O2 4.3(5) . . . . ?
C16 N2 C27 C28 -174.1(3) . . . . ?
O2 C27 C28 C21 33.0(5) . . . . ?
N2 C27 C28 C21 -148.6(3) . . . . ?
C22 C21 C28 C27 66.2(5) . . . . ?
Mg1 O3 C31 C32 -108.7(4) . . . . ?
Mg1 O4 C41 C42 98.7(4) . . . . ?
C121 C18 C111 C116 -121.3(3) . . . . ?
C131 C18 C111 C116 -0.2(4) . . . . ?
C17 C18 C111 C116 115.4(3) . . . . ?
C121 C18 C111 C112 57.8(3) . . . . ?
C131 C18 C111 C112 178.9(3) . . . . ?
C17 C18 C111 C112 -65.5(3) . . . . ?
C116 C111 C112 C113 -1.8(4) . . . . ?
C18 C111 C112 C113 179.0(3) . . . . ?
C111 C112 C113 C114 1.3(5) . . . . ?
C112 C113 C114 C115 0.7(5) . . . . ?
C112 C113 C114 C117 -178.8(3) . . . . ?
C113 C114 C115 C116 -2.0(5) . . . . ?
C117 C114 C115 C116 177.5(3) . . . . ?
C114 C115 C116 C111 1.5(5) . . . . ?
C112 C111 C116 C115 0.5(4) . . . . ?
C18 C111 C116 C115 179.6(3) . . . . ?
C113 C114 C117 C119 114.0(5) . . . . ?
C115 C114 C117 C119 -65.5(6) . . . . ?
C113 C114 C117 C120 -122.4(4) . . . . ?
C115 C114 C117 C120 58.2(5) . . . . ?
C113 C114 C117 C118 -6.6(5) . . . . ?
C115 C114 C117 C118 174.0(4) . . . . ?
C111 C18 C121 C122 27.2(4) . . . . ?
C131 C18 C121 C122 -94.4(3) . . . . ?
C17 C18 C121 C122 151.8(3) . . . . ?
C111 C18 C121 C126 -158.7(3) . . . . ?
C131 C18 C121 C126 79.7(4) . . . . ?
C17 C18 C121 C126 -34.1(4) . . . . ?
C126 C121 C122 C123 0.8(5) . . . . ?
C18 C121 C122 C123 175.3(3) . . . . ?
C121 C122 C123 C124 0.2(5) . . . . ?
C122 C123 C124 C125 -1.0(5) . . . . ?
C122 C123 C124 C127 -179.3(3) . . . . ?
C123 C124 C125 C126 0.8(5) . . . . ?
C127 C124 C125 C126 179.1(3) . . . . ?
C124 C125 C126 C121 0.2(6) . . . . ?
C122 C121 C126 C125 -1.0(5) . . . . ?
C18 C121 C126 C125 -175.4(3) . . . . ?
C123 C124 C127 C129 -159.0(4) . . . . ?
C125 C124 C127 C129 22.8(5) . . . . ?
C123 C124 C127 C128 -33.2(5) . . . . ?
C125 C124 C127 C128 148.6(4) . . . . ?
C123 C124 C127 C130 82.8(5) . . . . ?
C125 C124 C127 C130 -95.4(5) . . . . ?
C111 C18 C131 C132 -105.0(3) . . . . ?
C121 C18 C131 C132 16.0(4) . . . . ?
C17 C18 C131 C132 134.0(3) . . . . ?
C111 C18 C131 C136 73.2(3) . . . . ?
C121 C18 C131 C136 -165.8(3) . . . . ?
C17 C18 C131 C136 -47.8(3) . . . . ?
C136 C131 C132 C133 -0.6(4) . . . . ?
C18 C131 C132 C133 177.7(3) . . . . ?
C131 C132 C133 C134 0.3(5) . . . . ?
C132 C133 C134 C135 -0.1(5) . . . . ?
C132 C133 C134 C137 -178.8(3) . . . . ?
C133 C134 C135 C136 0.4(5) . . . . ?
C137 C134 C135 C136 179.0(3) . . . . ?
C134 C135 C136 C131 -0.7(5) . . . . ?
C132 C131 C136 C135 0.8(5) . . . . ?
C18 C131 C136 C135 -177.5(3) . . . . ?
C133 C134 C137 C139 97.5(4) . . . . ?
C135 C134 C137 C139 -81.1(4) . . . . ?
C133 C134 C137 C138 -23.2(4) . . . . ?
C135 C134 C137 C138 158.3(3) . . . . ?
C133 C134 C137 C140 -141.0(3) . . . . ?
C135 C134 C137 C140 40.4(4) . . . . ?

_refine_diff_density_max         0.893
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.060

_shelxl_version_number           2014/6
_chemical_properties_physical    Efflorescent
####################################################################### 
# 
# 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/access/V1 
# 
# Audit and citation data items may have 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_MgL22(EtOH)-5(EtOH)
_database_code_depnum_ccdc_archive 'CCDC 1042064'
_audit_update_record             
;
2015-01-05 deposited with the CCDC.
2015-03-18 downloaded from the CCDC.
;
_audit_creation_date             2014-11-01
_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        
; 
[{(t-BuC6H4)3CCONHC6H4COO}2Mg(EtOH)4]-5(EtOH)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C96 H142 Mg N2 O15'
_chemical_formula_sum            'C96 H142 Mg N2 O15'
_chemical_formula_weight         1588.42

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'
Mg Mg 0.0486 0.0363 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.5903(5)
_cell_length_b                   27.0129(9)
_cell_length_c                   25.7904(17)
_cell_angle_alpha                90
_cell_angle_beta                 112.681(7)
_cell_angle_gamma                90
_cell_volume                     9378.6(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    200
_cell_measurement_reflns_used    32980
_cell_measurement_theta_min      3.02
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_F_000             3456
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.080
_shelx_estimated_absorpt_T_min   0.984
_shelx_estimated_absorpt_T_max   0.992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9841
_exptl_absorpt_correction_T_max  0.9920
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   
;
 MicroMax-007HF microfocus rotating anode X-ray generator
;
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            72173
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.016
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.972
_reflns_number_total             16494
_reflns_number_gt                11025
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'RAPID AUTO (Rigaku, 2006)'
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2006)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2006)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1152P)²+10.5406P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16494
_refine_ls_number_parameters     1124
_refine_ls_number_restraints     86
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.0852
_refine_ls_wR_factor_ref         0.2429
_refine_ls_wR_factor_gt          0.2156
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

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
Mg1 Mg 0.80721(9) 0.72646(6) 0.42332(5) 0.0567(4) Uani 1 1 d . . . . .
O1 O 0.29948(17) 0.88751(10) 0.31229(10) 0.0497(6) Uani 1 1 d . . . . .
O2 O 1.30935(18) 0.58690(10) 0.44652(12) 0.0598(8) Uani 1 1 d . . . . .
O3 O 0.8117(2) 0.78848(13) 0.47123(13) 0.0752(10) Uani 1 1 d D U . . .
H201 H 0.752(3) 0.7997(15) 0.4548(19) 0.090 Uiso 1 1 d . U . . .
O4 O 0.79491(19) 0.66694(11) 0.36957(12) 0.0571(7) Uani 1 1 d D . . . .
H202 H 0.850(2) 0.6539(15) 0.3819(18) 0.069 Uiso 1 1 d D U . . .
O5 O 0.7638(2) 0.68231(15) 0.47573(14) 0.0868(11) Uani 1 1 d D . . . .
H203 H 0.7059(14) 0.6806(10) 0.4722(9) 0.104 Uiso 1 1 d D U . . .
O6 O 0.8557(2) 0.77103(11) 0.37131(12) 0.0688(8) Uani 1 1 d D . . . .
H204 H 0.872(3) 0.7965(7) 0.3884(8) 0.083 Uiso 1 1 d D U . . .
O11 O 0.6639(2) 0.74348(11) 0.37701(11) 0.0634(8) Uani 1 1 d . . . . .
O12 O 0.6277(2) 0.81542(11) 0.40647(11) 0.0622(8) Uani 1 1 d . . . . .
O21 O 0.95319(19) 0.70963(11) 0.46749(11) 0.0616(8) Uani 1 1 d . . . . .
O22 O 0.98216(19) 0.64548(12) 0.42173(13) 0.0697(9) Uani 1 1 d . . . . .
O31 O 0.8471(7) 0.8674(3) 0.3684(4) 0.222(4) Uani 1 1 d D . . . .
O32 O 0.5804(3) 0.67156(14) 0.47307(19) 0.0920(12) Uani 1 1 d . . . . .
H205 H 0.553(5) 0.642(2) 0.467(3) 0.110 Uiso 1 1 d . U . . .
O33 O 0.5066(2) 0.57765(12) 0.46632(14) 0.0695(9) Uani 1 1 d . . . . .
H206 H 0.442(4) 0.5761(18) 0.455(2) 0.083 Uiso 1 1 d . U . . .
O34 O 0.0362(5) 0.8233(6) 0.3808(4) 0.172(7) Uani 0.676(16) 1 d D . P A 1
O34B O 0.0548(12) 0.8718(6) 0.3974(8) 0.111(6) Uani 0.324(16) 1 d D . P A 2
O35 O 0.0988(3) 0.87747(16) 0.30925(19) 0.0988(12) Uani 1 1 d D . . . .
H207 H 0.1595(17) 0.884(2) 0.317(2) 0.119 Uiso 1 1 d D U . . .
N1 N 0.4574(2) 0.85797(10) 0.34580(11) 0.0364(6) Uani 1 1 d . . . . .
H1 H 0.5137 0.8588 0.3753 0.044 Uiso 1 1 calc R U . . .
N2 N 1.16414(19) 0.62080(10) 0.44063(11) 0.0392(7) Uani 1 1 d . . . . .
H2 H 1.0994 0.6173 0.4233 0.047 Uiso 1 1 calc R U . . .
C1 C 0.6113(3) 0.78191(15) 0.37009(15) 0.0483(9) Uani 1 1 d . . . . .
C2 C 1.0108(3) 0.67964(15) 0.45773(15) 0.0485(9) Uani 1 1 d . . . . .
C11 C 0.5259(2) 0.78705(12) 0.31466(14) 0.0384(8) Uani 1 1 d . . . . .
C12 C 0.4521(2) 0.82405(11) 0.30313(13) 0.0328(7) Uani 1 1 d . . . . .
C13 C 0.3792(3) 0.82756(12) 0.24928(14) 0.0399(8) Uani 1 1 d . . . . .
H3 H 0.3296 0.8524 0.2412 0.048 Uiso 1 1 calc R U . . .
C14 C 0.3779(3) 0.79539(13) 0.20739(14) 0.0446(8) Uani 1 1 d . . . . .
H4 H 0.3281 0.7986 0.1707 0.054 Uiso 1 1 calc R U . . .
C15 C 0.4483(3) 0.75870(14) 0.21848(16) 0.0494(9) Uani 1 1 d . . . . .
H5 H 0.4466 0.7362 0.1898 0.059 Uiso 1 1 calc R U . . .
