# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_JVR180719O1
_database_code_depnum_ccdc_archive 'CCDC 1956669'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2019-09-30 deposited with the CCDC.	2020-01-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H31 N O2'
_chemical_formula_weight         485.60

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                   8.7448(8)
_cell_length_b                   12.2039(12)
_cell_length_c                   13.7109(12)
_cell_angle_alpha                71.125(4)
_cell_angle_beta                 73.114(4)
_cell_angle_gamma                76.737(4)
_cell_volume                     1309.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9968
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      28.30

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_F_000             516
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.583
_exptl_crystal_size_mid          0.473
_exptl_crystal_size_min          0.445
_exptl_absorpt_coefficient_mu    0.076
_shelx_estimated_absorpt_T_min   0.957
_shelx_estimated_absorpt_T_max   0.967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5569
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_absorpt_special_details   
;
The ratio of minimum to maximum
apparent transmission was 0.747
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            43758
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_av_R_equivalents  0.1077
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.462
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             5102
_reflns_number_gt                3978
_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       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'APEX3 v2016.9-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          'Bruker SHELXTL'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1138P)²+3.1540P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5102
_refine_ls_number_parameters     344
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0763
_refine_ls_wR_factor_ref         0.2467
_refine_ls_wR_factor_gt          0.2389
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_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
O1 O 0.5252(3) 0.55727(19) 0.81315(18) 0.0214(5) Uani 1 1 d . . . . .
O2 O 0.6838(3) 0.56125(19) 0.40673(18) 0.0198(5) Uani 1 1 d . . . . .
N1 N 0.4932(3) 0.6220(2) 0.5957(2) 0.0201(6) Uani 1 1 d . . . . .
H1 H 0.441(6) 0.588(4) 0.667(4) 0.051(14) Uiso 1 1 d . . . . .
H2 H 0.499(5) 0.587(4) 0.545(4) 0.039(12) Uiso 1 1 d . . . . .
C1 C 0.6209(4) 0.6783(3) 0.5801(2) 0.0165(6) Uani 1 1 d . . . . .
C2 C 0.6464(4) 0.7093(3) 0.6647(2) 0.0170(6) Uani 1 1 d . . . . .
C3 C 0.7854(4) 0.7553(3) 0.6490(2) 0.0190(7) Uani 1 1 d . . . . .
H3 H 0.804758 0.773169 0.706416 0.023 Uiso 1 1 calc R U . . .
C4 C 0.8971(4) 0.7760(3) 0.5522(3) 0.0212(7) Uani 1 1 d . . . . .
H4 H 0.992509 0.806227 0.543558 0.025 Uiso 1 1 calc R U . . .
C5 C 0.8666(4) 0.7517(3) 0.4684(2) 0.0193(7) Uani 1 1 d . . . . .
H5 H 0.942456 0.765702 0.401816 0.023 Uiso 1 1 calc R U . . .
C6 C 0.7278(4) 0.7073(3) 0.4790(2) 0.0178(6) Uani 1 1 d . . . . .
C7 C 0.6912(4) 0.6844(3) 0.3847(2) 0.0179(7) Uani 1 1 d . . . . .
C8 C 0.8115(4) 0.4815(3) 0.4493(3) 0.0247(7) Uani 1 1 d . . . . .
H8A H 0.812461 0.403260 0.443619 0.037 Uiso 1 1 calc R U . . .
H8B H 0.794357 0.478293 0.523942 0.037 Uiso 1 1 calc R U . . .
H8C H 0.915256 0.508160 0.409331 0.037 Uiso 1 1 calc R U . . .
C9 C 0.8128(4) 0.7252(3) 0.2782(2) 0.0207(7) Uani 1 1 d . . . . .
C10 C 0.8346(4) 0.8423(3) 0.2377(3) 0.0262(7) Uani 1 1 d . . . . .
H10 H 0.775494 0.896198 0.277024 0.031 Uiso 1 1 calc R U . . .
C11 C 0.9397(5) 0.8818(4) 0.1421(3) 0.0354(9) Uani 1 1 d . . . . .
H11 H 0.955822 0.961478 0.117271 0.043 Uiso 1 1 calc R U . . .
C12 C 1.0223(5) 0.8050(4) 0.0818(3) 0.0375(10) Uani 1 1 d . . . . .
H12 H 1.095279 0.831612 0.015771 0.045 Uiso 1 1 calc R U . . .
C13 C 0.9973(5) 0.6901(4) 0.1188(3) 0.0339(9) Uani 1 1 d . . . . .
H13 H 1.052068 0.637433 0.077307 0.041 Uiso 1 1 calc R U . . .
C14 C 0.8925(4) 0.6498(3) 0.2165(3) 0.0257(7) Uani 1 1 d . . . . .
H14 H 0.875761 0.570278 0.240901 0.031 Uiso 1 1 calc R U . . .
