# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_cm0525ta5
_database_code_depnum_ccdc_archive 'CCDC 2333365'
loop_
_audit_author_name
_audit_author_address
'Michelle Neary'
;Hunter College
United States of America
;
_audit_update_record             
;
2024-02-16 deposited with the CCDC.	2024-06-13 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_cm0525ta5           
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The overall quality of the crystal is mediocre due to twinning and disorder, but the connectivity should be accurate.
;
_vrf_PLAT213_cm0525ta5           
;
PROBLEM: Atom C40             has ADP max/min Ratio .....        4.5 prolat
RESPONSE: The overall quality of the crystal is mediocre due to twinning and disorder, but the connectivity should be accurate.
;
_vrf_PLAT234_cm0525ta5           
;
PROBLEM: Large Hirshfeld Difference C39      --C42      .       0.29 Ang.
RESPONSE: The overall quality of the crystal is mediocre due to twinning and disorder, but the connectivity should be accurate.
;
_vrf_PLAT340_cm0525ta5           
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02339 Ang.
RESPONSE: The overall quality of the crystal is mediocre due to twinning and disorder, but the connectivity should be accurate.
;
_vrf_PLAT369_cm0525ta5           
;
PROBLEM: Long   C(sp2)-C(sp2) Bond  C4       - C7       .       1.57 Ang.
RESPONSE: The overall quality of the crystal is mediocre due to twinning and disorder, but the connectivity should be accurate.
;
# Added during the CSD deposition process: Friday 16 February 2024 08:51 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H63 Cl N4 O5 Si3'
_chemical_formula_sum            'C42 H63 Cl N4 O5 Si3'
_chemical_formula_weight         823.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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'

_cell_length_a                   13.9738(7)
_cell_length_b                   7.6693(4)
_cell_length_c                   22.8201(14)
_cell_angle_alpha                90
_cell_angle_beta                 106.684(4)
_cell_angle_gamma                90
_cell_volume                     2342.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9972
_cell_measurement_theta_min      3.30
_cell_measurement_theta_max      67.40

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_F_000             884
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.730
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.808
_shelx_estimated_absorpt_T_min   0.352
_shelx_estimated_absorpt_T_max   0.965
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.358408
_exptl_absorpt_correction_T_max  0.864248
_exptl_absorpt_process_details   twinabs-2012/1
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 with PHOTON III detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            66750
_diffrn_reflns_av_unetI/netI     0.1037
_diffrn_reflns_av_R_equivalents  0.2150
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.021
_diffrn_reflns_theta_max         67.694
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.536
_diffrn_reflns_point_group_measured_fraction_full 0.536
_reflns_number_total             4604
_reflns_number_gt                3994
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     0.000
_reflns_Friedel_fraction_full    0.000

_reflns_special_details          
; 
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. Completness statistics refer to single and 
 composite reflections containing twin component 1 only. 
;

_computing_data_collection       'Bruker APEX4'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT-2018 (Sheldrick 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 Refined as a 2-component twin. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1741P)²+17.0425P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
No quotients, so Flack parameter determined by classical intensity fit 
;
_refine_ls_abs_structure_Flack   0.14(7)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         4538
_refine_ls_number_parameters     518
_refine_ls_number_restraints     328
_refine_ls_R_factor_all          0.1502
_refine_ls_R_factor_gt           0.1290
_refine_ls_wR_factor_ref         0.3493
_refine_ls_wR_factor_gt          0.3283
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.001
_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
Cl1 Cl 0.2308(3) 0.9131(8) 0.1794(2) 0.0593(12) Uani 1 1 d . . . . .
N1 N 0.4570(7) 0.1938(15) 0.3154(6) 0.030(3) Uani 1 1 d . . . . .
N2 N 0.5772(9) 0.173(2) 0.2579(6) 0.037(3) Uani 1 1 d . . . . .
N3 N 0.7336(7) 0.3132(15) 0.3112(5) 0.026(2) Uani 1 1 d . . . . .
N4 N 0.6976(8) 0.4025(15) 0.3969(5) 0.025(2) Uani 1 1 d . . . . .
O1 O 0.2353(7) 0.1841(18) 0.3380(5) 0.046(3) Uani 1 1 d . . . . .
O2 O 0.8864(7) 0.2464(12) 0.2957(5) 0.030(2) Uani 1 1 d . . . . .
O3 O 0.9619(6) 0.5821(16) 0.3410(4) 0.035(2) Uani 1 1 d . . . . .
O4 O 0.8712(7) 0.3121(15) 0.1666(5) 0.042(2) Uani 1 1 d D . . . .
O5 O 0.7078(8) 0.4989(16) 0.1843(5) 0.043(3) Uani 1 1 d . . . . .
Si1 Si 0.9941(2) 0.7864(5) 0.35818(17) 0.0256(8) Uani 1 1 d . . . . .