C16 C 0.5210(3) 0.75505(13) 0.27147(16) 0.0454(9) Uani 1 1 d . . . . .
H6 H 0.5696 0.7298 0.2789 0.055 Uiso 1 1 calc R U . . .
C17 C 0.3849(2) 0.88951(12) 0.34632(13) 0.0351(7) Uani 1 1 d . . . . .
C18 C 0.4210(2) 0.92974(12) 0.39304(13) 0.0324(7) Uani 1 1 d . . . . .
C21 C 1.1206(2) 0.68664(13) 0.49037(13) 0.0387(8) Uani 1 1 d . . . . .
C22 C 1.1946(2) 0.65809(12) 0.48154(13) 0.0350(7) Uani 1 1 d . . . . .
C23 C 1.2944(3) 0.66853(13) 0.51282(14) 0.0423(8) Uani 1 1 d . . . . .
H7 H 1.3446 0.6493 0.5076 0.051 Uiso 1 1 calc R U . . .
C24 C 1.3206(3) 0.70664(13) 0.55135(15) 0.0468(9) Uani 1 1 d . . . . .
H8 H 1.3888 0.7137 0.5720 0.056 Uiso 1 1 calc R U . . .
C25 C 1.2486(3) 0.73490(13) 0.56043(15) 0.0481(9) Uani 1 1 d . . . . .
H9 H 1.2671 0.7611 0.5870 0.058 Uiso 1 1 calc R U . . .
C26 C 1.1503(3) 0.72425(13) 0.53030(14) 0.0438(8) Uani 1 1 d . . . . .
H10 H 1.1010 0.7432 0.5369 0.053 Uiso 1 1 calc R U . . .
C27 C 1.2193(2) 0.58951(12) 0.42387(14) 0.0360(7) Uani 1 1 d . . . . .
C28 C 1.1589(2) 0.56027(11) 0.36883(13) 0.0337(7) Uani 1 1 d . . . . .
C31 C 0.8824(7) 0.8067(5) 0.5204(5) 0.103(4) Uani 0.573(16) 1 d D U P B 1
H89 H 0.9109 0.7793 0.5473 0.124 Uiso 0.573(16) 1 calc R U P B 1
H90 H 0.8513 0.8306 0.5378 0.124 Uiso 0.573(16) 1 calc R U P B 1
C31B C 0.8711(9) 0.8329(6) 0.4820(8) 0.139(8) Uani 0.427(16) 1 d D U P B 2
H109 H 0.8585 0.8484 0.4451 0.167 Uiso 0.427(16) 1 calc R U P B 2
H110 H 0.8444 0.8558 0.5027 0.167 Uiso 0.427(16) 1 calc R U P B 2
C32 C 0.9619(7) 0.8316(4) 0.5077(5) 0.172(4) Uani 0.573(16) 1 d D U P B 1
H91 H 1.0122 0.8446 0.5426 0.207 Uiso 0.573(16) 1 calc R U P B 1
H92 H 0.9928 0.8077 0.4908 0.207 Uiso 0.573(16) 1 calc R U P B 1
H93 H 0.9334 0.8589 0.4814 0.207 Uiso 0.573(16) 1 calc R U P B 1
C32B C 0.9619(7) 0.8316(4) 0.5077(5) 0.172(4) Uani 0.427(16) 1 d . . P B 2
H111 H 0.9890 0.8651 0.5109 0.207 Uiso 0.427(16) 1 calc R U P B 2
H112 H 0.9774 0.8180 0.5454 0.207 Uiso 0.427(16) 1 calc R U P B 2
H113 H 0.9915 0.8105 0.4874 0.207 Uiso 0.427(16) 1 calc R U P B 2
C41 C 0.7208(3) 0.62990(18) 0.3495(2) 0.0724(13) Uani 1 1 d . . . . .
H94 H 0.6550 0.6450 0.3418 0.087 Uiso 1 1 calc R U . . .
H95 H 0.7325 0.6045 0.3790 0.087 Uiso 1 1 calc R U . . .
C42 C 0.7193(5) 0.6056(2) 0.2974(3) 0.1029(19) Uani 1 1 d . . . . .
H96 H 0.6670 0.5804 0.2852 0.123 Uiso 1 1 calc R U . . .
H97 H 0.7062 0.6305 0.2677 0.123 Uiso 1 1 calc R U . . .
H98 H 0.7838 0.5900 0.3049 0.123 Uiso 1 1 calc R U . . .
C51 C 0.8264(6) 0.6699(4) 0.5323(4) 0.081(3) Uani 0.660(16) 1 d D . P C 1
H99 H 0.7933 0.6771 0.5585 0.098 Uiso 0.660(16) 1 calc R U P C 1
H100 H 0.8901 0.6882 0.5446 0.098 Uiso 0.660(16) 1 calc R U P C 1
C51B C 0.8079(12) 0.6335(6) 0.5061(6) 0.066(6) Uani 0.340(16) 1 d D . P C 2
H114 H 0.7547 0.6086 0.4990 0.079 Uiso 0.340(16) 1 calc R U P C 2
H115 H 0.8574 0.6203 0.4921 0.079 Uiso 0.340(16) 1 calc R U P C 2
C52 C 0.8419(11) 0.6165(4) 0.5287(7) 0.125(6) Uani 0.660(16) 1 d D . P C 1
H101 H 0.8845 0.6039 0.5659 0.150 Uiso 0.660(16) 1 calc R U P C 1
H102 H 0.7776 0.5994 0.5159 0.150 Uiso 0.660(16) 1 calc R U P C 1
H103 H 0.8737 0.6104 0.5021 0.150 Uiso 0.660(16) 1 calc R U P C 1
C52B C 0.8559(15) 0.6442(9) 0.5672(6) 0.096(7) Uani 0.340(16) 1 d D . P C 2
H116 H 0.8846 0.6137 0.5875 0.116 Uiso 0.340(16) 1 calc R U P C 2
H117 H 0.9086 0.6688 0.5738 0.116 Uiso 0.340(16) 1 calc R U P C 2
H118 H 0.8063 0.6572 0.5806 0.116 Uiso 0.340(16) 1 calc R U P C 2
C61 C 0.8795(7) 0.7548(4) 0.3281(4) 0.059(3) Uani 0.466(11) 1 d D . P D 1
H104 H 0.9061 0.7207 0.3364 0.071 Uiso 0.466(11) 1 calc R U P D 1
H105 H 0.9327 0.7762 0.3255 0.071 Uiso 0.466(11) 1 calc R U P D 1
C61B C 0.8068(7) 0.7826(4) 0.3099(3) 0.083(4) Uani 0.534(11) 1 d D U P D 2
H119 H 0.7345 0.7768 0.2972 0.099 Uiso 0.534(11) 1 calc R U P D 2
H120 H 0.8169 0.8181 0.3039 0.099 Uiso 0.534(11) 1 calc R U P D 2
C62 C 0.7937(9) 0.7550(5) 0.2730(5) 0.055(3) Uani 0.466(11) 1 d D . P D 1
H106 H 0.8154 0.7431 0.2437 0.066 Uiso 0.466(11) 1 calc R U P D 1
H107 H 0.7413 0.7334 0.2750 0.066 Uiso 0.466(11) 1 calc R U P D 1
H108 H 0.7680 0.7888 0.2640 0.066 Uiso 0.466(11) 1 calc R U P D 1
C62B C 0.8465(13) 0.7523(7) 0.2754(7) 0.109(6) Uani 0.534(11) 1 d D U P D 2
H121 H 0.8124 0.7612 0.2357 0.131 Uiso 0.534(11) 1 calc R U P D 2
H122 H 0.9178 0.7585 0.2873 0.131 Uiso 0.534(11) 1 calc R U P D 2
H123 H 0.8354 0.7172 0.2805 0.131 Uiso 0.534(11) 1 calc R U P D 2
C111 C 0.4849(2) 0.90401(11) 0.44866(13) 0.0328(7) Uani 1 1 d . . . . .
C112 C 0.5782(2) 0.91938(12) 0.48407(13) 0.0358(7) Uani 1 1 d . . . . .
H11 H 0.6068 0.9475 0.4740 0.043 Uiso 1 1 calc R U . . .
C113 C 0.6310(2) 0.89507(12) 0.53356(14) 0.0390(8) Uani 1 1 d . . . . .
H12 H 0.6948 0.9071 0.5569 0.047 Uiso 1 1 calc R U . . .
C114 C 0.5937(3) 0.85330(12) 0.55046(14) 0.0380(8) Uani 1 1 d . . . . .
C115 C 0.5004(3) 0.83738(13) 0.51453(14) 0.0422(8) Uani 1 1 d . . . . .
H13 H 0.4723 0.8089 0.5243 0.051 Uiso 1 1 calc R U . . .
C116 C 0.4476(3) 0.86168(12) 0.46515(14) 0.0408(8) Uani 1 1 d . . . . .
H14 H 0.3841 0.8495 0.4416 0.049 Uiso 1 1 calc R U . . .
C117 C 0.6530(3) 0.82483(14) 0.60440(15) 0.0465(9) Uani 1 1 d . . . . .
C118 C 0.6942(4) 0.7773(2) 0.5895(2) 0.0895(17) Uani 1 1 d . . . . .
H15 H 0.7374 0.7856 0.5696 0.107 Uiso 1 1 calc R U . . .
H16 H 0.7326 0.7592 0.6240 0.107 Uiso 1 1 calc R U . . .
H17 H 0.6391 0.7566 0.5653 0.107 Uiso 1 1 calc R U . . .
C119 C 0.7409(4) 0.8546(2) 0.6442(2) 0.098(2) Uani 1 1 d . . . . .
H18 H 0.7835 0.8647 0.6246 0.118 Uiso 1 1 calc R U . . .
H19 H 0.7163 0.8841 0.6569 0.118 Uiso 1 1 calc R U . . .
H20 H 0.7793 0.8342 0.6768 0.118 Uiso 1 1 calc R U . . .
C120 C 0.5879(4) 0.8094(2) 0.6347(2) 0.0938(19) Uani 1 1 d . . . . .
H21 H 0.5315 0.7903 0.6092 0.113 Uiso 1 1 calc R U . . .
H22 H 0.6263 0.7890 0.6672 0.113 Uiso 1 1 calc R U . . .
H23 H 0.5634 0.8389 0.6474 0.113 Uiso 1 1 calc R U . . .
C121 C 0.4789(2) 0.97029(12) 0.37610(12) 0.0330(7) Uani 1 1 d . . . . .
C122 C 0.5029(3) 1.01408(12) 0.40684(14) 0.0394(8) Uani 1 1 d . . . . .
H24 H 0.4824 1.0183 0.4373 0.047 Uiso 1 1 calc R U . . .
C123 C 0.5553(3) 1.05157(12) 0.39456(14) 0.0397(8) Uani 1 1 d . . . . .
H25 H 0.5710 1.0806 0.4171 0.048 Uiso 1 1 calc R U . . .
C124 C 0.5857(3) 1.04767(13) 0.34975(15) 0.0426(8) Uani 1 1 d . . . . .
C125 C 0.5569(3) 1.00538(14) 0.31722(17) 0.0561(11) Uani 1 1 d . . . . .