C15 C 0.5238(4) 0.7486(3) 0.3666(2) 0.0180(6) Uani 1 1 d . . . . .
C16 C 0.4497(4) 0.7116(3) 0.3085(3) 0.0215(7) Uani 1 1 d . . . . .
H16 H 0.499050 0.643859 0.284930 0.026 Uiso 1 1 calc R U . . .
C17 C 0.3046(4) 0.7724(3) 0.2845(3) 0.0277(8) Uani 1 1 d . . . . .
H17 H 0.255175 0.746198 0.244520 0.033 Uiso 1 1 calc R U . . .
C18 C 0.2319(4) 0.8706(3) 0.3184(3) 0.0269(8) Uani 1 1 d . . . . .
H18 H 0.132264 0.912013 0.302097 0.032 Uiso 1 1 calc R U . . .
C19 C 0.3037(4) 0.9087(3) 0.3760(3) 0.0289(8) Uani 1 1 d . . . . .
H19 H 0.253442 0.976137 0.399843 0.035 Uiso 1 1 calc R U . . .
C20 C 0.4501(4) 0.8481(3) 0.3993(3) 0.0249(7) Uani 1 1 d . . . . .
H20 H 0.500039 0.875357 0.438206 0.030 Uiso 1 1 calc R U . . .
C21 C 0.5268(4) 0.6825(3) 0.7736(2) 0.0182(7) Uani 1 1 d . . . . .
C22 C 0.6797(4) 0.4870(3) 0.8010(3) 0.0268(8) Uani 1 1 d . . . . .
H22A H 0.671521 0.408287 0.849420 0.040 Uiso 1 1 calc R U . . .
H22B H 0.755727 0.522383 0.817419 0.040 Uiso 1 1 calc R U . . .
H22C H 0.718480 0.481929 0.727736 0.040 Uiso 1 1 calc R U . . .
C23 C 0.5651(4) 0.7266(3) 0.8562(2) 0.0197(7) Uani 1 1 d . . . . .
C24 C 0.5968(4) 0.6504(3) 0.9503(3) 0.0256(7) Uani 1 1 d . . . . .
H24 H 0.598116 0.568832 0.963842 0.031 Uiso 1 1 calc R U . . .
C25 C 0.6268(5) 0.6921(4) 1.0253(3) 0.0329(9) Uani 1 1 d . . . . .
H25 H 0.649194 0.638671 1.089204 0.039 Uiso 1 1 calc R U . . .
C26 C 0.6243(5) 0.8103(4) 1.0075(3) 0.0331(9) Uani 1 1 d . . . . .
H26 H 0.646493 0.838365 1.058254 0.040 Uiso 1 1 calc R U . . .
C27 C 0.5891(5) 0.8872(4) 0.9153(3) 0.0315(8) Uani 1 1 d . . . . .
H27 H 0.585207 0.968937 0.902986 0.038 Uiso 1 1 calc R U . . .
C28 C 0.5593(4) 0.8461(3) 0.8403(3) 0.0254(7) Uani 1 1 d . . . . .
H28 H 0.534561 0.900118 0.777246 0.030 Uiso 1 1 calc R U . . .
C29 C 0.3527(4) 0.7373(3) 0.7669(2) 0.0192(7) Uani 1 1 d . . . . .
C30 C 0.3201(4) 0.8427(3) 0.6924(3) 0.0237(7) Uani 1 1 d . . . . .
H30 H 0.407071 0.878857 0.641965 0.028 Uiso 1 1 calc R U . . .
C31 C 0.1623(4) 0.8959(3) 0.6905(3) 0.0277(8) Uani 1 1 d . . . . .
H31 H 0.141855 0.967941 0.639025 0.033 Uiso 1 1 calc R U . . .
C32 C 0.0348(4) 0.8442(3) 0.7636(3) 0.0311(8) Uani 1 1 d . . . . .
H32 H -0.073338 0.881207 0.763285 0.037 Uiso 1 1 calc R U . . .
C33 C 0.0655(4) 0.7379(4) 0.8374(3) 0.0312(8) Uani 1 1 d . . . . .
H33 H -0.021711 0.701192 0.886923 0.037 Uiso 1 1 calc R U . . .
C34 C 0.2234(4) 0.6853(3) 0.8388(3) 0.0253(7) Uani 1 1 d . . . . .
H34 H 0.243466 0.612574 0.889553 0.030 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 C22 1.421(4) . ?
O1 C21 1.449(4) . ?
O2 C8 1.431(4) . ?
O2 C7 1.447(4) . ?
N1 C1 1.373(4) . ?
N1 H1 0.95(5) . ?
N1 H2 0.91(5) . ?
C1 C6 1.415(4) . ?
C1 C2 1.417(4) . ?
C2 C3 1.386(4) . ?
C2 C21 1.537(4) . ?
C3 C4 1.387(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.383(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.392(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.538(4) . ?
C7 C15 1.542(4) . ?
C7 C9 1.544(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C14 1.383(5) . ?
C9 C10 1.392(5) . ?
C10 C11 1.375(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.387(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.374(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.394(5) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C20 1.385(5) . ?
C15 C16 1.386(4) . ?
C16 C17 1.387(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.377(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.376(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.392(5) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C29 1.532(4) . ?
C21 C23 1.543(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.385(5) . ?
C23 C28 1.395(5) . ?
C24 C25 1.394(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.379(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.379(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.388(5) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.390(5) . ?
C29 C30 1.390(5) . ?
C30 C31 1.388(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.382(5) . ?
C31 H31 0.9500 . ?
C32 C33 1.389(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.385(5) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?