Si2 Si 0.8389(3) 0.3301(6) 0.0920(2) 0.0352(11) Uani 0.892(8) 1 d D U P A 1
C31 C 0.7115(14) 0.240(3) 0.0605(10) 0.062(6) Uani 0.892(8) 1 d D U P A 1
H31A H 0.691174 0.249416 0.015834 0.094 Uiso 0.892(8) 1 calc R U P A 1
H31B H 0.711307 0.116533 0.072138 0.094 Uiso 0.892(8) 1 calc R U P A 1
H31C H 0.664690 0.304722 0.076990 0.094 Uiso 0.892(8) 1 calc R U P A 1
C32 C 0.8427(18) 0.562(3) 0.0707(11) 0.058(5) Uani 0.892(8) 1 d D U P A 1
H32A H 0.823340 0.572428 0.026033 0.086 Uiso 0.892(8) 1 calc R U P A 1
H32B H 0.796129 0.628755 0.086860 0.086 Uiso 0.892(8) 1 calc R U P A 1
H32C H 0.910517 0.607124 0.087911 0.086 Uiso 0.892(8) 1 calc R U P A 1
C33 C 0.9268(15) 0.203(3) 0.0647(9) 0.051(3) Uani 0.892(8) 1 d D U P A 1
C34 C 0.8991(19) 0.208(4) -0.0055(10) 0.068(5) Uani 0.892(8) 1 d D U P A 1
H34A H 0.830277 0.167275 -0.022645 0.101 Uiso 0.892(8) 1 calc R U P A 1
H34B H 0.904913 0.327859 -0.018946 0.101 Uiso 0.892(8) 1 calc R U P A 1
H34C H 0.944521 0.132270 -0.019560 0.101 Uiso 0.892(8) 1 calc R U P A 1
C35 C 0.9299(19) 0.008(3) 0.0856(11) 0.061(5) Uani 0.892(8) 1 d D U P A 1
H35A H 0.863011 -0.042949 0.070539 0.091 Uiso 0.892(8) 1 calc R U P A 1
H35B H 0.976435 -0.057386 0.068844 0.091 Uiso 0.892(8) 1 calc R U P A 1
H35C H 0.952344 0.002034 0.130331 0.091 Uiso 0.892(8) 1 calc R U P A 1
C36 C 1.0339(14) 0.266(3) 0.0905(10) 0.050(4) Uani 0.892(8) 1 d D U P A 1
H36A H 1.052435 0.263526 0.135337 0.075 Uiso 0.892(8) 1 calc R U P A 1
H36B H 1.078841 0.190399 0.076151 0.075 Uiso 0.892(8) 1 calc R U P A 1
H36C H 1.039233 0.385988 0.076765 0.075 Uiso 0.892(8) 1 calc R U P A 1
Si2A Si 0.887(3) 0.427(5) 0.0922(16) 0.0352(11) Uani 0.108(8) 1 d D U P A 2
C31A C 0.769(5) 0.529(12) 0.047(4) 0.062(6) Uani 0.108(8) 1 d D . P A 2
H31D H 0.749413 0.621324 0.070501 0.094 Uiso 0.108(8) 1 calc R U P A 2
H31E H 0.777933 0.578016 0.008984 0.094 Uiso 0.108(8) 1 calc R U P A 2
H31F H 0.715746 0.440086 0.035981 0.094 Uiso 0.108(8) 1 calc R U P A 2
C32A C 0.987(6) 0.594(9) 0.112(4) 0.058(5) Uani 0.108(8) 1 d D U P A 2
H32D H 0.968461 0.687086 0.135851 0.086 Uiso 0.108(8) 1 calc R U P A 2
H32E H 1.049599 0.539827 0.135845 0.086 Uiso 0.108(8) 1 calc R U P A 2
H32F H 0.996285 0.643063 0.074163 0.086 Uiso 0.108(8) 1 calc R U P A 2
C33A C 0.922(5) 0.255(8) 0.048(3) 0.051(3) Uani 0.108(8) 1 d D U P A 2
C34A C 0.883(11) 0.298(18) -0.021(3) 0.068(5) Uani 0.108(8) 1 d D U P A 2
H34D H 0.810507 0.315682 -0.032013 0.101 Uiso 0.108(8) 1 calc R U P A 2
H34E H 0.915161 0.405243 -0.029225 0.101 Uiso 0.108(8) 1 calc R U P A 2
H34F H 0.898557 0.201972 -0.044643 0.101 Uiso 0.108(8) 1 calc R U P A 2
C35A C 0.878(11) 0.076(9) 0.060(7) 0.061(5) Uani 0.108(8) 1 d D U P A 2
H35D H 0.804940 0.083996 0.049153 0.091 Uiso 0.108(8) 1 calc R U P A 2
H35E H 0.896197 -0.014038 0.034097 0.091 Uiso 0.108(8) 1 calc R U P A 2
H35F H 0.904913 0.044148 0.102782 0.091 Uiso 0.108(8) 1 calc R U P A 2
C36A C 1.034(6) 0.229(15) 0.065(7) 0.050(4) Uani 0.108(8) 1 d D U P A 2
H36D H 1.059252 0.200956 0.108766 0.075 Uiso 0.108(8) 1 calc R U P A 2
H36E H 1.049780 0.132122 0.041131 0.075 Uiso 0.108(8) 1 calc R U P A 2
H36F H 1.066384 0.335393 0.056549 0.075 Uiso 0.108(8) 1 calc R U P A 2
Si3 Si 0.6389(3) 0.6753(8) 0.1842(2) 0.0481(12) Uani 1 1 d . . . . .
C1 C 0.2560(11) 0.731(3) 0.2269(7) 0.048(5) Uani 1 1 d . . . . .
C2 C 0.3203(11) 0.7528(19) 0.2873(8) 0.040(4) Uani 1 1 d . . . . .
H2A H 0.350251 0.862156 0.301102 0.048 Uiso 1 1 calc R U . . .
C3 C 0.3373(10) 0.6093(19) 0.3248(7) 0.031(3) Uani 1 1 d . . . . .
H3A H 0.381710 0.618583 0.364937 0.037 Uiso 1 1 calc R U . . .
C4 C 0.2918(9) 0.4535(18) 0.3057(7) 0.029(3) Uani 1 1 d . . . . .
C5 C 0.2306(11) 0.434(3) 0.2458(7) 0.043(4) Uani 1 1 d . . . . .
H5A H 0.200636 0.324631 0.232305 0.052 Uiso 1 1 calc R U . . .
C6 C 0.2135(12) 0.574(3) 0.2062(8) 0.046(4) Uani 1 1 d . . . . .
H6A H 0.172942 0.561612 0.165177 0.055 Uiso 1 1 calc R U . . .
C7 C 0.3004(10) 0.293(2) 0.3497(7) 0.034(3) Uani 1 1 d . . . . .
C8 C 0.3790(9) 0.3063(19) 0.4093(6) 0.031(3) Uani 1 1 d . . . . .
C9 C 0.3472(10) 0.3174(18) 0.4608(7) 0.035(3) Uani 1 1 d . . . . .
H9A H 0.277962 0.304532 0.456810 0.042 Uiso 1 1 calc R U . . .
C10 C 0.4123(12) 0.3468(19) 0.5184(7) 0.038(3) Uani 1 1 d . . . . .
C11 C 0.5133(11) 0.365(2) 0.5235(6) 0.041(4) Uani 1 1 d . . . . .