H26 H 0.5724 1.0024 0.2848 0.067 Uiso 1 1 calc R U . . .
C126 C 0.5058(3) 0.96697(13) 0.33034(16) 0.0483(9) Uani 1 1 d . . . . .
H27 H 0.4892 0.9381 0.3075 0.058 Uiso 1 1 calc R U . . .
C127 C 0.6452(3) 1.08857(14) 0.33554(19) 0.0566(10) Uani 1 1 d . . . . .
C128 C 0.7285(4) 1.06735(18) 0.3225(3) 0.0909(18) Uani 1 1 d . . . . .
H28 H 0.7029 1.0411 0.2943 0.109 Uiso 1 1 calc R U . . .
H29 H 0.7584 1.0935 0.3078 0.109 Uiso 1 1 calc R U . . .
H30 H 0.7788 1.0535 0.3569 0.109 Uiso 1 1 calc R U . . .
C129 C 0.6767(5) 1.12891(19) 0.3781(3) 0.104(2) Uani 1 1 d . . . . .
H31 H 0.6189 1.1411 0.3847 0.124 Uiso 1 1 calc R U . . .
H32 H 0.7262 1.1161 0.4134 0.124 Uiso 1 1 calc R U . . .
H33 H 0.7059 1.1560 0.3643 0.124 Uiso 1 1 calc R U . . .
C130 C 0.5754(4) 1.1149(2) 0.2802(3) 0.0920(17) Uani 1 1 d . . . . .
H34 H 0.5511 1.0906 0.2497 0.110 Uiso 1 1 calc R U . . .
H35 H 0.5189 1.1297 0.2861 0.110 Uiso 1 1 calc R U . . .
H36 H 0.6126 1.1409 0.2702 0.110 Uiso 1 1 calc R U . . .
C131 C 0.3276(2) 0.95495(12) 0.39578(13) 0.0359(7) Uani 1 1 d . . . . .
C132 C 0.3013(3) 0.95243(14) 0.44165(15) 0.0460(9) Uani 1 1 d . . . . .
H37 H 0.3431 0.9354 0.4745 0.055 Uiso 1 1 calc R U . . .
C133 C 0.2142(3) 0.97455(15) 0.44062(16) 0.0517(10) Uani 1 1 d . . . . .
H38 H 0.1982 0.9721 0.4729 0.062 Uiso 1 1 calc R U . . .
C134 C 0.1505(3) 0.99983(14) 0.39428(15) 0.0460(9) Uani 1 1 d . . . . .
C135 C 0.1804(3) 1.00425(14) 0.34944(15) 0.0459(9) Uani 1 1 d . . . . .
H39 H 0.1401 1.0226 0.3173 0.055 Uiso 1 1 calc R U . . .
C136 C 0.2666(3) 0.98289(13) 0.35014(14) 0.0430(8) Uani 1 1 d . . . . .
H40 H 0.2848 0.9873 0.3188 0.052 Uiso 1 1 calc R U . . .
C137 C 0.0497(3) 1.02046(16) 0.39023(18) 0.0574(10) Uani 1 1 d . . . . .
C138 C 0.0368(5) 1.0182(4) 0.4435(3) 0.149(4) Uani 1 1 d . U . . .
H41 H 0.0902 1.0368 0.4721 0.179 Uiso 1 1 calc R U . . .
H42 H -0.0275 1.0326 0.4388 0.179 Uiso 1 1 calc R U . . .
H43 H 0.0390 0.9836 0.4553 0.179 Uiso 1 1 calc R U . . .
C139 C -0.0298(4) 0.9927(3) 0.3456(4) 0.162(4) Uani 1 1 d . . . . .
H44 H -0.0193 0.9948 0.3104 0.195 Uiso 1 1 calc R U . . .
H45 H -0.0280 0.9579 0.3568 0.195 Uiso 1 1 calc R U . . .
H46 H -0.0946 1.0070 0.3403 0.195 Uiso 1 1 calc R U . . .
C140 C 0.0359(6) 1.0731(3) 0.3700(4) 0.163(4) Uani 1 1 d . . . . .
H47 H 0.0444 1.0752 0.3342 0.196 Uiso 1 1 calc R U . . .
H48 H -0.0309 1.0843 0.3648 0.196 Uiso 1 1 calc R U . . .
H49 H 0.0854 1.0942 0.3979 0.196 Uiso 1 1 calc R U . . .
C211 C 1.0656(2) 0.53486(11) 0.37036(13) 0.0326(7) Uani 1 1 d . . . . .
C212 C 1.0568(3) 0.52093(17) 0.41909(16) 0.0633(12) Uani 1 1 d . . . . .
H50 H 1.1077 0.5299 0.4539 0.076 Uiso 1 1 calc R U . . .
C213 C 0.9765(4) 0.49421(18) 0.41942(16) 0.0691(13) Uani 1 1 d . . . . .
H51 H 0.9746 0.4849 0.4545 0.083 Uiso 1 1 calc R U . . .
C214 C 0.8986(3) 0.48050(13) 0.37055(14) 0.0433(8) Uani 1 1 d . . . . .
C215 C 0.9089(3) 0.49319(15) 0.32169(15) 0.0479(9) Uani 1 1 d . . . . .
H52 H 0.8583 0.4842 0.2868 0.058 Uiso 1 1 calc R U . . .
C216 C 0.9911(3) 0.51876(14) 0.32174(14) 0.0457(9) Uani 1 1 d . . . . .
H53 H 0.9963 0.5255 0.2868 0.055 Uiso 1 1 calc R U . . .
C217 C 0.8101(3) 0.45032(15) 0.37172(16) 0.0546(10) Uani 1 1 d . . . . .
C218 C 0.7778(5) 0.4695(3) 0.4180(2) 0.126(3) Uani 1 1 d . . . . .
H54 H 0.8338 0.4675 0.4544 0.152 Uiso 1 1 calc R U . . .
H55 H 0.7563 0.5041 0.4102 0.152 Uiso 1 1 calc R U . . .
H56 H 0.7227 0.4493 0.4189 0.152 Uiso 1 1 calc R U . . .
C219 C 0.7199(3) 0.45474(19) 0.31715(19) 0.0692(12) Uani 1 1 d . . . . .
H57 H 0.6997 0.4895 0.3104 0.083 Uiso 1 1 calc R U . . .
H58 H 0.7364 0.4424 0.2861 0.083 Uiso 1 1 calc R U . . .
H59 H 0.6652 0.4351 0.3197 0.083 Uiso 1 1 calc R U . . .
C220 C 0.8397(4) 0.3960(2) 0.3810(3) 0.115(2) Uani 1 1 d . . . . .
H60 H 0.8980 0.3924 0.4162 0.138 Uiso 1 1 calc R U . . .
H61 H 0.7844 0.3767 0.3833 0.138 Uiso 1 1 calc R U . . .
H62 H 0.8556 0.3839 0.3496 0.138 Uiso 1 1 calc R U . . .
C221 C 1.1364(2) 0.60190(11) 0.32424(13) 0.0333(7) Uani 1 1 d . . . . .
C222 C 1.0453(3) 0.62478(13) 0.29975(15) 0.0444(9) Uani 1 1 d . . . . .
H63 H 0.9914 0.6137 0.3087 0.053 Uiso 1 1 calc R U . . .
C223 C 1.0308(3) 0.66333(14) 0.26256(17) 0.0500(9) Uani 1 1 d . . . . .
H64 H 0.9663 0.6774 0.2457 0.060 Uiso 1 1 calc R U . . .
C224 C 1.1067(3) 0.68250(12) 0.24870(15) 0.0416(8) Uani 1 1 d . . . . .
C225 C 1.1989(3) 0.66066(13) 0.27554(17) 0.0469(9) Uani 1 1 d . . . . .
H65 H 1.2539 0.6734 0.2687 0.056 Uiso 1 1 calc R U . . .
C226 C 1.2137(3) 0.62131(12) 0.31165(16) 0.0434(8) Uani 1 1 d . . . . .
H66 H 1.2780 0.6071 0.3284 0.052 Uiso 1 1 calc R U . . .
C227 C 1.0931(3) 0.72594(14) 0.20886(18) 0.0559(10) Uani 1 1 d . . . . .
C228 C 0.9859(4) 0.7410(2) 0.1791(3) 0.102(2) Uani 1 1 d . . . . .
H67 H 0.9572 0.7482 0.2070 0.122 Uiso 1 1 calc R U . . .
H68 H 0.9819 0.7706 0.1564 0.122 Uiso 1 1 calc R U . . .
H69 H 0.9487 0.7139 0.1548 0.122 Uiso 1 1 calc R U . . .
C229 C 1.1483(5) 0.77083(17) 0.2435(3) 0.0924(17) Uani 1 1 d . . . . .
H70 H 1.2186 0.7625 0.2635 0.111 Uiso 1 1 calc R U . . .
H71 H 1.1424 0.7989 0.2183 0.111 Uiso 1 1 calc R U . . .
H72 H 1.1191 0.7797 0.2707 0.111 Uiso 1 1 calc R U . . .
C230 C 1.1400(5) 0.7144(2) 0.1672(2) 0.0927(18) Uani 1 1 d . . . . .
H73 H 1.2095 0.7048 0.1876 0.111 Uiso 1 1 calc R U . . .
H74 H 1.1039 0.6872 0.1428 0.111 Uiso 1 1 calc R U . . .
H75 H 1.1371 0.7438 0.1444 0.111 Uiso 1 1 calc R U . . .
C231 C 1.2231(2) 0.51804(11) 0.36015(14) 0.0345(7) Uani 1 1 d . . . . .
C232 C 1.2231(3) 0.50708(12) 0.30774(15) 0.0407(8) Uani 1 1 d . . . . .
H76 H 1.1858 0.5272 0.2765 0.049 Uiso 1 1 calc R U . . .
C233 C 1.2769(3) 0.46709(13) 0.29998(16) 0.0450(8) Uani 1 1 d . . . . .
H77 H 1.2748 0.4605 0.2634 0.054 Uiso 1 1 calc R U . . .
C234 C 1.3332(3) 0.43681(12) 0.34393(16) 0.0437(8) Uani 1 1 d . . . . .
C235 C 1.3303(3) 0.44728(14) 0.39629(17) 0.0540(10) Uani 1 1 d . . . . .
H78 H 1.3662 0.4268 0.4275 0.065 Uiso 1 1 calc R U . . .
C236 C 1.2764(3) 0.48681(13) 0.40388(15) 0.0492(9) Uani 1 1 d . . . . .
H79 H 1.2761 0.4926 0.4401 0.059 Uiso 1 1 calc R U . . .
C237 C 1.3958(3) 0.39368(13) 0.33760(19) 0.0543(10) Uani 1 1 d . . . . .
C238 C 1.3867(4) 0.38745(18) 0.2768(2) 0.0850(16) Uani 1 1 d . . . . .
H80 H 1.3170 0.3816 0.2524 0.102 Uiso 1 1 calc R U . . .
H81 H 1.4102 0.4176 0.2646 0.102 Uiso 1 1 calc R U . . .