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
C22 O1 C21 115.2(2) . . ?
C8 O2 C7 115.9(2) . . ?
C1 N1 H1 117(3) . . ?
C1 N1 H2 116(3) . . ?
H1 N1 H2 119(4) . . ?
N1 C1 C6 120.3(3) . . ?
N1 C1 C2 120.4(3) . . ?
C6 C1 C2 119.2(3) . . ?
C3 C2 C1 118.8(3) . . ?
C3 C2 C21 121.5(3) . . ?
C1 C2 C21 119.5(3) . . ?
C2 C3 C4 122.2(3) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 H3 118.9 . . ?
C5 C4 C3 118.6(3) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
C4 C5 C6 121.8(3) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C5 C6 C1 119.0(3) . . ?
C5 C6 C7 121.7(3) . . ?
C1 C6 C7 119.3(3) . . ?
O2 C7 C6 110.0(2) . . ?
O2 C7 C15 105.3(2) . . ?
C6 C7 C15 111.7(3) . . ?
O2 C7 C9 109.7(2) . . ?
C6 C7 C9 114.0(3) . . ?
C15 C7 C9 105.7(2) . . ?
O2 C8 H8A 109.5 . . ?
O2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C14 C9 C10 118.2(3) . . ?
C14 C9 C7 121.5(3) . . ?
C10 C9 C7 120.1(3) . . ?
C11 C10 C9 121.5(4) . . ?
C11 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C10 C11 C12 119.9(4) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C13 C12 C11 119.3(3) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C12 C13 C14 120.7(4) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C9 C14 C13 120.3(3) . . ?
C9 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C20 C15 C16 118.5(3) . . ?
C20 C15 C7 122.0(3) . . ?
C16 C15 C7 119.4(3) . . ?
C15 C16 C17 120.8(3) . . ?
C15 C16 H16 119.6 . . ?
C17 C16 H16 119.6 . . ?
C18 C17 C16 120.1(3) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C19 C18 C17 119.9(3) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 C20 119.9(3) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
C15 C20 C19 120.8(3) . . ?
C15 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
O1 C21 C29 105.6(2) . . ?
O1 C21 C2 109.0(2) . . ?
C29 C21 C2 112.2(2) . . ?
O1 C21 C23 109.6(2) . . ?
C29 C21 C23 106.5(2) . . ?
C2 C21 C23 113.7(2) . . ?
O1 C22 H22A 109.5 . . ?
O1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
O1 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C28 118.1(3) . . ?
C24 C23 C21 121.5(3) . . ?
C28 C23 C21 120.2(3) . . ?
C23 C24 C25 120.8(3) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C26 C25 C24 120.5(3) . . ?
C26 C25 H25 119.7 . . ?
C24 C25 H25 119.7 . . ?
C25 C26 C27 119.3(3) . . ?
C25 C26 H26 120.4 . . ?
C27 C26 H26 120.4 . . ?
C26 C27 C28 120.4(4) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C27 C28 C23 120.9(3) . . ?
C27 C28 H28 119.6 . . ?
C23 C28 H28 119.6 . . ?
C34 C29 C30 118.4(3) . . ?
C34 C29 C21 120.6(3) . . ?
C30 C29 C21 121.0(3) . . ?
C31 C30 C29 121.0(3) . . ?
C31 C30 H30 119.5 . . ?
C29 C30 H30 119.5 . . ?
C32 C31 C30 120.0(3) . . ?
C32 C31 H31 120.0 . . ?
C30 C31 H31 120.0 . . ?
C31 C32 C33 119.6(3) . . ?
C31 C32 H32 120.2 . . ?
C33 C32 H32 120.2 . . ?
C34 C33 C32 120.0(3) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C33 C34 C29 120.9(3) . . ?
C33 C34 H34 119.5 . . ?
C29 C34 H34 119.5 . . ?