H11A H 0.559768 0.387078 0.562273 0.049 Uiso 1 1 calc R U . . .
C12 C 0.5461(10) 0.352(2) 0.4714(7) 0.038(4) Uani 1 1 d . . . . .
H12A H 0.614984 0.368989 0.475356 0.046 Uiso 1 1 calc R U . . .
C13 C 0.4828(9) 0.316(2) 0.4151(6) 0.032(3) Uani 1 1 d . . . . .
C14 C 0.3759(13) 0.355(2) 0.5747(7) 0.044(4) Uani 1 1 d . . . . .
H14A H 0.351132 0.239876 0.582238 0.066 Uiso 1 1 calc R U . . .
H14B H 0.321809 0.440482 0.568318 0.066 Uiso 1 1 calc R U . . .
H14C H 0.431158 0.389372 0.610100 0.066 Uiso 1 1 calc R U . . .
C15 C 0.5202(9) 0.276(2) 0.3633(6) 0.031(3) Uani 1 1 d . . . . .
C16 C 0.4885(11) 0.150(3) 0.2677(7) 0.044(4) Uani 1 1 d . . . . .
H16A H 0.440308 0.092035 0.235537 0.053 Uiso 1 1 calc R U . . .
C17 C 0.6365(9) 0.2603(17) 0.3059(6) 0.0277(19) Uani 1 1 d . . . . .
C18 C 0.7650(9) 0.401(2) 0.3666(6) 0.034(3) Uani 1 1 d . . . . .
H18A H 0.828718 0.454779 0.381205 0.041 Uiso 1 1 calc R U . . .
C19 C 0.6157(9) 0.3134(17) 0.3583(6) 0.0277(19) Uani 1 1 d . U . . .
C20 C 0.7875(9) 0.304(2) 0.2661(7) 0.033(3) Uani 1 1 d . . . . .
H20A H 0.754659 0.213305 0.235381 0.040 Uiso 1 1 calc R U . . .
C21 C 0.7949(10) 0.4672(19) 0.2320(6) 0.030(3) Uani 1 1 d . . . . .
H21A H 0.806835 0.567784 0.261063 0.036 Uiso 1 1 calc R U . . .
C22 C 0.8904(11) 0.4302(19) 0.2149(6) 0.034(3) Uani 1 1 d . . . . .
H22A H 0.921582 0.539765 0.205229 0.040 Uiso 1 1 calc R U . . .
C23 C 0.9556(10) 0.343(2) 0.2719(6) 0.035(3) Uani 1 1 d . . . . .
H23A H 0.998923 0.256594 0.258810 0.041 Uiso 1 1 calc R U . . .
C24 C 1.0233(11) 0.459(3) 0.3202(8) 0.046(4) Uani 1 1 d . . . . .
H24A H 1.062385 0.387732 0.355021 0.056 Uiso 1 1 calc R U . . .
H24B H 1.070559 0.522170 0.302735 0.056 Uiso 1 1 calc R U . . .
C25 C 1.0318(11) 0.892(2) 0.2939(7) 0.043(4) Uani 1 1 d . . . . .
H25A H 0.972862 0.943917 0.264788 0.064 Uiso 1 1 calc R U . . .
H25B H 1.061012 0.804665 0.272919 0.064 Uiso 1 1 calc R U . . .
H25C H 1.081121 0.983900 0.310371 0.064 Uiso 1 1 calc R U . . .
C26 C 0.8778(10) 0.882(2) 0.3699(8) 0.041(4) Uani 1 1 d . . . . .
H26A H 0.821172 0.858441 0.333914 0.062 Uiso 1 1 calc R U . . .
H26B H 0.886117 1.008020 0.375986 0.062 Uiso 1 1 calc R U . . .
H26C H 0.865116 0.828909 0.406099 0.062 Uiso 1 1 calc R U . . .
C27 C 1.1017(9) 0.808(3) 0.4314(6) 0.039(4) Uani 1 1 d . . . . .
C28 C 1.1927(13) 0.725(3) 0.4200(10) 0.068(6) Uani 1 1 d . . . . .
H28A H 1.238799 0.816588 0.415055 0.102 Uiso 1 1 calc R U . . .
H28B H 1.172345 0.654433 0.382668 0.102 Uiso 1 1 calc R U . . .
H28C H 1.226086 0.650800 0.454748 0.102 Uiso 1 1 calc R U . . .
C29 C 1.0711(18) 0.716(3) 0.4817(9) 0.085(9) Uani 1 1 d . . . . .
H29A H 1.130914 0.677378 0.513393 0.127 Uiso 1 1 calc R U . . .
H29B H 1.029853 0.614222 0.464749 0.127 Uiso 1 1 calc R U . . .
H29C H 1.032720 0.795947 0.499679 0.127 Uiso 1 1 calc R U . . .
C30 C 1.1243(11) 0.995(2) 0.4484(7) 0.042(4) Uani 1 1 d . . . . .
H30A H 1.175477 1.001635 0.487983 0.063 Uiso 1 1 calc R U . . .
H30B H 1.063378 1.053325 0.451168 0.063 Uiso 1 1 calc R U . . .
H30C H 1.148751 1.052279 0.417084 0.063 Uiso 1 1 calc R U . . .
C37 C 0.7170(17) 0.871(3) 0.1792(10) 0.068(6) Uani 1 1 d . . . . .
H37A H 0.774685 0.876372 0.215784 0.103 Uiso 1 1 calc R U . . .
H37B H 0.676834 0.976839 0.176591 0.103 Uiso 1 1 calc R U . . .
H37C H 0.740381 0.861469 0.142761 0.103 Uiso 1 1 calc R U . . .
C38 C 0.5993(14) 0.690(3) 0.2558(9) 0.058(3) Uani 1 1 d . . . . .
H38A H 0.542950 0.610874 0.252729 0.087 Uiso 1 1 calc R U . . .
H38B H 0.578964 0.809754 0.261128 0.087 Uiso 1 1 calc R U . . .
H38C H 0.655235 0.656699 0.290986 0.087 Uiso 1 1 calc R U . . .