H82 H 1.4270 0.3592 0.2744 0.102 Uiso 1 1 calc R U . . .
C239 C 1.5043(3) 0.40271(19) 0.3749(3) 0.0880(16) Uani 1 1 d . . . . .
H83 H 1.5447 0.3751 0.3709 0.106 Uiso 1 1 calc R U . . .
H84 H 1.5267 0.4336 0.3636 0.106 Uiso 1 1 calc R U . . .
H85 H 1.5113 0.4053 0.4141 0.106 Uiso 1 1 calc R U . . .
C240 C 1.3628(4) 0.34546(15) 0.3562(3) 0.0931(18) Uani 1 1 d . . . . .
H86 H 1.2930 0.3391 0.3326 0.112 Uiso 1 1 calc R U . . .
H87 H 1.4038 0.3181 0.3524 0.112 Uiso 1 1 calc R U . . .
H88 H 1.3704 0.3483 0.3955 0.112 Uiso 1 1 calc R U . . .
C311 C 0.7728(11) 0.9067(4) 0.3648(6) 0.242(6) Uani 1 1 d D U . . .
H124 H 0.7827 0.9338 0.3417 0.290 Uiso 1 1 calc R U . . .
H125 H 0.7063 0.8926 0.3434 0.290 Uiso 1 1 calc R U . . .
C312 C 0.7693(12) 0.9287(6) 0.4141(6) 0.341(11) Uani 1 1 d D U . . .
H126 H 0.7163 0.9535 0.4035 0.409 Uiso 1 1 calc R U . . .
H127 H 0.7562 0.9030 0.4373 0.409 Uiso 1 1 calc R U . . .
H128 H 0.8332 0.9446 0.4355 0.409 Uiso 1 1 calc R U . . .
C321 C 0.5095(4) 0.71037(19) 0.4561(3) 0.0844(15) Uani 1 1 d . . . . .
H129 H 0.5439 0.7421 0.4569 0.101 Uiso 1 1 calc R U . . .
H130 H 0.4764 0.7129 0.4831 0.101 Uiso 1 1 calc R U . . .
C322 C 0.4356(5) 0.7023(3) 0.4005(3) 0.122(2) Uani 1 1 d . . . . .
H131 H 0.3881 0.7298 0.3903 0.147 Uiso 1 1 calc R U . . .
H132 H 0.4680 0.7005 0.3736 0.147 Uiso 1 1 calc R U . . .
H133 H 0.4005 0.6712 0.3997 0.147 Uiso 1 1 calc R U . . .
C331 C 0.5429(4) 0.54225(19) 0.4374(2) 0.0774(14) Uani 1 1 d . . . . .
H134 H 0.5215 0.5087 0.4435 0.093 Uiso 1 1 calc R U . . .
H135 H 0.6164 0.5429 0.4536 0.093 Uiso 1 1 calc R U . . .
C332 C 0.5075(4) 0.5518(2) 0.3769(2) 0.0800(14) Uani 1 1 d . . . . .
H136 H 0.5343 0.5267 0.3592 0.096 Uiso 1 1 calc R U . . .
H137 H 0.4347 0.5505 0.3604 0.096 Uiso 1 1 calc R U . . .
H138 H 0.5296 0.5847 0.3705 0.096 Uiso 1 1 calc R U . . .
C341 C 0.1303(9) 0.8177(10) 0.4256(7) 0.166(9) Uani 0.676(16) 1 d D . P A 1
H139 H 0.1224 0.8044 0.4594 0.199 Uiso 0.676(16) 1 calc R U P A 1
H140 H 0.1648 0.8500 0.4352 0.199 Uiso 0.676(16) 1 calc R U P A 1
C342 C 0.1881(14) 0.7821(6) 0.4049(8) 0.158(8) Uani 0.676(16) 1 d D . P A 1
H141 H 0.2541 0.7770 0.4345 0.190 Uiso 0.676(16) 1 calc R U P A 1
H142 H 0.1528 0.7504 0.3955 0.190 Uiso 0.676(16) 1 calc R U P A 1
H143 H 0.1951 0.7958 0.3715 0.190 Uiso 0.676(16) 1 calc R U P A 1
C343 C 0.142(2) 0.8511(14) 0.4407(13) 0.19(2) Uani 0.324(16) 1 d D . P A 2
H144 H 0.1249 0.8356 0.4708 0.231 Uiso 0.324(16) 1 calc R U P A 2
H145 H 0.1935 0.8765 0.4575 0.231 Uiso 0.324(16) 1 calc R U P A 2
C344 C 0.174(3) 0.8129(15) 0.4089(17) 0.199(18) Uani 0.324(16) 1 d D U P A 2
H146 H 0.2338 0.7960 0.4347 0.239 Uiso 0.324(16) 1 calc R U P A 2
H147 H 0.1209 0.7886 0.3923 0.239 Uiso 0.324(16) 1 calc R U P A 2
H148 H 0.1889 0.8291 0.3791 0.239 Uiso 0.324(16) 1 calc R U P A 2
C351 C 0.0411(4) 0.8977(2) 0.2552(2) 0.0895(16) Uani 1 1 d . . . . .
H149 H 0.0690 0.8868 0.2276 0.107 Uiso 1 1 calc R U . . .
H150 H 0.0436 0.9343 0.2570 0.107 Uiso 1 1 calc R U . . .
C352 C -0.0637(4) 0.8807(2) 0.2367(3) 0.121(3) Uani 1 1 d . . . . .
H151 H -0.1028 0.8947 0.1997 0.146 Uiso 1 1 calc R U . . .
H152 H -0.0660 0.8445 0.2345 0.146 Uiso 1 1 calc R U . . .
H153 H -0.0914 0.8919 0.2638 0.146 Uiso 1 1 calc R U . . .


_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
Mg1 O11 2.021(3) . ?
Mg1 O21 2.042(3) . ?
Mg1 O3 2.068(3) . ?
Mg1 O5 2.076(4) . ?
Mg1 O4 2.085(3) . ?
Mg1 O6 2.117(4) . ?
Mg1 H201 2.39(5) . ?
O1 C17 1.218(4) . ?
O2 C27 1.217(4) . ?
O3 C31 1.380(9) . ?
O3 C31B 1.442(13) . ?
O3 H201 0.86(5) . ?
O4 C41 1.417(5) . ?
O4 H202 0.816(19) . ?
O5 C51 1.430(9) . ?
O5 C51B 1.542(14) . ?
O5 H203 0.82(2) . ?
O6 C61 1.360(8) . ?
O6 C61B 1.499(8) . ?
O6 H204 0.802(18) . ?
O11 C1 1.262(4) . ?
O12 C1 1.259(4) . ?
O21 C2 1.261(4) . ?
O22 C2 1.261(4) . ?
O31 C311 1.492(11) . ?
O32 C321 1.418(6) . ?
O32 H205 0.89(6) . ?
O33 C331 1.434(6) . ?
O33 H206 0.88(5) . ?
O34 C341 1.420(12) . ?
O34B C343 1.441(19) . ?
O35 C351 1.430(6) . ?
O35 H207 0.85(2) . ?
N1 C17 1.362(4) . ?
N1 C12 1.411(4) . ?
N1 H1 0.8800 . ?
N2 C27 1.348(4) . ?
N2 C22 1.401(4) . ?
N2 H2 0.8800 . ?
C1 C11 1.497(5) . ?
C2 C21 1.507(5) . ?
C11 C16 1.390(5) . ?
C11 C12 1.414(4) . ?
C12 C13 1.389(5) . ?
C13 C14 1.381(5) . ?
C13 H3 0.9500 . ?
C14 C15 1.376(5) . ?
C14 H4 0.9500 . ?
C15 C16 1.373(5) . ?
C15 H5 0.9500 . ?
C16 H6 0.9500 . ?
C17 C18 1.556(4) . ?
C18 C111 1.542(4) . ?
C18 C121 1.546(4) . ?
C18 C131 1.549(4) . ?
C21 C26 1.391(5) . ?
C21 C22 1.414(5) . ?
C22 C23 1.395(5) . ?
C23 C24 1.379(5) . ?
C23 H7 0.9500 . ?
C24 C25 1.389(5) . ?
C24 H8 0.9500 . ?
C25 C26 1.373(5) . ?
C25 H9 0.9500 . ?
C26 H10 0.9500 . ?
C27 C28 1.565(4) . ?
C28 C211 1.538(4) . ?
C28 C231 1.547(4) . ?
C28 C221 1.550(4) . ?
C31 C32 1.481(13) . ?
C31 H89 0.9900 . ?
C31 H90 0.9900 . ?
C31B C32B 1.233(13) . ?
C31B H109 0.9900 . ?
C31B H110 0.9900 . ?
C32 H91 0.9800 . ?
C32 H92 0.9800 . ?
C32 H93 0.9800 . ?
C32B H111 0.9800 . ?
C32B H112 0.9800 . ?
C32B H113 0.9800 . ?
C41 C42 1.488(7) . ?
C41 H94 0.9900 . ?
C41 H95 0.9900 . ?
C42 H96 0.9800 . ?
C42 H97 0.9800 . ?
C42 H98 0.9800 . ?
C51 C52 1.470(13) . ?
C51 H99 0.9900 . ?
C51 H100 0.9900 . ?
C51B C52B 1.485(17) . ?
C51B H114 0.9900 . ?
C51B H115 0.9900 . ?
C52 H101 0.9800 . ?
C52 H102 0.9800 . ?
C52 H103 0.9800 . ?
C52B H116 0.9800 . ?
C52B H117 0.9800 . ?
C52B H118 0.9800 . ?
C61 C62 1.489(13) . ?
C61 H104 0.9900 . ?
C61 H105 0.9900 . ?
C61B C62B 1.480(14) . ?
C61B H119 0.9900 . ?
C61B H120 0.9900 . ?
C62 H106 0.9800 . ?
C62 H107 0.9800 . ?
C62 H108 0.9800 . ?
C62B H121 0.9800 . ?
C62B H122 0.9800 . ?
C62B H123 0.9800 . ?
C111 C112 1.379(5) . ?
C111 C116 1.402(5) . ?
C112 C113 1.377(5) . ?
C112 H11 0.9500 . ?
C113 C114 1.394(5) . ?
C113 H12 0.9500 . ?
C114 C115 1.387(5) . ?
C114 C117 1.532(5) . ?
C115 C116 1.375(5) . ?
C115 H13 0.9500 . ?
C116 H14 0.9500 . ?
C117 C120 1.503(6) . ?
C117 C119 1.527(6) . ?
C117 C118 1.528(6) . ?
C118 H15 0.9800 . ?
C118 H16 0.9800 . ?
C118 H17 0.9800 . ?
C119 H18 0.9800 . ?
C119 H19 0.9800 . ?
C119 H20 0.9800 . ?
C120 H21 0.9800 . ?
C120 H22 0.9800 . ?
C120 H23 0.9800 . ?
C121 C126 1.383(4) . ?
C121 C122 1.392(4) . ?
C122 C123 1.378(5) . ?
C122 H24 0.9500 . ?
C123 C124 1.392(5) . ?
C123 H25 0.9500 . ?