_refine_diff_density_max         0.516
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.090

####################################################################### 
# 
# 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_jvr190128O1
_database_code_depnum_ccdc_archive 'CCDC 1956673'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2019-09-30 deposited with the CCDC.	2020-01-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H30.50 N O2.50'
_chemical_formula_weight         505.10

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           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                   16.515(4)
_cell_length_b                   6.8442(13)
_cell_length_c                   24.238(4)
_cell_angle_alpha                90
_cell_angle_beta                 105.844(6)
_cell_angle_gamma                90
_cell_volume                     2635.6(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3321
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      25.40

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_F_000             1070
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.079
_shelx_estimated_absorpt_T_min   0.976
_shelx_estimated_absorpt_T_max   0.985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7957
_exptl_absorpt_correction_T_max  0.9585
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_absorpt_special_details   
;
The ratio of minimum to maximum
apparent transmission was 0.830
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            31014
_diffrn_reflns_av_unetI/netI     0.1056
_diffrn_reflns_av_R_equivalents  0.1790
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.433
_diffrn_reflns_theta_max         26.393
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5468
_reflns_number_gt                3313
_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       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'APEX3 v2016.9-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_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)+(0.0809P)²+2.4572P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0126(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5468
_refine_ls_number_parameters     373
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1437
_refine_ls_R_factor_gt           0.0791
_refine_ls_wR_factor_ref         0.2014
_refine_ls_wR_factor_gt          0.1711
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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
O1 O 0.80158(19) -0.3748(4) 0.53778(12) 0.0350(7) Uani 1 1 d . . . . .
H1A H 0.758(3) -1.183(7) 0.469(2) 0.058(17) Uiso 1 1 d . . . . .
O2 O 0.76741(16) -1.1274(4) 0.44060(12) 0.0307(7) Uani 1 1 d . . . . .
H2A H 0.819(4) -0.446(8) 0.515(2) 0.08(2) Uiso 1 1 d . . . . .
N1 N 0.81686(19) -0.7512(5) 0.49331(15) 0.0270(8) Uani 1 1 d . . . . .
H1 H 0.824(2) -0.839(6) 0.4706(16) 0.025(11) Uiso 1 1 d . . . . .
H2 H 0.851(3) -0.748(7) 0.529(2) 0.050(13) Uiso 1 1 d . . . . .
C1 C 0.7329(2) -0.7626(5) 0.49589(13) 0.0202(8) Uani 1 1 d . . . . .
C2 C 0.7080(2) -0.6447(5) 0.53646(13) 0.0201(8) Uani 1 1 d . . . . .
C3 C 0.6244(2) -0.6467(5) 0.53759(14) 0.0229(8) Uani 1 1 d . . . . .
H3 H 0.607787 -0.571117 0.565513 0.027 Uiso 1 1 calc R U . . .
C4 C 0.5653(2) -0.7560(5) 0.49910(14) 0.0209(8) Uani 1 1 d . . . . .
H4 H 0.508259 -0.754968 0.500192 0.025 Uiso 1 1 calc R U . . .
C5 C 0.5896(2) -0.8681(5) 0.45851(14) 0.0216(8) Uani 1 1 d . . . . .
H5 H 0.548220 -0.940996 0.431413 0.026 Uiso 1 1 calc R U . . .
C6 C 0.6727(2) -0.8763(5) 0.45653(13) 0.0186(7) Uani 1 1 d . . . . .
C7 C 0.7718(2) -0.5047(5) 0.57493(14) 0.0218(8) Uani 1 1 d . . . . .
C8 C 0.8469(2) -0.6100(5) 0.61481(14) 0.0230(8) Uani 1 1 d . . . . .
C9 C 0.8409(2) -0.7985(6) 0.63366(14) 0.0282(9) Uani 1 1 d . . . . .
H9 H 0.790039 -0.869594 0.619728 0.034 Uiso 1 1 calc R U . . .
C10 C 0.9089(3) -0.8845(7) 0.67286(16) 0.0405(11) Uani 1 1 d . . . . .
H10 H 0.904392 -1.014540 0.685406 0.049 Uiso 1 1 calc R U . . .
C11 C 0.9828(3) -0.7821(8) 0.69368(18) 0.0512(13) Uani 1 1 d . . . . .
H11 H 1.028984 -0.840496 0.720939 0.061 Uiso 1 1 calc R U . . .
C12 C 0.9893(3) -0.5961(8) 0.67483(17) 0.0497(13) Uani 1 1 d . . . . .
H12 H 1.040478 -0.526077 0.688763 0.060 Uiso 1 1 calc R U . . .
C13 C 0.9228(2) -0.5093(7) 0.63611(16) 0.0361(10) Uani 1 1 d . . . . .
H13 H 0.928266 -0.379628 0.623595 0.043 Uiso 1 1 calc R U . . .
C14 C 0.7302(2) -0.3747(5) 0.61084(14) 0.0227(8) Uani 1 1 d . . . . .
C15 C 0.7336(2) -0.4233(5) 0.66704(15) 0.0294(9) Uani 1 1 d . . . . .
H15 H 0.764299 -0.535355 0.684154 0.035 Uiso 1 1 calc R U . . .
C16 C 0.6926(3) -0.3095(6) 0.69842(16) 0.0348(10) Uani 1 1 d . . . . .
H16 H 0.695608 -0.344292 0.736869 0.042 Uiso 1 1 calc R U . . .
C17 C 0.6475(3) -0.1462(6) 0.67431(16) 0.0331(9) Uani 1 1 d . . . . .
H17 H 0.619331 -0.068311 0.695767 0.040 Uiso 1 1 calc R U . . .
C18 C 0.6441(2) -0.0986(6) 0.61833(17) 0.0316(9) Uani 1 1 d . . . . .
H18 H 0.613034 0.012912 0.601148 0.038 Uiso 1 1 calc R U . . .
C19 C 0.6850(2) -0.2105(5) 0.58705(16) 0.0277(9) Uani 1 1 d . . . . .
H19 H 0.682198 -0.174622 0.548718 0.033 Uiso 1 1 calc R U . . .
C20 C 0.6987(2) -1.0021(5) 0.41185(13) 0.0199(8) Uani 1 1 d . . . . .
C21 C 0.6246(2) -1.1289(5) 0.37858(14) 0.0214(8) Uani 1 1 d . . . . .
C22 C 0.5793(2) -1.0847(6) 0.32323(14) 0.0260(8) Uani 1 1 d . . . . .
H22 H 0.595843 -0.976769 0.304181 0.031 Uiso 1 1 calc R U . . .
C23 C 0.5097(3) -1.1954(6) 0.29482(16) 0.0340(10) Uani 1 1 d . . . . .
H23 H 0.479022 -1.162760 0.256763 0.041 Uiso 1 1 calc R U . . .
C24 C 0.4855(3) -1.3520(6) 0.32198(16) 0.0331(9) Uani 1 1 d . . . . .
H24 H 0.437573 -1.426790 0.302929 0.040 Uiso 1 1 calc R U . . .
C25 C 0.5311(2) -1.4009(6) 0.37711(17) 0.0317(9) Uani 1 1 d . . . . .
H25 H 0.514849 -1.510079 0.395845 0.038 Uiso 1 1 calc R U . . .
C26 C 0.5999(2) -1.2909(5) 0.40468(16) 0.0265(8) Uani 1 1 d . . . . .
H26 H 0.631325 -1.326334 0.442338 0.032 Uiso 1 1 calc R U . . .
C27 C 0.7322(2) -0.8775(5) 0.37049(13) 0.0221(8) Uani 1 1 d . . . . .
C28 C 0.7009(3) -0.6921(6) 0.35604(16) 0.0341(10) Uani 1 1 d . . . . .
H28 H 0.660405 -0.639890 0.373262 0.041 Uiso 1 1 calc R U . . .
C29 C 0.7280(3) -0.5810(6) 0.31660(18) 0.0444(12) Uani 1 1 d . . . . .
H29 H 0.706822 -0.452448 0.307552 0.053 Uiso 1 1 calc R U . . .
C30 C 0.7856(3) -0.6565(7) 0.29057(17) 0.0376(10) Uani 1 1 d . . . . .
H30 H 0.802822 -0.582183 0.262665 0.045 Uiso 1 1 calc R U . . .
C31 C 0.8178(3) -0.8401(7) 0.30528(16) 0.0351(10) Uani 1 1 d . . . . .
H31 H 0.858586 -0.891713 0.288226 0.042 Uiso 1 1 calc R U . . .
C32 C 0.7910(2) -0.9502(6) 0.34482(15) 0.0290(9) Uani 1 1 d . . . . .
H32 H 0.813343 -1.077504 0.354445 0.035 Uiso 1 1 calc R U . . .
C33 C 0.9764(3) -0.1344(12) 0.4569(2) 0.074(2) Uani 1 1 d . . . . .
H33 H 0.959866 -0.226904 0.426664 0.089 Uiso 1 1 calc R U . . .
C34 C 0.9816(3) -0.1897(11) 0.5127(2) 0.0738(19) Uani 1 1 d . . . . .
H34 H 0.968993 -0.320086 0.520949 0.089 Uiso 1 1 calc R U . . .
C35 C 1.0045(3) -0.0575(13) 0.5550(2) 0.075(2) Uani 1 1 d . . . . .
H35 H 1.007831 -0.094496 0.593366 0.090 Uiso 1 1 calc R U . . .
O3 O 0.8440(13) -0.440(4) 0.4136(9) 0.105(6) Uani 0.25 1 d G . P . .
H3A H 0.797349 -0.448549 0.389470 0.158 Uiso 0.25 1 d G U P . .
H3B H 0.840828 -0.367973 0.443450 0.158 Uiso 0.25 1 d G U P . .