C39 C 0.5230(14) 0.661(3) 0.1167(9) 0.058(3) Uani 1 1 d . U . . .
C40 C 0.4555(18) 0.818(4) 0.1188(10) 0.099(11) Uani 1 1 d . . . . .
H40A H 0.399491 0.820475 0.081288 0.148 Uiso 1 1 calc R U . . .
H40B H 0.494206 0.925686 0.122046 0.148 Uiso 1 1 calc R U . . .
H40C H 0.429796 0.806987 0.154302 0.148 Uiso 1 1 calc R U . . .
C41 C 0.560(2) 0.664(5) 0.0574(11) 0.118(13) Uani 1 1 d . . . . .
H41A H 0.501942 0.653476 0.021022 0.177 Uiso 1 1 calc R U . . .
H41B H 0.605449 0.566447 0.058619 0.177 Uiso 1 1 calc R U . . .
H41C H 0.594308 0.774183 0.055617 0.177 Uiso 1 1 calc R U . . .
C42 C 0.4745(16) 0.488(5) 0.1176(10) 0.097(11) Uani 1 1 d . . . . .
H42A H 0.426030 0.466548 0.077686 0.146 Uiso 1 1 calc R U . . .
H42B H 0.440067 0.487838 0.149428 0.146 Uiso 1 1 calc R U . . .
H42C H 0.525478 0.396481 0.126164 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
Cl1 C1 1.74(2) . ?
N1 C16 1.331(19) . ?
N1 C15 1.347(18) . ?
N2 C16 1.333(18) . ?
N2 C17 1.346(19) . ?
N3 C18 1.388(18) . ?
N3 C17 1.389(15) . ?
N3 C20 1.441(16) . ?
N4 C18 1.320(16) . ?
N4 C19 1.405(17) . ?
O1 C7 1.208(18) . ?
O2 C20 1.424(16) . ?
O2 C23 1.442(16) . ?
O3 C24 1.442(18) . ?
O3 Si1 1.646(12) . ?
O4 C22 1.392(17) . ?
O4 Si2 1.637(12) . ?
O4 Si2A 1.98(4) . ?
O5 C21 1.402(17) . ?
O5 Si3 1.659(12) . ?
Si1 C26 1.870(14) . ?
Si1 C25 1.881(15) . ?
Si1 C27 1.907(12) . ?
Si2 C33 1.814(18) . ?
Si2 C32 1.85(2) . ?
Si2 C31 1.85(2) . ?
C33 C36 1.52(3) . ?
C33 C34 1.54(3) . ?
C33 C35 1.56(3) . ?
Si2A C33A 1.81(3) . ?
Si2A C31A 1.85(3) . ?
Si2A C32A 1.86(3) . ?
C33A C36A 1.52(3) . ?
C33A C34A 1.54(3) . ?
C33A C35A 1.56(4) . ?
Si3 C38 1.873(19) . ?
Si3 C37 1.88(2) . ?
Si3 C39 1.89(2) . ?
C1 C6 1.37(3) . ?
C1 C2 1.42(2) . ?
C2 C3 1.37(2) . ?
C3 C4 1.36(2) . ?
C4 C5 1.40(2) . ?
C4 C7 1.570(19) . ?
C5 C6 1.38(2) . ?
C7 C8 1.48(2) . ?
C8 C9 1.374(19) . ?
C8 C13 1.420(17) . ?
C9 C10 1.38(2) . ?
C10 C11 1.39(2) . ?
C10 C14 1.513(19) . ?
C11 C12 1.39(2) . ?
C12 C13 1.36(2) . ?
C13 C15 1.456(18) . ?
C15 C19 1.402(16) . ?
C17 C19 1.370(19) . ?
C20 C21 1.49(2) . ?
C21 C22 1.520(18) . ?
C22 C23 1.51(2) . ?
C23 C24 1.52(2) . ?
C27 C30 1.50(3) . ?
C27 C28 1.51(2) . ?
C27 C29 1.51(2) . ?
C39 C42 1.49(4) . ?
C39 C40 1.54(3) . ?
C39 C41 1.58(3) . ?

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
C16 N1 C15 119.3(11) . . ?
C16 N2 C17 108.4(12) . . ?
C18 N3 C17 105.4(10) . . ?
C18 N3 C20 125.5(11) . . ?
C17 N3 C20 128.5(11) . . ?
C18 N4 C19 104.1(11) . . ?
C20 O2 C23 109.0(10) . . ?
C24 O3 Si1 123.6(9) . . ?
C22 O4 Si2 134.6(11) . . ?
C22 O4 Si2A 110.3(14) . . ?
C21 O5 Si3 121.1(10) . . ?
O3 Si1 C26 102.6(6) . . ?
O3 Si1 C25 110.1(7) . . ?
C26 Si1 C25 113.1(8) . . ?
O3 Si1 C27 112.5(7) . . ?
C26 Si1 C27 109.9(7) . . ?
C25 Si1 C27 108.6(7) . . ?
O4 Si2 C33 107.4(8) . . ?
O4 Si2 C32 109.5(9) . . ?
C33 Si2 C32 110.8(9) . . ?
O4 Si2 C31 108.6(8) . . ?
C33 Si2 C31 109.6(10) . . ?
C32 Si2 C31 110.8(11) . . ?
C36 C33 C34 108.7(16) . . ?
C36 C33 C35 104.5(18) . . ?
C34 C33 C35 108.6(17) . . ?
C36 C33 Si2 112.4(13) . . ?
C34 C33 Si2 110.5(15) . . ?
C35 C33 Si2 111.9(13) . . ?
C33A Si2A C31A 109(2) . . ?
C33A Si2A C32A 109(2) . . ?
C31A Si2A C32A 110(3) . . ?
C33A Si2A O4 106(3) . . ?
C31A Si2A O4 112(3) . . ?
C32A Si2A O4 111(3) . . ?
C36A C33A C34A 109(3) . . ?
C36A C33A C35A 105(3) . . ?
C34A C33A C35A 109(3) . . ?
C36A C33A Si2A 112(3) . . ?
C34A C33A Si2A 110(3) . . ?