C124 C125 1.384(5) . ?
C124 C127 1.534(5) . ?
C125 C126 1.393(5) . ?
C125 H26 0.9500 . ?
C126 H27 0.9500 . ?
C127 C129 1.489(7) . ?
C127 C128 1.494(6) . ?
C127 C130 1.569(7) . ?
C128 H28 0.9800 . ?
C128 H29 0.9800 . ?
C128 H30 0.9800 . ?
C129 H31 0.9800 . ?
C129 H32 0.9800 . ?
C129 H33 0.9800 . ?
C130 H34 0.9800 . ?
C130 H35 0.9800 . ?
C130 H36 0.9800 . ?
C131 C132 1.379(5) . ?
C131 C136 1.393(5) . ?
C132 C133 1.395(5) . ?
C132 H37 0.9500 . ?
C133 C134 1.379(5) . ?
C133 H38 0.9500 . ?
C134 C135 1.389(5) . ?
C134 C137 1.539(5) . ?
C135 C136 1.377(5) . ?
C135 H39 0.9500 . ?
C136 H40 0.9500 . ?
C137 C138 1.458(7) . ?
C137 C139 1.484(7) . ?
C137 C140 1.501(8) . ?
C138 H41 0.9800 . ?
C138 H42 0.9800 . ?
C138 H43 0.9800 . ?
C139 H44 0.9800 . ?
C139 H45 0.9800 . ?
C139 H46 0.9800 . ?
C140 H47 0.9800 . ?
C140 H48 0.9800 . ?
C140 H49 0.9800 . ?
C211 C212 1.365(5) . ?
C211 C216 1.375(5) . ?
C212 C213 1.379(6) . ?
C212 H50 0.9500 . ?
C213 C214 1.383(5) . ?
C213 H51 0.9500 . ?
C214 C215 1.369(5) . ?
C214 C217 1.537(5) . ?
C215 C216 1.384(5) . ?
C215 H52 0.9500 . ?
C216 H53 0.9500 . ?
C217 C219 1.516(6) . ?
C217 C220 1.522(7) . ?
C217 C218 1.532(6) . ?
C218 H54 0.9800 . ?
C218 H55 0.9800 . ?
C218 H56 0.9800 . ?
C219 H57 0.9800 . ?
C219 H58 0.9800 . ?
C219 H59 0.9800 . ?
C220 H60 0.9800 . ?
C220 H61 0.9800 . ?
C220 H62 0.9800 . ?
C221 C222 1.378(5) . ?
C221 C226 1.391(5) . ?
C222 C223 1.376(5) . ?
C222 H63 0.9500 . ?
C223 C224 1.388(5) . ?
C223 H64 0.9500 . ?
C224 C225 1.385(5) . ?
C224 C227 1.522(5) . ?
C225 C226 1.374(5) . ?
C225 H65 0.9500 . ?
C226 H66 0.9500 . ?
C227 C228 1.509(6) . ?
C227 C230 1.511(6) . ?
C227 C229 1.537(7) . ?
C228 H67 0.9800 . ?
C228 H68 0.9800 . ?
C228 H69 0.9800 . ?
C229 H70 0.9800 . ?
C229 H71 0.9800 . ?
C229 H72 0.9800 . ?
C230 H73 0.9800 . ?
C230 H74 0.9800 . ?
C230 H75 0.9800 . ?
C231 C236 1.383(5) . ?
C231 C232 1.384(5) . ?
C232 C233 1.394(5) . ?
C232 H76 0.9500 . ?
C233 C234 1.382(5) . ?
C233 H77 0.9500 . ?
C234 C235 1.396(5) . ?
C234 C237 1.528(5) . ?
C235 C236 1.384(5) . ?
C235 H78 0.9500 . ?
C236 H79 0.9500 . ?
C237 C239 1.522(6) . ?
C237 C240 1.529(6) . ?
C237 C238 1.531(7) . ?
C238 H80 0.9800 . ?
C238 H81 0.9800 . ?
C238 H82 0.9800 . ?
C239 H83 0.9800 . ?
C239 H84 0.9800 . ?
C239 H85 0.9800 . ?
C240 H86 0.9800 . ?
C240 H87 0.9800 . ?
C240 H88 0.9800 . ?
C311 C312 1.422(12) . ?
C311 H124 0.9900 . ?
C311 H125 0.9900 . ?
C312 H126 0.9800 . ?
C312 H127 0.9800 . ?
C312 H128 0.9800 . ?
C321 C322 1.441(8) . ?
C321 H129 0.9900 . ?
C321 H130 0.9900 . ?
C322 H131 0.9800 . ?
C322 H132 0.9800 . ?
C322 H133 0.9800 . ?
C331 C332 1.467(7) . ?
C331 H134 0.9900 . ?
C331 H135 0.9900 . ?
C332 H136 0.9800 . ?
C332 H137 0.9800 . ?
C332 H138 0.9800 . ?
C341 C342 1.505(18) . ?
C341 H139 0.9900 . ?
C341 H140 0.9900 . ?
C342 H141 0.9800 . ?
C342 H142 0.9800 . ?
C342 H143 0.9800 . ?
C343 C344 1.50(2) . ?
C343 H144 0.9900 . ?
C343 H145 0.9900 . ?
C344 H146 0.9800 . ?
C344 H147 0.9800 . ?
C344 H148 0.9800 . ?
C351 C352 1.487(8) . ?
C351 H149 0.9900 . ?
C351 H150 0.9900 . ?
C352 H151 0.9800 . ?
C352 H152 0.9800 . ?
C352 H153 0.9800 . ?

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
O11 Mg1 O21 177.85(14) . . ?
O11 Mg1 O3 87.48(12) . . ?
O21 Mg1 O3 93.50(13) . . ?
O11 Mg1 O5 90.56(14) . . ?
O21 Mg1 O5 91.33(13) . . ?
O3 Mg1 O5 91.35(16) . . ?
O11 Mg1 O4 88.76(12) . . ?
O21 Mg1 O4 90.18(11) . . ?
O3 Mg1 O4 175.50(14) . . ?
O5 Mg1 O4 91.15(15) . . ?
O11 Mg1 O6 91.07(13) . . ?
O21 Mg1 O6 87.04(13) . . ?
O3 Mg1 O6 88.66(14) . . ?
O5 Mg1 O6 178.37(14) . . ?
O4 Mg1 O6 88.94(12) . . ?
O11 Mg1 H201 66.7(10) . . ?
O21 Mg1 H201 114.2(10) . . ?
O3 Mg1 H201 20.7(9) . . ?
O5 Mg1 H201 91.5(12) . . ?
O4 Mg1 H201 155.4(10) . . ?
O6 Mg1 H201 89.1(12) . . ?
C31 O3 Mg1 132.7(5) . . ?
C31B O3 Mg1 131.8(7) . . ?
C31 O3 H201 125(2) . . ?
C31B O3 H201 103(2) . . ?
Mg1 O3 H201 101(2) . . ?
C41 O4 Mg1 130.2(3) . . ?
C41 O4 H202 109(3) . . ?
Mg1 O4 H202 105(3) . . ?
C51 O5 Mg1 124.3(4) . . ?
C51B O5 Mg1 130.5(7) . . ?
C51 O5 H203 109.1(16) . . ?
C51B O5 H203 102.7(18) . . ?
Mg1 O5 H203 121.5(15) . . ?
C61 O6 Mg1 126.1(5) . . ?
C61B O6 Mg1 130.5(4) . . ?
C61 O6 H204 128(3) . . ?
C61B O6 H204 108.7(17) . . ?
Mg1 O6 H204 104(2) . . ?
C1 O11 Mg1 134.8(3) . . ?
C2 O21 Mg1 131.6(2) . . ?
C321 O32 H205 113(4) . . ?
C331 O33 H206 111(3) . . ?
C351 O35 H207 109(3) . . ?
C17 N1 C12 127.2(3) . . ?
C17 N1 H1 116.4 . . ?
C12 N1 H1 116.4 . . ?
C27 N2 C22 129.6(3) . . ?
C27 N2 H2 115.2 . . ?
C22 N2 H2 115.2 . . ?
O12 C1 O11 123.7(3) . . ?
O12 C1 C11 119.6(3) . . ?
O11 C1 C11 116.6(3) . . ?
O22 C2 O21 124.1(3) . . ?
O22 C2 C21 118.8(3) . . ?
O21 C2 C21 117.1(3) . . ?
C16 C11 C12 118.1(3) . . ?
C16 C11 C1 118.3(3) . . ?
C12 C11 C1 123.5(3) . . ?
C13 C12 N1 121.7(3) . . ?
C13 C12 C11 119.1(3) . . ?
N1 C12 C11 119.1(3) . . ?
C14 C13 C12 120.9(3) . . ?
C14 C13 H3 119.6 . . ?
C12 C13 H3 119.6 . . ?
C15 C14 C13 120.5(3) . . ?
C15 C14 H4 119.8 . . ?
C13 C14 H4 119.8 . . ?
C16 C15 C14 119.1(3) . . ?
C16 C15 H5 120.4 . . ?
C14 C15 H5 120.4 . . ?
C15 C16 C11 122.3(3) . . ?
C15 C16 H6 118.8 . . ?
C11 C16 H6 118.8 . . ?
O1 C17 N1 123.2(3) . . ?
O1 C17 C18 122.4(3) . . ?
N1 C17 C18 114.4(3) . . ?
C111 C18 C121 112.4(3) . . ?
C111 C18 C131 112.5(2) . . ?
C121 C18 C131 106.7(2) . . ?
C111 C18 C17 108.0(2) . . ?
C121 C18 C17 109.6(2) . . ?
C131 C18 C17 107.6(2) . . ?
C26 C21 C22 118.5(3) . . ?
C26 C21 C2 117.8(3) . . ?
C22 C21 C2 123.7(3) . . ?
C23 C22 N2 122.5(3) . . ?
C23 C22 C21 119.2(3) . . ?
N2 C22 C21 118.3(3) . . ?
C24 C23 C22 120.3(3) . . ?
C24 C23 H7 119.8 . . ?
C22 C23 H7 119.8 . . ?
C23 C24 C25 121.0(3) . . ?
C23 C24 H8 119.5 . . ?
C25 C24 H8 119.5 . . ?
C26 C25 C24 118.8(3) . . ?
C26 C25 H9 120.6 . . ?
C24 C25 H9 120.6 . . ?
C25 C26 C21 122.1(3) . . ?
C25 C26 H10 118.9 . . ?
C21 C26 H10 118.9 . . ?
O2 C27 N2 123.4(3) . . ?
O2 C27 C28 122.2(3) . . ?
N2 C27 C28 114.2(3) . . ?
C211 C28 C231 105.4(2) . . ?
C211 C28 C221 114.0(3) . . ?
C231 C28 C221 113.2(2) . . ?
C211 C28 C27 113.4(3) . . ?
C231 C28 C27 110.0(3) . . ?
C221 C28 C27 101.0(2) . . ?
O3 C31 C32 109.3(9) . . ?
O3 C31 H89 109.8 . . ?
C32 C31 H89 109.8 . . ?
O3 C31 H90 109.8 . . ?