_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 C7 1.444(4) . ?
O1 H2A 0.84(6) . ?
O2 C20 1.441(4) . ?
O2 H1A 0.84(5) . ?
N1 C1 1.407(4) . ?
N1 H1 0.85(4) . ?
N1 H2 0.89(5) . ?
C1 C6 1.409(5) . ?
C1 C2 1.417(5) . ?
C2 C3 1.389(5) . ?
C2 C7 1.536(5) . ?
C3 C4 1.373(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.391(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.388(5) . ?
C5 H5 0.9500 . ?
C6 C20 1.533(5) . ?
C7 C8 1.529(5) . ?
C7 C14 1.532(5) . ?
C8 C9 1.381(5) . ?
C8 C13 1.400(5) . ?
C9 C10 1.388(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.379(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.367(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.370(6) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C19 1.384(5) . ?
C14 C15 1.388(5) . ?
C15 C16 1.387(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.382(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.381(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.378(5) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C27 1.530(5) . ?
C20 C21 1.537(5) . ?
C21 C22 1.379(5) . ?
C21 C26 1.392(5) . ?
C22 C23 1.392(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.373(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.384(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.375(5) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.379(5) . ?
C27 C32 1.381(5) . ?
C28 C29 1.388(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.377(6) . ?
C29 H29 0.9500 . ?
C30 C31 1.373(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.383(5) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C34 1.384(8) . ?
C33 C35 1.399(9) 3_756 ?
C33 H33 0.9500 . ?
C34 C35 1.343(9) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
O3 H3A 0.8332 . ?
O3 H3B 0.8883 . ?

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
C7 O1 H2A 106(4) . . ?
C20 O2 H1A 111(3) . . ?
C1 N1 H1 108(3) . . ?
C1 N1 H2 110(3) . . ?
H1 N1 H2 119(4) . . ?
N1 C1 C6 121.5(3) . . ?
N1 C1 C2 118.4(3) . . ?
C6 C1 C2 120.0(3) . . ?
C3 C2 C1 119.1(3) . . ?
C3 C2 C7 121.0(3) . . ?
C1 C2 C7 119.7(3) . . ?
C4 C3 C2 121.2(3) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 119.5(3) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C6 C5 C4 121.7(3) . . ?
C6 C5 H5 119.1 . . ?
C4 C5 H5 119.1 . . ?
C5 C6 C1 118.4(3) . . ?
C5 C6 C20 121.1(3) . . ?
C1 C6 C20 120.5(3) . . ?
O1 C7 C8 109.2(3) . . ?
O1 C7 C14 106.2(3) . . ?
C8 C7 C14 109.1(3) . . ?
O1 C7 C2 107.4(3) . . ?
C8 C7 C2 113.1(3) . . ?
C14 C7 C2 111.6(3) . . ?
C9 C8 C13 118.4(4) . . ?
C9 C8 C7 122.0(3) . . ?
C13 C8 C7 119.4(3) . . ?
C8 C9 C10 120.4(4) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C11 C10 C9 120.3(4) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C12 C11 C10 119.6(4) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C11 C12 C13 120.8(4) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C12 C13 C8 120.6(4) . . ?
C12 C13 H13 119.7 . . ?
C8 C13 H13 119.7 . . ?
C19 C14 C15 118.4(3) . . ?
C19 C14 C7 120.6(3) . . ?
C15 C14 C7 120.9(3) . . ?
C16 C15 C14 120.5(4) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C17 C16 C15 120.7(4) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C16 C17 C18 118.6(4) . . ?
C16 C17 H17 120.7 . . ?
C18 C17 H17 120.7 . . ?
C19 C18 C17 121.0(4) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C18 C19 C14 120.8(3) . . ?
C18 C19 H19 119.6 . . ?
C14 C19 H19 119.6 . . ?
O2 C20 C27 105.7(3) . . ?
O2 C20 C6 109.1(3) . . ?
C27 C20 C6 111.8(3) . . ?
O2 C20 C21 109.1(3) . . ?
C27 C20 C21 110.5(3) . . ?
C6 C20 C21 110.6(3) . . ?
C22 C21 C26 117.9(3) . . ?
C22 C21 C20 122.0(3) . . ?
C26 C21 C20 120.1(3) . . ?
C21 C22 C23 121.1(4) . . ?
C21 C22 H22 119.4 . . ?
C23 C22 H22 119.4 . . ?
C24 C23 C22 119.8(4) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C23 C24 C25 120.0(4) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C26 C25 C24 119.7(4) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C25 C26 C21 121.4(4) . . ?
C25 C26 H26 119.3 . . ?
C21 C26 H26 119.3 . . ?
C28 C27 C32 118.6(3) . . ?
C28 C27 C20 120.1(3) . . ?
C32 C27 C20 121.3(3) . . ?
C27 C28 C29 120.7(4) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 H28 119.7 . . ?
C30 C29 C28 120.2(4) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C31 C30 C29 119.4(4) . . ?
C31 C30 H30 120.3 . . ?
C29 C30 H30 120.3 . . ?
C30 C31 C32 120.3(4) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
C27 C32 C31 120.8(4) . . ?
C27 C32 H32 119.6 . . ?
C31 C32 H32 119.6 . . ?
C34 C33 C35 120.1(6) . 3_756 ?
C34 C33 H33 120.0 . . ?
C35 C33 H33 120.0 3_756 . ?
C35 C34 C33 119.5(7) . . ?
C35 C34 H34 120.3 . . ?
C33 C34 H34 120.3 . . ?
C34 C35 C33 120.5(5) . 3_756 ?
C34 C35 H35 119.8 . . ?
C33 C35 H35 119.8 3_756 . ?
H3A O3 H3B 111.2 . . ?