C35A C33A Si2A 111(3) . . ?
O5 Si3 C38 111.4(8) . . ?
O5 Si3 C37 107.7(7) . . ?
C38 Si3 C37 109.1(10) . . ?
O5 Si3 C39 108.4(8) . . ?
C38 Si3 C39 108.4(9) . . ?
C37 Si3 C39 112.0(10) . . ?
C6 C1 C2 122.0(17) . . ?
C6 C1 Cl1 120.1(12) . . ?
C2 C1 Cl1 118.0(15) . . ?
C3 C2 C1 117.3(14) . . ?
C4 C3 C2 121.4(13) . . ?
C3 C4 C5 120.2(14) . . ?
C3 C4 C7 122.6(13) . . ?
C5 C4 C7 117.1(13) . . ?
C6 C5 C4 120.1(16) . . ?
C1 C6 C5 118.9(15) . . ?
O1 C7 C8 124.2(13) . . ?
O1 C7 C4 119.1(13) . . ?
C8 C7 C4 115.6(12) . . ?
C9 C8 C13 119.3(13) . . ?
C9 C8 C7 116.9(11) . . ?
C13 C8 C7 123.8(12) . . ?
C8 C9 C10 122.4(12) . . ?
C9 C10 C11 118.1(12) . . ?
C9 C10 C14 121.6(14) . . ?
C11 C10 C14 120.3(15) . . ?
C10 C11 C12 119.7(14) . . ?
C13 C12 C11 122.4(13) . . ?
C12 C13 C8 117.9(12) . . ?
C12 C13 C15 121.5(11) . . ?
C8 C13 C15 120.5(13) . . ?
N1 C15 C19 116.6(12) . . ?
N1 C15 C13 117.0(11) . . ?
C19 C15 C13 126.4(13) . . ?
N1 C16 N2 130.1(14) . . ?
N2 C17 C19 128.5(11) . . ?
N2 C17 N3 124.9(12) . . ?
C19 C17 N3 106.6(11) . . ?
N4 C18 N3 113.2(12) . . ?
C17 C19 C15 117.1(12) . . ?
C17 C19 N4 110.6(10) . . ?
C15 C19 N4 132.3(12) . . ?
O2 C20 N3 108.1(11) . . ?
O2 C20 C21 107.7(11) . . ?
N3 C20 C21 117.4(12) . . ?
O5 C21 C20 112.0(12) . . ?
O5 C21 C22 117.7(12) . . ?
C20 C21 C22 100.0(11) . . ?
O4 C22 C23 109.0(12) . . ?
O4 C22 C21 109.9(11) . . ?
C23 C22 C21 102.6(11) . . ?
O2 C23 C22 104.4(10) . . ?
O2 C23 C24 111.9(12) . . ?
C22 C23 C24 117.4(14) . . ?
O3 C24 C23 108.4(11) . . ?
C30 C27 C28 108.8(14) . . ?
C30 C27 C29 109.6(15) . . ?
C28 C27 C29 111.8(19) . . ?
C30 C27 Si1 111.3(12) . . ?
C28 C27 Si1 107.8(11) . . ?
C29 C27 Si1 107.5(11) . . ?
C42 C39 C40 114.2(19) . . ?
C42 C39 C41 107(2) . . ?
C40 C39 C41 112(2) . . ?
C42 C39 Si3 109.1(14) . . ?
C40 C39 Si3 108.6(15) . . ?
C41 C39 Si3 106.5(16) . . ?

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
C24 O3 Si1 C26 171.9(12) . . . . ?
C24 O3 Si1 C25 51.2(13) . . . . ?
C24 O3 Si1 C27 -70.1(12) . . . . ?
C22 O4 Si2 C33 127.7(13) . . . . ?
C22 O4 Si2 C32 7.3(15) . . . . ?
C22 O4 Si2 C31 -113.8(14) . . . . ?
O4 Si2 C33 C36 -60.3(16) . . . . ?
C32 Si2 C33 C36 59.3(18) . . . . ?
C31 Si2 C33 C36 -178.1(15) . . . . ?
O4 Si2 C33 C34 178.0(14) . . . . ?
C32 Si2 C33 C34 -62.4(18) . . . . ?
C31 Si2 C33 C34 60.3(18) . . . . ?
O4 Si2 C33 C35 56.9(18) . . . . ?
C32 Si2 C33 C35 176.5(16) . . . . ?
C31 Si2 C33 C35 -60.9(19) . . . . ?
C31A Si2A C33A C36A 151(6) . . . . ?
C32A Si2A C33A C36A 31(6) . . . . ?
O4 Si2A C33A C36A -88(6) . . . . ?
C31A Si2A C33A C34A 29(6) . . . . ?
C32A Si2A C33A C34A -91(6) . . . . ?
O4 Si2A C33A C34A 150(6) . . . . ?
C31A Si2A C33A C35A -91(7) . . . . ?
C32A Si2A C33A C35A 149(6) . . . . ?
O4 Si2A C33A C35A 29(6) . . . . ?
C21 O5 Si3 C38 -56.0(14) . . . . ?
C21 O5 Si3 C37 63.6(13) . . . . ?
C21 O5 Si3 C39 -175.1(12) . . . . ?
C6 C1 C2 C3 -1(2) . . . . ?
Cl1 C1 C2 C3 178.2(11) . . . . ?
C1 C2 C3 C4 -2(2) . . . . ?
C2 C3 C4 C5 4(2) . . . . ?
C2 C3 C4 C7 -173.1(12) . . . . ?
C3 C4 C5 C6 -2(2) . . . . ?
C7 C4 C5 C6 175.0(13) . . . . ?
C2 C1 C6 C5 3(2) . . . . ?
Cl1 C1 C6 C5 -176.6(12) . . . . ?
C4 C5 C6 C1 -1(2) . . . . ?
C3 C4 C7 O1 154.9(13) . . . . ?
C5 C4 C7 O1 -21.9(18) . . . . ?
C3 C4 C7 C8 -13.4(17) . . . . ?
C5 C4 C7 C8 169.8(12) . . . . ?
O1 C7 C8 C9 -54(2) . . . . ?