C32 C31 H90 109.8 . . ?
H89 C31 H90 108.3 . . ?
C32B C31B O3 121.4(14) . . ?
C32B C31B H109 107.0 . . ?
O3 C31B H109 107.0 . . ?
C32B C31B H110 107.0 . . ?
O3 C31B H110 107.0 . . ?
H109 C31B H110 106.7 . . ?
C31 C32 H91 109.5 . . ?
C31 C32 H92 109.5 . . ?
H91 C32 H92 109.5 . . ?
C31 C32 H93 109.5 . . ?
H91 C32 H93 109.5 . . ?
H92 C32 H93 109.5 . . ?
C31B C32B H111 109.5 . . ?
C31B C32B H112 109.5 . . ?
H111 C32B H112 109.5 . . ?
C31B C32B H113 109.5 . . ?
H111 C32B H113 109.5 . . ?
H112 C32B H113 109.5 . . ?
O4 C41 C42 112.6(4) . . ?
O4 C41 H94 109.1 . . ?
C42 C41 H94 109.1 . . ?
O4 C41 H95 109.1 . . ?
C42 C41 H95 109.1 . . ?
H94 C41 H95 107.8 . . ?
C41 C42 H96 109.5 . . ?
C41 C42 H97 109.5 . . ?
H96 C42 H97 109.5 . . ?
C41 C42 H98 109.5 . . ?
H96 C42 H98 109.5 . . ?
H97 C42 H98 109.5 . . ?
O5 C51 C52 102.7(10) . . ?
O5 C51 H99 111.2 . . ?
C52 C51 H99 111.2 . . ?
O5 C51 H100 111.2 . . ?
C52 C51 H100 111.2 . . ?
H99 C51 H100 109.1 . . ?
C52B C51B O5 107.8(15) . . ?
C52B C51B H114 110.1 . . ?
O5 C51B H114 110.1 . . ?
C52B C51B H115 110.1 . . ?
O5 C51B H115 110.1 . . ?
H114 C51B H115 108.5 . . ?
C51 C52 H101 109.5 . . ?
C51 C52 H102 109.5 . . ?
H101 C52 H102 109.5 . . ?
C51 C52 H103 109.5 . . ?
H101 C52 H103 109.5 . . ?
H102 C52 H103 109.5 . . ?
C51B C52B H116 109.5 . . ?
C51B C52B H117 109.5 . . ?
H116 C52B H117 109.5 . . ?
C51B C52B H118 109.5 . . ?
H116 C52B H118 109.5 . . ?
H117 C52B H118 109.5 . . ?
O6 C61 C62 113.2(8) . . ?
O6 C61 H104 108.9 . . ?
C62 C61 H104 108.9 . . ?
O6 C61 H105 108.9 . . ?
C62 C61 H105 108.9 . . ?
H104 C61 H105 107.7 . . ?
C62B C61B O6 112.4(10) . . ?
C62B C61B H119 109.1 . . ?
O6 C61B H119 109.1 . . ?
C62B C61B H120 109.1 . . ?
O6 C61B H120 109.1 . . ?
H119 C61B H120 107.9 . . ?
C61 C62 H106 109.5 . . ?
C61 C62 H107 109.5 . . ?
H106 C62 H107 109.5 . . ?
C61 C62 H108 109.5 . . ?
H106 C62 H108 109.5 . . ?
H107 C62 H108 109.5 . . ?
C61B C62B H121 109.5 . . ?
C61B C62B H122 109.5 . . ?
H121 C62B H122 109.5 . . ?
C61B C62B H123 109.5 . . ?
H121 C62B H123 109.5 . . ?
H122 C62B H123 109.5 . . ?
C112 C111 C116 116.4(3) . . ?
C112 C111 C18 124.7(3) . . ?
C116 C111 C18 118.9(3) . . ?
C113 C112 C111 121.8(3) . . ?
C113 C112 H11 119.1 . . ?
C111 C112 H11 119.1 . . ?
C112 C113 C114 122.0(3) . . ?
C112 C113 H12 119.0 . . ?
C114 C113 H12 119.0 . . ?
C115 C114 C113 116.3(3) . . ?
C115 C114 C117 121.1(3) . . ?
C113 C114 C117 122.5(3) . . ?
C116 C115 C114 121.7(3) . . ?
C116 C115 H13 119.1 . . ?
C114 C115 H13 119.1 . . ?
C115 C116 C111 121.7(3) . . ?
C115 C116 H14 119.1 . . ?
C111 C116 H14 119.1 . . ?
C120 C117 C119 109.4(4) . . ?
C120 C117 C118 106.7(4) . . ?
C119 C117 C118 107.6(4) . . ?
C120 C117 C114 111.2(3) . . ?
C119 C117 C114 112.4(3) . . ?
C118 C117 C114 109.4(3) . . ?
C117 C118 H15 109.5 . . ?
C117 C118 H16 109.5 . . ?
H15 C118 H16 109.5 . . ?
C117 C118 H17 109.5 . . ?
H15 C118 H17 109.5 . . ?
H16 C118 H17 109.5 . . ?
C117 C119 H18 109.5 . . ?
C117 C119 H19 109.5 . . ?
H18 C119 H19 109.5 . . ?
C117 C119 H20 109.5 . . ?
H18 C119 H20 109.5 . . ?
H19 C119 H20 109.5 . . ?
C117 C120 H21 109.5 . . ?
C117 C120 H22 109.5 . . ?
H21 C120 H22 109.5 . . ?
C117 C120 H23 109.5 . . ?
H21 C120 H23 109.5 . . ?
H22 C120 H23 109.5 . . ?
C126 C121 C122 116.7(3) . . ?
C126 C121 C18 124.1(3) . . ?
C122 C121 C18 119.1(3) . . ?
C123 C122 C121 122.3(3) . . ?
C123 C122 H24 118.9 . . ?
C121 C122 H24 118.9 . . ?
C122 C123 C124 121.2(3) . . ?
C122 C123 H25 119.4 . . ?
C124 C123 H25 119.4 . . ?
C125 C124 C123 116.5(3) . . ?
C125 C124 C127 121.2(3) . . ?
C123 C124 C127 122.3(3) . . ?
C124 C125 C126 122.3(3) . . ?
C124 C125 H26 118.9 . . ?
C126 C125 H26 118.9 . . ?
C121 C126 C125 120.9(3) . . ?
C121 C126 H27 119.5 . . ?
C125 C126 H27 119.5 . . ?
C129 C127 C128 113.6(4) . . ?
C129 C127 C124 113.2(3) . . ?
C128 C127 C124 111.2(3) . . ?
C129 C127 C130 104.3(4) . . ?
C128 C127 C130 105.6(4) . . ?
C124 C127 C130 108.4(4) . . ?
C127 C128 H28 109.5 . . ?
C127 C128 H29 109.5 . . ?
H28 C128 H29 109.5 . . ?
C127 C128 H30 109.5 . . ?
H28 C128 H30 109.5 . . ?
H29 C128 H30 109.5 . . ?
C127 C129 H31 109.5 . . ?
C127 C129 H32 109.5 . . ?
H31 C129 H32 109.5 . . ?
C127 C129 H33 109.5 . . ?
H31 C129 H33 109.5 . . ?
H32 C129 H33 109.5 . . ?
C127 C130 H34 109.5 . . ?
C127 C130 H35 109.5 . . ?
H34 C130 H35 109.5 . . ?
C127 C130 H36 109.5 . . ?
H34 C130 H36 109.5 . . ?
H35 C130 H36 109.5 . . ?
C132 C131 C136 116.9(3) . . ?
C132 C131 C18 123.9(3) . . ?
C136 C131 C18 119.1(3) . . ?
C131 C132 C133 121.0(3) . . ?
C131 C132 H37 119.5 . . ?
C133 C132 H37 119.5 . . ?
C134 C133 C132 122.2(3) . . ?
C134 C133 H38 118.9 . . ?
C132 C133 H38 118.9 . . ?
C133 C134 C135 116.2(3) . . ?
C133 C134 C137 123.0(3) . . ?
C135 C134 C137 120.7(3) . . ?
C136 C135 C134 122.1(3) . . ?
C136 C135 H39 119.0 . . ?
C134 C135 H39 119.0 . . ?
C135 C136 C131 121.4(3) . . ?
C135 C136 H40 119.3 . . ?
C131 C136 H40 119.3 . . ?
C138 C137 C139 111.3(6) . . ?
C138 C137 C140 108.6(6) . . ?
C139 C137 C140 104.5(6) . . ?
C138 C137 C134 112.8(4) . . ?
C139 C137 C134 108.1(4) . . ?
C140 C137 C134 111.3(4) . . ?
C137 C138 H41 109.5 . . ?
C137 C138 H42 109.5 . . ?
H41 C138 H42 109.5 . . ?
C137 C138 H43 109.5 . . ?
H41 C138 H43 109.5 . . ?
H42 C138 H43 109.5 . . ?
C137 C139 H44 109.5 . . ?
C137 C139 H45 109.5 . . ?
H44 C139 H45 109.5 . . ?
C137 C139 H46 109.5 . . ?
H44 C139 H46 109.5 . . ?
H45 C139 H46 109.5 . . ?
C137 C140 H47 109.5 . . ?
C137 C140 H48 109.5 . . ?
H47 C140 H48 109.5 . . ?
C137 C140 H49 109.5 . . ?
H47 C140 H49 109.5 . . ?
H48 C140 H49 109.5 . . ?
C212 C211 C216 115.5(3) . . ?
C212 C211 C28 123.0(3) . . ?
C216 C211 C28 120.9(3) . . ?
C211 C212 C213 122.1(3) . . ?
C211 C212 H50 118.9 . . ?
C213 C212 H50 118.9 . . ?
C212 C213 C214 122.4(4) . . ?
C212 C213 H51 118.8 . . ?
C214 C213 H51 118.8 . . ?
C215 C214 C213 115.4(3) . . ?
C215 C214 C217 122.8(3) . . ?
C213 C214 C217 121.7(3) . . ?
C214 C215 C216 121.8(3) . . ?
C214 C215 H52 119.1 . . ?
C216 C215 H52 119.1 . . ?
C211 C216 C215 122.6(3) . . ?
C211 C216 H53 118.7 . . ?
C215 C216 H53 118.7 . . ?
C219 C217 C220 108.3(4) . . ?
C219 C217 C218 106.2(4) . . ?
C220 C217 C218 110.9(5) . . ?
C219 C217 C214 112.0(3) . . ?
C220 C217 C214 109.0(4) . . ?
C218 C217 C214 110.4(4) . . ?
C217 C218 H54 109.5 . . ?
C217 C218 H55 109.5 . . ?
H54 C218 H55 109.5 . . ?
C217 C218 H56 109.5 . . ?
H54 C218 H56 109.5 . . ?
H55 C218 H56 109.5 . . ?
C217 C219 H57 109.5 . . ?
C217 C219 H58 109.5 . . ?
H57 C219 H58 109.5 . . ?
C217 C219 H59 109.5 . . ?
H57 C219 H59 109.5 . . ?
H58 C219 H59 109.5 . . ?