_refine_diff_density_max         0.259
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.065

####################################################################### 
# 
# 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_jvr190108N1
_database_code_depnum_ccdc_archive 'CCDC 1956672'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2019-09-30 deposited with the CCDC.	2020-01-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H49 Cl2 N O2'
_chemical_formula_weight         682.73

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_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'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   8.0461(4)
_cell_length_b                   25.3743(11)
_cell_length_c                   9.3223(5)
_cell_angle_alpha                90
_cell_angle_beta                 98.680(2)
_cell_angle_gamma                90
_cell_volume                     1881.48(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9903
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      28.20

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_F_000             728
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          1.514
_exptl_crystal_size_mid          0.808
_exptl_crystal_size_min          0.548
_exptl_absorpt_coefficient_mu    0.209
_shelx_estimated_absorpt_T_min   0.743
_shelx_estimated_absorpt_T_max   0.894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7561
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_absorpt_special_details   
;
The ratio of minimum to maximum
apparent transmission was 0.878
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            45673
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.351
_diffrn_reflns_theta_max         28.336
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             4789
_reflns_number_gt                3812
_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       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'APEX3 v2016.9-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0673P)²+1.4983P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4789
_refine_ls_number_parameters     257
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0653
_refine_ls_wR_factor_ref         0.1683
_refine_ls_wR_factor_gt          0.1573
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.084
_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
O1 O -0.11174(15) 0.35435(5) 1.56451(14) 0.0260(3) Uani 1 1 d . . . . .
N1 N -0.2020(3) 0.250000 1.6590(2) 0.0236(5) Uani 1 2 d S T P . .
H1 H -0.177(3) 0.2784(8) 1.704(2) 0.020(5) Uiso 1 1 d . . . . .
C1 C -0.2950(3) 0.250000 1.5231(2) 0.0181(4) Uani 1 2 d S T P . .
C2 C -0.3394(2) 0.29834(7) 1.45033(17) 0.0186(3) Uani 1 1 d . . . . .
C3 C -0.4093(2) 0.29697(7) 1.30444(18) 0.0225(4) Uani 1 1 d . . . . .
H3 H -0.435020 0.329205 1.254128 0.027 Uiso 1 1 calc R U . . .
C4 C -0.4422(3) 0.250000 1.2309(3) 0.0246(5) Uani 1 2 d S T P . .
H4 H -0.487120 0.250000 1.130629 0.030 Uiso 1 2 calc R U P . .
C5 C -0.2925(2) 0.35068(7) 1.52815(18) 0.0210(3) Uani 1 1 d . . . . .
C6 C -0.0192(2) 0.33957(8) 1.4527(2) 0.0322(4) Uani 1 1 d . . . . .
H6A H 0.098019 0.350824 1.478713 0.048 Uiso 1 1 calc R U . . .
H6B H -0.068227 0.356486 1.361600 0.048 Uiso 1 1 calc R U . . .
H6C H -0.023410 0.301203 1.440685 0.048 Uiso 1 1 calc R U . . .
C7 C -0.3608(2) 0.39991(7) 1.44174(18) 0.0219(4) Uani 1 1 d . . . . .
C8 C -0.5319(2) 0.40464(8) 1.3874(2) 0.0268(4) Uani 1 1 d . . . . .
H8 H -0.605772 0.376376 1.399940 0.032 Uiso 1 1 calc R U . . .
C9 C -0.5958(2) 0.44984(8) 1.3154(2) 0.0295(4) Uani 1 1 d . . . . .
C10 C -0.4875(3) 0.49135(7) 1.3002(2) 0.0296(4) Uani 1 1 d . . . . .
H10 H -0.530507 0.522502 1.251572 0.036 Uiso 1 1 calc R U . . .
C11 C -0.3180(3) 0.48821(7) 1.3544(2) 0.0282(4) Uani 1 1 d . . . . .
C12 C -0.2563(2) 0.44219(7) 1.42568(19) 0.0246(4) Uani 1 1 d . . . . .
H12 H -0.140174 0.439848 1.463892 0.030 Uiso 1 1 calc R U . . .
C13 C -0.7795(3) 0.45409(10) 1.2541(3) 0.0463(6) Uani 1 1 d . . . . .
H13A H -0.801459 0.488521 1.207481 0.070 Uiso 1 1 calc R U . . .
H13B H -0.809447 0.426123 1.182405 0.070 Uiso 1 1 calc R U . . .
H13C H -0.847021 0.450402 1.332670 0.070 Uiso 1 1 calc R U . . .
C14 C -0.2022(3) 0.53332(8) 1.3351(3) 0.0404(5) Uani 1 1 d . . . . .
H14A H -0.087582 0.524397 1.379931 0.061 Uiso 1 1 calc R U . . .
H14B H -0.203957 0.540006 1.231335 0.061 Uiso 1 1 calc R U . . .
H14C H -0.239644 0.564951 1.381388 0.061 Uiso 1 1 calc R U . . .
C15 C -0.3571(2) 0.35563(7) 1.67497(19) 0.0255(4) Uani 1 1 d . . . . .
C16 C -0.5138(3) 0.33607(8) 1.6936(2) 0.0320(4) Uani 1 1 d . . . . .
H16 H -0.577439 0.316288 1.617978 0.038 Uiso 1 1 calc R U . . .
C17 C -0.5791(3) 0.34512(10) 1.8224(2) 0.0459(6) Uani 1 1 d . . . . .
C18 C -0.4836(4) 0.37321(11) 1.9317(2) 0.0544(8) Uani 1 1 d . . . . .
H18 H -0.527412 0.379737 2.019080 0.065 Uiso 1 1 calc R U . . .
C19 C -0.3252(4) 0.39223(10) 1.9174(2) 0.0522(7) Uani 1 1 d . . . . .
C20 C -0.2632(3) 0.38369(8) 1.7871(2) 0.0374(5) Uani 1 1 d . . . . .
H20 H -0.156064 0.397167 1.775099 0.045 Uiso 1 1 calc R U . . .
C21 C -0.7512(4) 0.32556(13) 1.8394(3) 0.0676(9) Uani 1 1 d . . . . .
H21A H -0.744997 0.305835 1.930439 0.101 Uiso 1 1 calc R U . . .
H21B H -0.793457 0.302473 1.757765 0.101 Uiso 1 1 calc R U . . .
H21C H -0.827309 0.355621 1.841147 0.101 Uiso 1 1 calc R U . . .
C22 C -0.2226(6) 0.42321(14) 2.0372(3) 0.0840(12) Uani 1 1 d . . . . .
H22A H -0.267965 0.459008 2.039075 0.126 Uiso 1 1 calc R U . . .
H22B H -0.105553 0.424833 2.020051 0.126 Uiso 1 1 calc R U . . .
H22C H -0.227711 0.405937 2.130476 0.126 Uiso 1 1 calc R U . . .
Cl2S Cl 0.1522(6) 0.26683(16) 1.1974(5) 0.0377(9) Uani 0.25 1 d D U P A -1
C1S C -0.0493(14) 0.2794(5) 1.0943(19) 0.041(3) Uani 0.25 1 d D U P A -1
H1SA H -0.132143 0.290864 1.156307 0.049 Uiso 0.25 1 calc R U P A -1
H1SB H -0.043545 0.305739 1.016858 0.049 Uiso 0.25 1 calc R U P A -1
Cl1S Cl -0.0934(9) 0.2154(4) 1.0230(11) 0.0602(14) Uani 0.25 1 d D U P A -1
C1S' C -0.0655(14) 0.2700(5) 1.1193(17) 0.041(3) Uani 0.25 1 d D U P B -2
H1SC H -0.129143 0.270648 1.202307 0.049 Uiso 0.25 1 calc R U P B -2
H1SD H -0.106455 0.300245 1.056645 0.049 Uiso 0.25 1 calc R U P B -2
Cl1' Cl 0.1456(8) 0.2840(2) 1.1910(7) 0.0602(14) Uani 0.25 1 d D U P B -2
Cl2' Cl -0.1291(6) 0.2129(3) 1.0197(7) 0.0388(9) Uani 0.25 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
O1 C6 1.420(2) . ?
O1 C5 1.446(2) . ?
N1 C1 1.370(3) . ?
N1 H1 0.84(2) . ?
N1 H1 0.84(2) 4_565 ?
C1 C2 1.421(2) 4_565 ?
C1 C2 1.421(2) . ?
C2 C3 1.392(2) . ?
C2 C5 1.533(2) . ?
C3 C4 1.381(2) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 C15 1.541(2) . ?
C5 C7 1.542(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C12 1.385(3) . ?
C7 C8 1.398(3) . ?
C8 C9 1.388(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.388(3) . ?
C9 C13 1.506(3) . ?
C10 C11 1.383(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.397(3) . ?
C11 C14 1.504(3) . ?
C12 H12 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C20 1.390(3) . ?
C15 C16 1.390(3) . ?
C16 C17 1.400(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.378(4) . ?
C17 C21 1.502(4) . ?
C18 C19 1.388(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.397(3) . ?
C19 C22 1.506(4) . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
Cl2S C1S 1.784(9) . ?
C1S Cl1S 1.769(8) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
C1S' Cl2' 1.755(8) . ?
C1S' Cl1' 1.765(8) . ?
C1S' H1SC 0.9900 . ?
C1S' H1SD 0.9900 . ?