C4 C7 C8 C9 113.3(14) . . . . ?
O1 C7 C8 C13 128.8(16) . . . . ?
C4 C7 C8 C13 -63.5(19) . . . . ?
C13 C8 C9 C10 3(2) . . . . ?
C7 C8 C9 C10 -173.8(14) . . . . ?
C8 C9 C10 C11 0(2) . . . . ?
C8 C9 C10 C14 -178.7(14) . . . . ?
C9 C10 C11 C12 -1(2) . . . . ?
C14 C10 C11 C12 178.0(16) . . . . ?
C10 C11 C12 C13 -2(3) . . . . ?
C11 C12 C13 C8 5(3) . . . . ?
C11 C12 C13 C15 -170.0(16) . . . . ?
C9 C8 C13 C12 -6(2) . . . . ?
C7 C8 C13 C12 171.1(15) . . . . ?
C9 C8 C13 C15 169.5(14) . . . . ?
C7 C8 C13 C15 -14(2) . . . . ?
C16 N1 C15 C19 2(2) . . . . ?
C16 N1 C15 C13 -178.2(14) . . . . ?
C12 C13 C15 N1 161.1(15) . . . . ?
C8 C13 C15 N1 -14(2) . . . . ?
C12 C13 C15 C19 -19(2) . . . . ?
C8 C13 C15 C19 166.1(14) . . . . ?
C15 N1 C16 N2 0(3) . . . . ?
C17 N2 C16 N1 -2(3) . . . . ?
C16 N2 C17 C19 2(2) . . . . ?
C16 N2 C17 N3 -178.0(15) . . . . ?
C18 N3 C17 N2 178.5(14) . . . . ?
C20 N3 C17 N2 7(2) . . . . ?
C18 N3 C17 C19 -1.7(15) . . . . ?
C20 N3 C17 C19 -173.4(13) . . . . ?
C19 N4 C18 N3 -1.4(16) . . . . ?
C17 N3 C18 N4 2.1(17) . . . . ?
C20 N3 C18 N4 174.1(13) . . . . ?
N2 C17 C19 C15 -1(2) . . . . ?
N3 C17 C19 C15 179.4(12) . . . . ?
N2 C17 C19 N4 -179.3(14) . . . . ?
N3 C17 C19 N4 1.0(15) . . . . ?
N1 C15 C19 C17 -1(2) . . . . ?
C13 C15 C19 C17 178.7(14) . . . . ?
N1 C15 C19 N4 176.6(14) . . . . ?
C13 C15 C19 N4 -3(3) . . . . ?
C18 N4 C19 C17 0.3(16) . . . . ?
C18 N4 C19 C15 -177.8(15) . . . . ?
C23 O2 C20 N3 -139.9(12) . . . . ?
C23 O2 C20 C21 -12.1(14) . . . . ?
C18 N3 C20 O2 52.3(18) . . . . ?
C17 N3 C20 O2 -137.5(13) . . . . ?
C18 N3 C20 C21 -69.7(18) . . . . ?
C17 N3 C20 C21 100.4(17) . . . . ?
Si3 O5 C21 C20 117.2(11) . . . . ?
Si3 O5 C21 C22 -127.7(11) . . . . ?
O2 C20 C21 O5 157.8(11) . . . . ?
N3 C20 C21 O5 -80.1(15) . . . . ?
O2 C20 C21 C22 32.3(13) . . . . ?
N3 C20 C21 C22 154.5(11) . . . . ?
Si2 O4 C22 C23 -157.3(10) . . . . ?
Si2A O4 C22 C23 -135.7(14) . . . . ?
Si2 O4 C22 C21 91.0(14) . . . . ?
Si2A O4 C22 C21 112.6(15) . . . . ?
O5 C21 C22 O4 -45.1(18) . . . . ?
C20 C21 C22 O4 76.4(14) . . . . ?
O5 C21 C22 C23 -161.0(13) . . . . ?
C20 C21 C22 C23 -39.5(13) . . . . ?
C20 O2 C23 C22 -13.8(14) . . . . ?
C20 O2 C23 C24 114.2(13) . . . . ?
O4 C22 C23 O2 -82.8(12) . . . . ?
C21 C22 C23 O2 33.6(13) . . . . ?
O4 C22 C23 C24 152.6(11) . . . . ?
C21 C22 C23 C24 -90.9(14) . . . . ?
Si1 O3 C24 C23 -142.5(11) . . . . ?
O2 C23 C24 O3 -60.6(16) . . . . ?
C22 C23 C24 O3 60.1(17) . . . . ?
O5 Si3 C39 C42 51.2(16) . . . . ?
C38 Si3 C39 C42 -69.8(17) . . . . ?
C37 Si3 C39 C42 169.9(15) . . . . ?
O5 Si3 C39 C40 176.3(17) . . . . ?
C38 Si3 C39 C40 55(2) . . . . ?
C37 Si3 C39 C40 -65(2) . . . . ?
O5 Si3 C39 C41 -63.4(19) . . . . ?
C38 Si3 C39 C41 175.6(18) . . . . ?
C37 Si3 C39 C41 55(2) . . . . ?

_refine_diff_density_max         0.822
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.146

####################################################################### 
# 
# 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_ml1_0m
_database_code_depnum_ccdc_archive 'CCDC 2333366'
loop_
_audit_author_name
_audit_author_address
'Michelle Neary'
;Hunter College
United States of America
;
_audit_update_record             
;
2024-02-16 deposited with the CCDC.	2024-06-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32.50 H23.50 N4 O'
_chemical_formula_weight         486.05

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9632(2)
_cell_length_b                   11.4926(2)
_cell_length_c                   12.0157(2)
_cell_angle_alpha                91.2850(10)
_cell_angle_beta                 98.9400(10)
_cell_angle_gamma                113.2640(10)
_cell_volume                     1243.28(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9990
_cell_measurement_theta_min      3.45
_cell_measurement_theta_max      30.03

_exptl_crystal_description       bar
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             509
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.9549
_exptl_absorpt_correction_T_max  0.9857
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26186
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         30.03
_reflns_number_total             7201
_reflns_number_gt                6077
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0661P)²+0.2896P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7201
_refine_ls_number_parameters     338
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0452
_refine_ls_wR_factor_ref         0.1275
_refine_ls_wR_factor_gt          0.1197
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.91199(9) 0.31869(8) 0.35368(7) 0.03277(18) Uani 1 1 d . . .