C217 C220 H60 109.5 . . ?
C217 C220 H61 109.5 . . ?
H60 C220 H61 109.5 . . ?
C217 C220 H62 109.5 . . ?
H60 C220 H62 109.5 . . ?
H61 C220 H62 109.5 . . ?
C222 C221 C226 116.7(3) . . ?
C222 C221 C28 123.8(3) . . ?
C226 C221 C28 119.2(3) . . ?
C223 C222 C221 121.4(3) . . ?
C223 C222 H63 119.3 . . ?
C221 C222 H63 119.3 . . ?
C222 C223 C224 122.6(3) . . ?
C222 C223 H64 118.7 . . ?
C224 C223 H64 118.7 . . ?
C225 C224 C223 115.4(3) . . ?
C225 C224 C227 121.0(3) . . ?
C223 C224 C227 123.5(3) . . ?
C226 C225 C224 122.5(3) . . ?
C226 C225 H65 118.8 . . ?
C224 C225 H65 118.8 . . ?
C225 C226 C221 121.3(3) . . ?
C225 C226 H66 119.3 . . ?
C221 C226 H66 119.3 . . ?
C228 C227 C230 111.1(4) . . ?
C228 C227 C224 113.0(3) . . ?
C230 C227 C224 110.1(3) . . ?
C228 C227 C229 106.9(4) . . ?
C230 C227 C229 107.2(4) . . ?
C224 C227 C229 108.3(4) . . ?
C227 C228 H67 109.5 . . ?
C227 C228 H68 109.5 . . ?
H67 C228 H68 109.5 . . ?
C227 C228 H69 109.5 . . ?
H67 C228 H69 109.5 . . ?
H68 C228 H69 109.5 . . ?
C227 C229 H70 109.5 . . ?
C227 C229 H71 109.5 . . ?
H70 C229 H71 109.5 . . ?
C227 C229 H72 109.5 . . ?
H70 C229 H72 109.5 . . ?
H71 C229 H72 109.5 . . ?
C227 C230 H73 109.5 . . ?
C227 C230 H74 109.5 . . ?
H73 C230 H74 109.5 . . ?
C227 C230 H75 109.5 . . ?
H73 C230 H75 109.5 . . ?
H74 C230 H75 109.5 . . ?
C236 C231 C232 117.0(3) . . ?
C236 C231 C28 120.9(3) . . ?
C232 C231 C28 121.8(3) . . ?
C231 C232 C233 121.2(3) . . ?
C231 C232 H76 119.4 . . ?
C233 C232 H76 119.4 . . ?
C234 C233 C232 122.0(3) . . ?
C234 C233 H77 119.0 . . ?
C232 C233 H77 119.0 . . ?
C233 C234 C235 116.3(3) . . ?
C233 C234 C237 123.7(3) . . ?
C235 C234 C237 120.0(3) . . ?
C236 C235 C234 121.6(3) . . ?
C236 C235 H78 119.2 . . ?
C234 C235 H78 119.2 . . ?
C231 C236 C235 121.8(3) . . ?
C231 C236 H79 119.1 . . ?
C235 C236 H79 119.1 . . ?
C239 C237 C234 109.2(3) . . ?
C239 C237 C240 108.4(4) . . ?
C234 C237 C240 110.0(3) . . ?
C239 C237 C238 108.9(4) . . ?
C234 C237 C238 111.9(3) . . ?
C240 C237 C238 108.3(4) . . ?
C237 C238 H80 109.5 . . ?
C237 C238 H81 109.5 . . ?
H80 C238 H81 109.5 . . ?
C237 C238 H82 109.5 . . ?
H80 C238 H82 109.5 . . ?
H81 C238 H82 109.5 . . ?
C237 C239 H83 109.5 . . ?
C237 C239 H84 109.5 . . ?
H83 C239 H84 109.5 . . ?
C237 C239 H85 109.5 . . ?
H83 C239 H85 109.5 . . ?
H84 C239 H85 109.5 . . ?
C237 C240 H86 109.5 . . ?
C237 C240 H87 109.5 . . ?
H86 C240 H87 109.5 . . ?
C237 C240 H88 109.5 . . ?
H86 C240 H88 109.5 . . ?
H87 C240 H88 109.5 . . ?
C312 C311 O31 121.0(13) . . ?
C312 C311 H124 107.1 . . ?
O31 C311 H124 107.1 . . ?
C312 C311 H125 107.1 . . ?
O31 C311 H125 107.1 . . ?
H124 C311 H125 106.8 . . ?
C311 C312 H126 109.5 . . ?
C311 C312 H127 109.5 . . ?
H126 C312 H127 109.5 . . ?
C311 C312 H128 109.5 . . ?
H126 C312 H128 109.5 . . ?
H127 C312 H128 109.5 . . ?
O32 C321 C322 111.9(5) . . ?
O32 C321 H129 109.2 . . ?
C322 C321 H129 109.2 . . ?
O32 C321 H130 109.2 . . ?
C322 C321 H130 109.2 . . ?
H129 C321 H130 107.9 . . ?
C321 C322 H131 109.5 . . ?
C321 C322 H132 109.5 . . ?
H131 C322 H132 109.5 . . ?
C321 C322 H133 109.5 . . ?
H131 C322 H133 109.5 . . ?
H132 C322 H133 109.5 . . ?
O33 C331 C332 112.8(4) . . ?
O33 C331 H134 109.0 . . ?
C332 C331 H134 109.0 . . ?
O33 C331 H135 109.0 . . ?
C332 C331 H135 109.0 . . ?
H134 C331 H135 107.8 . . ?
C331 C332 H136 109.5 . . ?
C331 C332 H137 109.5 . . ?
H136 C332 H137 109.5 . . ?
C331 C332 H138 109.5 . . ?
H136 C332 H138 109.5 . . ?
H137 C332 H138 109.5 . . ?
O34 C341 C342 106.1(16) . . ?
O34 C341 H139 110.5 . . ?
C342 C341 H139 110.5 . . ?
O34 C341 H140 110.5 . . ?
C342 C341 H140 110.5 . . ?
H139 C341 H140 108.7 . . ?
C341 C342 H141 109.5 . . ?
C341 C342 H142 109.5 . . ?
H141 C342 H142 109.5 . . ?
C341 C342 H143 109.5 . . ?
H141 C342 H143 109.5 . . ?
H142 C342 H143 109.5 . . ?
O34B C343 C344 102(3) . . ?
O34B C343 H144 111.3 . . ?
C344 C343 H144 111.3 . . ?
O34B C343 H145 111.3 . . ?
C344 C343 H145 111.3 . . ?
H144 C343 H145 109.2 . . ?
C343 C344 H146 109.5 . . ?
C343 C344 H147 109.5 . . ?
H146 C344 H147 109.5 . . ?
C343 C344 H148 109.5 . . ?
H146 C344 H148 109.5 . . ?
H147 C344 H148 109.5 . . ?
O35 C351 C352 109.9(5) . . ?
O35 C351 H149 109.7 . . ?
C352 C351 H149 109.7 . . ?
O35 C351 H150 109.7 . . ?
C352 C351 H150 109.7 . . ?
H149 C351 H150 108.2 . . ?
C351 C352 H151 109.5 . . ?
C351 C352 H152 109.5 . . ?
H151 C352 H152 109.5 . . ?
C351 C352 H153 109.5 . . ?
H151 C352 H153 109.5 . . ?
H152 C352 H153 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
Mg1 O11 C1 O12 -27.1(6) . . . . ?
Mg1 O11 C1 C11 152.0(3) . . . . ?
Mg1 O21 C2 O22 -15.0(6) . . . . ?
Mg1 O21 C2 C21 163.1(3) . . . . ?
O12 C1 C11 C16 167.3(4) . . . . ?
O11 C1 C11 C16 -11.9(5) . . . . ?
O12 C1 C11 C12 -10.0(5) . . . . ?
O11 C1 C11 C12 170.9(3) . . . . ?
C17 N1 C12 C13 16.7(5) . . . . ?
C17 N1 C12 C11 -166.6(3) . . . . ?
C16 C11 C12 C13 -1.2(5) . . . . ?
C1 C11 C12 C13 176.1(3) . . . . ?
C16 C11 C12 N1 -178.0(3) . . . . ?
C1 C11 C12 N1 -0.7(5) . . . . ?
N1 C12 C13 C14 177.0(3) . . . . ?
C11 C12 C13 C14 0.3(5) . . . . ?
C12 C13 C14 C15 0.9(5) . . . . ?
C13 C14 C15 C16 -1.2(6) . . . . ?
C14 C15 C16 C11 0.3(6) . . . . ?
C12 C11 C16 C15 0.9(5) . . . . ?
C1 C11 C16 C15 -176.6(3) . . . . ?
C12 N1 C17 O1 10.5(5) . . . . ?
C12 N1 C17 C18 -167.6(3) . . . . ?
O1 C17 C18 C111 135.1(3) . . . . ?
N1 C17 C18 C111 -46.8(3) . . . . ?
O1 C17 C18 C121 -102.1(4) . . . . ?
N1 C17 C18 C121 75.9(3) . . . . ?
O1 C17 C18 C131 13.5(4) . . . . ?
N1 C17 C18 C131 -168.4(3) . . . . ?
O22 C2 C21 C26 -179.3(4) . . . . ?
O21 C2 C21 C26 2.4(5) . . . . ?
O22 C2 C21 C22 2.5(6) . . . . ?
O21 C2 C21 C22 -175.8(3) . . . . ?
C27 N2 C22 C23 0.1(5) . . . . ?
C27 N2 C22 C21 178.8(3) . . . . ?
C26 C21 C22 C23 -0.1(5) . . . . ?
C2 C21 C22 C23 178.0(3) . . . . ?
C26 C21 C22 N2 -179.0(3) . . . . ?
C2 C21 C22 N2 -0.8(5) . . . . ?
N2 C22 C23 C24 177.9(3) . . . . ?
C21 C22 C23 C24 -0.9(5) . . . . ?
C22 C23 C24 C25 0.9(6) . . . . ?
C23 C24 C25 C26 0.0(6) . . . . ?
C24 C25 C26 C21 -1.1(6) . . . . ?
C22 C21 C26 C25 1.1(5) . . . . ?
C2 C21 C26 C25 -177.2(3) . . . . ?
C22 N2 C27 O2 5.9(6) . . . . ?
C22 N2 C27 C28 -168.3(3) . . . . ?
O2 C27 C28 C211 135.4(3) . . . . ?
N2 C27 C28 C211 -50.3(4) . . . . ?
O2 C27 C28 C231 17.6(4) . . . . ?
N2 C27 C28 C231 -168.1(3) . . . . ?
O2 C27 C28 C221 -102.3(4) . . . . ?
N2 C27 C28 C221 72.0(3) . . . . ?
Mg1 O3 C31 C32 78.1(12) . . . . ?
Mg1 O3 C31B C32B -65(2) . . . . ?
Mg1 O4 C41 C42 159.3(4) . . . . ?
Mg1 O5 C51 C52 -112.4(8) . . . . ?
Mg1 O5 C51B C52B 109.6(12) . . . . ?