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
C6 O1 C5 115.57(14) . . ?
C1 N1 H1 120.9(14) . . ?
C1 N1 H1 120.9(14) . 4_565 ?
H1 N1 H1 118(3) . 4_565 ?
N1 C1 C2 120.28(10) . 4_565 ?
N1 C1 C2 120.28(10) . . ?
C2 C1 C2 119.3(2) 4_565 . ?
C3 C2 C1 118.72(16) . . ?
C3 C2 C5 121.23(15) . . ?
C1 C2 C5 119.72(14) . . ?
C4 C3 C2 121.72(17) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C3 119.4(2) . 4_565 ?
C3 C4 H4 120.3 . . ?
C3 C4 H4 120.3 4_565 . ?
O1 C5 C2 109.49(13) . . ?
O1 C5 C15 104.41(14) . . ?
C2 C5 C15 113.52(14) . . ?
O1 C5 C7 109.70(14) . . ?
C2 C5 C7 114.32(14) . . ?
C15 C5 C7 104.87(13) . . ?
O1 C6 H6A 109.5 . . ?
O1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
O1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C12 C7 C8 118.35(16) . . ?
C12 C7 C5 120.63(15) . . ?
C8 C7 C5 120.84(16) . . ?
C9 C8 C7 121.24(18) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C8 C9 C10 118.97(18) . . ?
C8 C9 C13 120.88(19) . . ?
C10 C9 C13 120.16(18) . . ?
C11 C10 C9 121.21(17) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C10 C11 C12 118.85(18) . . ?
C10 C11 C14 120.44(18) . . ?
C12 C11 C14 120.71(18) . . ?
C7 C12 C11 121.35(17) . . ?
C7 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C20 C15 C16 119.27(19) . . ?
C20 C15 C5 119.47(18) . . ?
C16 C15 C5 121.06(16) . . ?
C15 C16 C17 120.9(2) . . ?
C15 C16 H16 119.6 . . ?
C17 C16 H16 119.6 . . ?
C18 C17 C16 118.6(2) . . ?
C18 C17 C21 120.9(2) . . ?
C16 C17 C21 120.5(3) . . ?
C17 C18 C19 121.8(2) . . ?
C17 C18 H18 119.1 . . ?
C19 C18 H18 119.1 . . ?
C18 C19 C20 118.8(2) . . ?
C18 C19 C22 121.2(3) . . ?
C20 C19 C22 119.9(3) . . ?
C15 C20 C19 120.6(2) . . ?
C15 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C17 C21 H21A 109.5 . . ?
C17 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C17 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Cl1S C1S Cl2S 98.8(6) . . ?
Cl1S C1S H1SA 112.0 . . ?
Cl2S C1S H1SA 112.0 . . ?
Cl1S C1S H1SB 112.0 . . ?
Cl2S C1S H1SB 112.0 . . ?
H1SA C1S H1SB 109.7 . . ?
Cl2' C1S' Cl1' 123.6(8) . . ?
Cl2' C1S' H1SC 106.4 . . ?
Cl1' C1S' H1SC 106.4 . . ?
Cl2' C1S' H1SD 106.4 . . ?
Cl1' C1S' H1SD 106.4 . . ?
H1SC C1S' H1SD 106.5 . . ?