N1 N 0.57939(10) 0.32244(8) 0.24444(8) 0.02567(18) Uani 1 1 d . . .
N2 N 0.38512(11) 0.39898(8) 0.21257(8) 0.02882(19) Uani 1 1 d . . .
N3 N 0.20837(10) 0.06127(8) 0.14955(9) 0.0298(2) Uani 1 1 d . . .
N4 N 0.14303(10) 0.22825(9) 0.15063(8) 0.02674(18) Uani 1 1 d . . .
C1 C 0.48521(11) 0.20029(9) 0.21569(8) 0.02188(18) Uani 1 1 d . . .
C2 C 0.52580(13) 0.41273(10) 0.24229(10) 0.0296(2) Uani 1 1 d . . .
H2 H 0.5969 0.4972 0.2648 0.036 Uiso 1 1 calc R . .
C3 C 0.29402(11) 0.27723(9) 0.18460(8) 0.02372(19) Uani 1 1 d . . .
C4 C 0.33378(11) 0.17270(9) 0.18405(8) 0.02292(19) Uani 1 1 d . . .
C5 C 0.09969(12) 0.09997(10) 0.13081(10) 0.0308(2) Uani 1 1 d . . .
H5 H -0.0009 0.0432 0.1055 0.037 Uiso 1 1 calc R . .
C6 C 0.55184(10) 0.10622(9) 0.21597(8) 0.02102(18) Uani 1 1 d . . .
C7 C 0.47833(11) -0.00665(9) 0.14757(8) 0.02291(19) Uani 1 1 d . . .
H7 H 0.3816 -0.0256 0.1064 0.027 Uiso 1 1 calc R . .
C8 C 0.54368(11) -0.09494(9) 0.13735(8) 0.02167(18) Uani 1 1 d . . .
C9 C 0.46793(12) -0.21163(10) 0.06844(9) 0.0263(2) Uani 1 1 d . . .
H9 H 0.3703 -0.2325 0.0280 0.032 Uiso 1 1 calc R . .
C10 C 0.53470(12) -0.29446(10) 0.05984(9) 0.0285(2) Uani 1 1 d . . .
H10 H 0.4830 -0.3725 0.0136 0.034 Uiso 1 1 calc R . .
C11 C 0.67947(12) -0.26481(10) 0.11910(9) 0.0286(2) Uani 1 1 d . . .
H11 H 0.7249 -0.3227 0.1121 0.034 Uiso 1 1 calc R . .
C12 C 0.75535(12) -0.15293(10) 0.18685(9) 0.0264(2) Uani 1 1 d . . .
H12 H 0.8527 -0.1341 0.2268 0.032 Uiso 1 1 calc R . .
C13 C 0.68931(11) -0.06523(9) 0.19752(8) 0.02160(18) Uani 1 1 d . . .
C14 C 0.76335(11) 0.05108(9) 0.26749(8) 0.02271(19) Uani 1 1 d . . .
H14 H 0.8610 0.0717 0.3077 0.027 Uiso 1 1 calc R . .
C15 C 0.69745(10) 0.13471(9) 0.27865(8) 0.02105(18) Uani 1 1 d . . .
C16 C 0.78466(11) 0.25098(9) 0.36140(8) 0.02335(19) Uani 1 1 d . . .
C17 C 0.71737(11) 0.27323(9) 0.45807(8) 0.02403(19) Uani 1 1 d . . .
C18 C 0.77395(13) 0.39459(11) 0.51453(10) 0.0320(2) Uani 1 1 d . . .
H18 H 0.8549 0.4614 0.4919 0.038 Uiso 1 1 calc R . .
C19 C 0.71197(15) 0.41777(12) 0.60385(11) 0.0391(3) Uani 1 1 d . . .
H19 H 0.7489 0.5011 0.6409 0.047 Uiso 1 1 calc R . .
C20 C 0.59686(16) 0.32030(14) 0.63912(10) 0.0409(3) Uani 1 1 d . . .
H20 H 0.5557 0.3365 0.7009 0.049 Uiso 1 1 calc R . .
C21 C 0.54161(16) 0.19927(13) 0.58460(11) 0.0422(3) Uani 1 1 d . . .
H21 H 0.4632 0.1320 0.6094 0.051 Uiso 1 1 calc R . .
C22 C 0.60088(14) 0.17592(11) 0.49333(10) 0.0327(2) Uani 1 1 d . . .
H22 H 0.5614 0.0930 0.4550 0.039 Uiso 1 1 calc R . .
C23 C 0.05033(13) 0.30087(11) 0.12795(10) 0.0307(2) Uani 1 1 d . . .
H23A H 0.0893 0.3767 0.1834 0.037 Uiso 1 1 calc R . .
H23B H -0.0523 0.2475 0.1377 0.037 Uiso 1 1 calc R . .
C24 C 0.04800(11) 0.34254(9) 0.00985(9) 0.02446(19) Uani 1 1 d . . .
C25 C -0.04930(12) 0.26036(11) -0.08143(11) 0.0333(2) Uani 1 1 d . . .
H25 H -0.1140 0.1769 -0.0696 0.040 Uiso 1 1 calc R . .
C26 C -0.05208(15) 0.29999(14) -0.18975(12) 0.0435(3) Uani 1 1 d . . .
H26 H -0.1195 0.2439 -0.2518 0.052 Uiso 1 1 calc R . .
C27 C 0.04325(16) 0.42097(14) -0.20756(11) 0.0423(3) Uani 1 1 d . . .
H27 H 0.0418 0.4479 -0.2818 0.051 Uiso 1 1 calc R . .
C28 C 0.14046(14) 0.50239(12) -0.11727(11) 0.0355(3) Uani 1 1 d . . .
H28 H 0.2061 0.5854 -0.1295 0.043 Uiso 1 1 calc R . .