Mg1 O6 C61 C62 90.9(9) . . . . ?
Mg1 O6 C61B C62B -99.9(10) . . . . ?
C121 C18 C111 C112 8.9(4) . . . . ?
C131 C18 C111 C112 -111.7(3) . . . . ?
C17 C18 C111 C112 129.8(3) . . . . ?
C121 C18 C111 C116 -170.6(3) . . . . ?
C131 C18 C111 C116 68.8(4) . . . . ?
C17 C18 C111 C116 -49.7(4) . . . . ?
C116 C111 C112 C113 -1.3(5) . . . . ?
C18 C111 C112 C113 179.2(3) . . . . ?
C111 C112 C113 C114 0.6(5) . . . . ?
C112 C113 C114 C115 0.3(5) . . . . ?
C112 C113 C114 C117 177.9(3) . . . . ?
C113 C114 C115 C116 -0.4(5) . . . . ?
C117 C114 C115 C116 -178.0(3) . . . . ?
C114 C115 C116 C111 -0.4(5) . . . . ?
C112 C111 C116 C115 1.2(5) . . . . ?
C18 C111 C116 C115 -179.3(3) . . . . ?
C115 C114 C117 C120 -43.4(5) . . . . ?
C113 C114 C117 C120 139.1(4) . . . . ?
C115 C114 C117 C119 -166.4(4) . . . . ?
C113 C114 C117 C119 16.2(5) . . . . ?
C115 C114 C117 C118 74.1(5) . . . . ?
C113 C114 C117 C118 -103.3(4) . . . . ?
C111 C18 C121 C126 111.6(4) . . . . ?
C131 C18 C121 C126 -124.6(3) . . . . ?
C17 C18 C121 C126 -8.4(4) . . . . ?
C111 C18 C121 C122 -71.1(4) . . . . ?
C131 C18 C121 C122 52.7(4) . . . . ?
C17 C18 C121 C122 168.8(3) . . . . ?
C126 C121 C122 C123 -3.3(5) . . . . ?
C18 C121 C122 C123 179.3(3) . . . . ?
C121 C122 C123 C124 1.1(5) . . . . ?
C122 C123 C124 C125 2.6(5) . . . . ?
C122 C123 C124 C127 -179.3(3) . . . . ?
C123 C124 C125 C126 -4.1(6) . . . . ?
C127 C124 C125 C126 177.8(4) . . . . ?
C122 C121 C126 C125 1.8(5) . . . . ?
C18 C121 C126 C125 179.1(3) . . . . ?
C124 C125 C126 C121 2.0(7) . . . . ?
C125 C124 C127 C129 -175.0(5) . . . . ?
C123 C124 C127 C129 7.0(6) . . . . ?
C125 C124 C127 C128 -45.7(6) . . . . ?
C123 C124 C127 C128 136.3(4) . . . . ?
C125 C124 C127 C130 69.9(5) . . . . ?
C123 C124 C127 C130 -108.1(4) . . . . ?
C111 C18 C131 C132 -3.4(5) . . . . ?
C121 C18 C131 C132 -127.2(3) . . . . ?
C17 C18 C131 C132 115.3(4) . . . . ?
C111 C18 C131 C136 175.2(3) . . . . ?
C121 C18 C131 C136 51.4(4) . . . . ?
C17 C18 C131 C136 -66.1(4) . . . . ?
C136 C131 C132 C133 3.7(5) . . . . ?
C18 C131 C132 C133 -177.7(3) . . . . ?
C131 C132 C133 C134 0.0(6) . . . . ?
C132 C133 C134 C135 -3.1(6) . . . . ?
C132 C133 C134 C137 174.3(4) . . . . ?
C133 C134 C135 C136 2.6(6) . . . . ?
C137 C134 C135 C136 -174.9(4) . . . . ?
C134 C135 C136 C131 1.1(6) . . . . ?
C132 C131 C136 C135 -4.2(5) . . . . ?
C18 C131 C136 C135 177.1(3) . . . . ?
C133 C134 C137 C138 10.1(7) . . . . ?
C135 C134 C137 C138 -172.5(5) . . . . ?
C133 C134 C137 C139 -113.4(6) . . . . ?
C135 C134 C137 C139 64.0(6) . . . . ?
C133 C134 C137 C140 132.5(6) . . . . ?
C135 C134 C137 C140 -50.2(6) . . . . ?
C231 C28 C211 C212 94.4(4) . . . . ?
C221 C28 C211 C212 -140.8(4) . . . . ?
C27 C28 C211 C212 -26.0(5) . . . . ?
C231 C28 C211 C216 -76.6(4) . . . . ?
C221 C28 C211 C216 48.2(4) . . . . ?
C27 C28 C211 C216 163.0(3) . . . . ?
C216 C211 C212 C213 -2.5(6) . . . . ?
C28 C211 C212 C213 -174.0(4) . . . . ?
C211 C212 C213 C214 -1.2(8) . . . . ?
C212 C213 C214 C215 3.0(7) . . . . ?
C212 C213 C214 C217 179.5(4) . . . . ?
C213 C214 C215 C216 -1.1(6) . . . . ?
C217 C214 C215 C216 -177.5(4) . . . . ?
C212 C211 C216 C215 4.5(6) . . . . ?
C28 C211 C216 C215 176.1(3) . . . . ?
C214 C215 C216 C211 -2.7(6) . . . . ?
C215 C214 C217 C219 -23.7(6) . . . . ?
C213 C214 C217 C219 160.2(4) . . . . ?
C215 C214 C217 C220 96.2(5) . . . . ?
C213 C214 C217 C220 -80.0(5) . . . . ?
C215 C214 C217 C218 -141.8(5) . . . . ?
C213 C214 C217 C218 42.1(6) . . . . ?
C211 C28 C221 C222 18.5(4) . . . . ?
C231 C28 C221 C222 139.0(3) . . . . ?
C27 C28 C221 C222 -103.4(3) . . . . ?
C211 C28 C221 C226 -168.3(3) . . . . ?
C231 C28 C221 C226 -47.8(4) . . . . ?
C27 C28 C221 C226 69.8(3) . . . . ?
C226 C221 C222 C223 3.1(5) . . . . ?
C28 C221 C222 C223 176.5(3) . . . . ?
C221 C222 C223 C224 -2.0(6) . . . . ?
C222 C223 C224 C225 -0.9(6) . . . . ?
C222 C223 C224 C227 -178.4(4) . . . . ?
C223 C224 C225 C226 2.6(6) . . . . ?
C227 C224 C225 C226 -179.8(4) . . . . ?
C224 C225 C226 C221 -1.5(6) . . . . ?
C222 C221 C226 C225 -1.4(5) . . . . ?
C28 C221 C226 C225 -175.2(3) . . . . ?
C225 C224 C227 C228 173.8(4) . . . . ?
C223 C224 C227 C228 -8.8(6) . . . . ?
C225 C224 C227 C230 49.0(5) . . . . ?
C223 C224 C227 C230 -133.7(5) . . . . ?
C225 C224 C227 C229 -67.9(5) . . . . ?
C223 C224 C227 C229 109.4(5) . . . . ?
C211 C28 C231 C236 -75.7(4) . . . . ?
C221 C28 C231 C236 159.1(3) . . . . ?
C27 C28 C231 C236 46.9(4) . . . . ?
C211 C28 C231 C232 98.6(3) . . . . ?
C221 C28 C231 C232 -26.6(4) . . . . ?
C27 C28 C231 C232 -138.8(3) . . . . ?
C236 C231 C232 C233 -1.7(5) . . . . ?
C28 C231 C232 C233 -176.2(3) . . . . ?
C231 C232 C233 C234 -0.5(5) . . . . ?
C232 C233 C234 C235 2.3(5) . . . . ?
C232 C233 C234 C237 -177.9(3) . . . . ?
C233 C234 C235 C236 -1.9(6) . . . . ?
C237 C234 C235 C236 178.3(4) . . . . ?
C232 C231 C236 C235 2.1(6) . . . . ?
C28 C231 C236 C235 176.7(3) . . . . ?
C234 C235 C236 C231 -0.3(6) . . . . ?
C233 C234 C237 C239 119.3(4) . . . . ?
C235 C234 C237 C239 -61.0(5) . . . . ?
C233 C234 C237 C240 -121.8(5) . . . . ?
C235 C234 C237 C240 57.9(5) . . . . ?
C233 C234 C237 C238 -1.4(5) . . . . ?
C235 C234 C237 C238 178.4(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H202 O22 0.816(19) 1.82(2) 2.603(4) 160(5) .
O5 H203 O32 0.82(2) 1.86(2) 2.666(5) 172(2) .
O6 H204 O31 0.802(18) 1.98(2) 2.607(8) 134(2) .
O32 H205 O33 0.89(6) 1.86(6) 2.735(5) 172(6) .
O33 H206 O2 0.88(5) 1.88(5) 2.733(4) 163(5) 1_455
O35 H207 O1 0.85(2) 2.10(3) 2.911(4) 160(6) .
N1 H1 O12 0.88 1.94 2.636(4) 135.1 .
N2 H2 O22 0.88 1.86 2.595(4) 139.9 .
C13 H3 O1 0.95 2.25 2.841(4) 119.3 .
C23 H7 O2 0.95 2.23 2.850(4) 122.3 .
C31B H109 O31 0.99 1.99 2.96(2) 168.3 .
C51 H100 O21 0.99 2.56 3.122(9) 115.9 .
C61 H104 O4 0.99 2.56 3.053(10) 110.8 .
C61 H105 O34 0.99 2.07 2.844(15) 133.9 1_655
C61B H120 O31 0.99 2.04 2.681(12) 120.2 .
C344 H148 O35 0.98 2.20 2.95(5) 131.7 .
O4 H202 O22 0.816(19) 1.82(2) 2.603(4) 160(5) .
O5 H203 O32 0.82(2) 1.86(2) 2.666(5) 172(2) .
O6 H204 O31 0.802(18) 1.98(2) 2.607(8) 134(2) .
O32 H205 O33 0.89(6) 1.86(6) 2.735(5) 172(6) .
O33 H206 O2 0.88(5) 1.88(5) 2.733(4) 163(5) 1_455
O35 H207 O1 0.85(2) 2.10(3) 2.911(4) 160(6) .
N1 H1 O12 0.88 1.94 2.636(4) 135.1 .
N2 H2 O22 0.88 1.86 2.595(4) 139.9 .
C13 H3 O1 0.95 2.25 2.841(4) 119.3 .
C23 H7 O2 0.95 2.23 2.850(4) 122.3 .
C31B H109 O31 0.99 1.99 2.96(2) 168.3 .
C51 H100 O21 0.99 2.56 3.122(9) 115.9 .
C61 H104 O4 0.99 2.56 3.053(10) 110.8 .
C61 H105 O34 0.99 2.07 2.844(15) 133.9 1_655
C61B H120 O31 0.99 2.04 2.681(12) 120.2 .
C344 H148 O35 0.98 2.20 2.95(5) 131.7 .

_refine_diff_density_max         0.750
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.063

_shelxl_version_number           2014/6

#===END
_chemical_properties_physical    Efflorescent