C29 C 0.14295(11) 0.46381(10) -0.00892(10) 0.0283(2) Uani 1 1 d . . .
H29 H 0.2099 0.5206 0.0529 0.034 Uiso 1 1 calc R . .
C1T C 0.1951(3) 0.2284(2) 0.47760(16) 0.0937(16) Uani 0.50 1 d P . .
H1T1 H 0.1541 0.2631 0.4137 0.141 Uiso 0.50 1 calc PR . .
H1T2 H 0.2851 0.2206 0.4622 0.141 Uiso 0.50 1 calc PR . .
H1T3 H 0.2197 0.2855 0.5464 0.141 Uiso 0.50 1 calc PR . .
C2T C 0.0994(3) 0.1191(2) 0.49122(16) 0.0962(8) Uani 1 1 d R . .
C3T C -0.0158(3) 0.1022(2) 0.54727(16) 0.1012(10) Uani 1 1 d R . .
H3T H -0.0255 0.1739 0.5799 0.121 Uiso 1 1 calc R . .
C4T C -0.1140(4) -0.0144(4) 0.5560(2) 0.1091(11) Uani 1 1 d . . .
H4T H -0.1941 -0.0261 0.5946 0.131 Uiso 1 1 calc R . .


_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 C16 1.2180(12) . ?
N1 C2 1.3404(13) . ?
N1 C1 1.3444(13) . ?
N2 C3 1.3325(13) . ?
N2 C2 1.3357(14) . ?
N3 C5 1.3154(14) . ?
N3 C4 1.3871(13) . ?
N4 C5 1.3660(14) . ?
N4 C3 1.3698(13) . ?
N4 C23 1.4713(13) . ?
C1 C4 1.3999(14) . ?
C1 C6 1.4751(13) . ?
C3 C4 1.4059(13) . ?
C6 C7 1.3818(13) . ?
C6 C15 1.4329(13) . ?
C7 C8 1.4176(13) . ?
C8 C9 1.4178(13) . ?
C8 C13 1.4198(13) . ?
C9 C10 1.3698(14) . ?
C10 C11 1.4090(16) . ?
C11 C12 1.3716(15) . ?
C12 C13 1.4176(13) . ?
C13 C14 1.4198(13) . ?
C14 C15 1.3759(13) . ?
C15 C16 1.5112(13) . ?
C16 C17 1.4927(14) . ?
C17 C22 1.3878(15) . ?
C17 C18 1.3932(14) . ?
C18 C19 1.3882(16) . ?
C19 C20 1.381(2) . ?
C20 C21 1.3816(19) . ?
C21 C22 1.3917(16) . ?
C23 C24 1.5074(15) . ?
C24 C29 1.3882(14) . ?
C24 C25 1.3909(15) . ?
C25 C26 1.3885(19) . ?
C26 C27 1.384(2) . ?
C27 C28 1.379(2) . ?
C28 C29 1.3845(17) . ?
C1T C2T 1.2746 . ?
C2T C3T 1.3705 . ?
C2T C4T 1.387(4) 2_556 ?
C3T C4T 1.330(4) . ?
C4T C2T 1.387(4) 2_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 N1 C1 119.35(9) . . ?
C3 N2 C2 111.28(9) . . ?
C5 N3 C4 103.72(9) . . ?
C5 N4 C3 105.66(8) . . ?
C5 N4 C23 127.34(9) . . ?
C3 N4 C23 126.66(9) . . ?
N1 C1 C4 118.13(9) . . ?
N1 C1 C6 116.63(9) . . ?
C4 C1 C6 125.20(9) . . ?
N2 C2 N1 128.22(10) . . ?
N2 C3 N4 127.21(9) . . ?
N2 C3 C4 126.81(9) . . ?
N4 C3 C4 105.98(9) . . ?
N3 C4 C1 133.81(9) . . ?
N3 C4 C3 109.99(9) . . ?
C1 C4 C3 116.20(9) . . ?
N3 C5 N4 114.65(10) . . ?
C7 C6 C15 119.31(8) . . ?
C7 C6 C1 119.58(9) . . ?
C15 C6 C1 120.89(8) . . ?
C6 C7 C8 121.63(9) . . ?
C7 C8 C9 121.84(9) . . ?
C7 C8 C13 118.98(9) . . ?
C9 C8 C13 119.18(9) . . ?
C10 C9 C8 120.36(10) . . ?
C9 C10 C11 120.51(10) . . ?
C12 C11 C10 120.51(9) . . ?
C11 C12 C13 120.34(9) . . ?
C12 C13 C14 122.18(9) . . ?
C12 C13 C8 119.11(9) . . ?
C14 C13 C8 118.71(8) . . ?
C15 C14 C13 121.75(9) . . ?
C14 C15 C6 119.59(9) . . ?
C14 C15 C16 116.31(8) . . ?
C6 C15 C16 124.07(8) . . ?
O1 C16 C17 121.12(9) . . ?
O1 C16 C15 119.81(9) . . ?
C17 C16 C15 118.79(8) . . ?
C22 C17 C18 119.40(10) . . ?
C22 C17 C16 121.60(9) . . ?
C18 C17 C16 118.99(9) . . ?
C19 C18 C17 119.96(11) . . ?
C20 C19 C18 120.34(11) . . ?
C19 C20 C21 120.02(11) . . ?
C20 C21 C22 119.98(12) . . ?
C17 C22 C21 120.27(10) . . ?
N4 C23 C24 111.56(8) . . ?
C29 C24 C25 119.23(10) . . ?
C29 C24 C23 120.24(10) . . ?
C25 C24 C23 120.53(10) . . ?
C26 C25 C24 120.19(11) . . ?
C27 C26 C25 120.11(12) . . ?
C28 C27 C26 119.80(12) . . ?
C27 C28 C29 120.37(11) . . ?
C28 C29 C24 120.29(11) . . ?
C1T C2T C3T 123.1 . . ?
C1T C2T C4T 116.9(2) . 2_556 ?
C3T C2T C4T 120.0(2) . 2_556 ?
C4T C3T C2T 120.09(16) . . ?
C3T C4T C2T 119.9(3) . 2_556 ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        30.03
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.046