_refine_diff_density_max         0.387
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.054

####################################################################### 
# 
# 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_jvr181203N1
_database_code_depnum_ccdc_archive 'CCDC 1956671'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2019-09-30 deposited with the CCDC.	2020-01-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H31 N'
_chemical_formula_weight         453.60

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'

_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                   10.6940(10)
_cell_length_b                   14.5078(15)
_cell_length_c                   16.6117(17)
_cell_angle_alpha                96.571(5)
_cell_angle_beta                 104.496(5)
_cell_angle_gamma                90.146(5)
_cell_volume                     2477.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9931
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      26.44

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_F_000             968
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.318
_exptl_crystal_size_min          0.187
_exptl_absorpt_coefficient_mu    0.069
_shelx_estimated_absorpt_T_min   0.978
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6188
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_absorpt_special_details   
;
The ratio of minimum to maximum
apparent transmission was 0.830
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            44031
_diffrn_reflns_av_unetI/netI     0.0809
_diffrn_reflns_av_R_equivalents  0.1070
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.386
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             9480
_reflns_number_gt                6874
_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       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'APEX3 v2016.9-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_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)+(0.1781P)²+2.8149P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9480
_refine_ls_number_parameters     652
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1328
_refine_ls_R_factor_gt           0.0985
_refine_ls_wR_factor_ref         0.2837
_refine_ls_wR_factor_gt          0.2561
_refine_ls_goodness_of_fit_ref   1.032
_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
N1A N 0.2522(4) 0.4711(3) 0.6569(2) 0.0231(8) Uani 1 1 d . . . . .
H1A H 0.319(5) 0.463(3) 0.636(3) 0.020(11) Uiso 1 1 d . . . . .
H2A H 0.197(5) 0.514(4) 0.624(3) 0.035(14) Uiso 1 1 d . . . . .
C1A C 0.2863(4) 0.5038(3) 0.7431(2) 0.0160(8) Uani 1 1 d . . . . .
C2A C 0.4015(4) 0.4746(3) 0.7961(2) 0.0182(8) Uani 1 1 d . . . . .
C3A C 0.4308(4) 0.5077(3) 0.8812(2) 0.0183(8) Uani 1 1 d . . . . .
H3A H 0.508879 0.489918 0.916775 0.022 Uiso 1 1 calc R U . . .
C4A C 0.3507(4) 0.5650(3) 0.9151(2) 0.0194(8) Uani 1 1 d . . . . .
H4A H 0.372772 0.586170 0.973286 0.023 Uiso 1 1 calc R U . . .
C5A C 0.2369(4) 0.5916(3) 0.8632(2) 0.0171(8) Uani 1 1 d . . . . .
H5A H 0.180923 0.630681 0.886857 0.020 Uiso 1 1 calc R U . . .
C6A C 0.2024(4) 0.5627(3) 0.7775(2) 0.0171(8) Uani 1 1 d . . . . .
C7A C 0.0723(4) 0.5908(3) 0.7235(2) 0.0171(8) Uani 1 1 d . . . . .
C8A C -0.0134(4) 0.5007(3) 0.6950(3) 0.0261(9) Uani 1 1 d . . . . .
H8AA H -0.101727 0.516471 0.667771 0.039 Uiso 1 1 calc R U . . .
H8AB H -0.014200 0.468950 0.743903 0.039 Uiso 1 1 calc R U . . .
H8AC H 0.021602 0.459739 0.655438 0.039 Uiso 1 1 calc R U . . .
C9A C 0.0890(4) 0.6367(3) 0.6474(2) 0.0194(8) Uani 1 1 d . . . . .
C10A C 0.2012(4) 0.6882(3) 0.6514(3) 0.0245(9) Uani 1 1 d . . . . .
H10A H 0.269380 0.693027 0.700988 0.029 Uiso 1 1 calc R U . . .
C11A C 0.2150(5) 0.7324(3) 0.5844(3) 0.0305(10) Uani 1 1 d . . . . .
H11A H 0.292279 0.767005 0.588466 0.037 Uiso 1 1 calc R U . . .
C12A C 0.1165(5) 0.7262(3) 0.5115(3) 0.0337(11) Uani 1 1 d . . . . .
H12A H 0.125751 0.756749 0.465585 0.040 Uiso 1 1 calc R U . . .
C13A C 0.0055(5) 0.6756(3) 0.5062(3) 0.0328(10) Uani 1 1 d . . . . .
H13A H -0.062200 0.671160 0.456339 0.039 Uiso 1 1 calc R U . . .
C14A C -0.0090(4) 0.6304(3) 0.5734(3) 0.0256(9) Uani 1 1 d . . . . .
H14A H -0.086046 0.595240 0.568686 0.031 Uiso 1 1 calc R U . . .
C15A C 0.0062(4) 0.6616(3) 0.7748(2) 0.0187(8) Uani 1 1 d . . . . .
C16A C 0.0495(4) 0.7543(3) 0.7939(3) 0.0250(9) Uani 1 1 d . . . . .
H16A H 0.116629 0.774846 0.771445 0.030 Uiso 1 1 calc R U . . .
C17A C -0.0026(5) 0.8170(3) 0.8445(3) 0.0309(10) Uani 1 1 d . . . . .
H17A H 0.029904 0.879337 0.857204 0.037 Uiso 1 1 calc R U . . .
C18A C -0.1026(5) 0.7889(4) 0.8769(3) 0.0362(11) Uani 1 1 d . . . . .
H18A H -0.139159 0.831603 0.911689 0.043 Uiso 1 1 calc R U . . .
C19A C -0.1472(5) 0.6987(4) 0.8575(3) 0.0387(12) Uani 1 1 d . . . . .
H19A H -0.215429 0.678688 0.879363 0.046 Uiso 1 1 calc R U . . .
C20A C -0.0949(5) 0.6359(3) 0.8068(3) 0.0337(11) Uani 1 1 d . . . . .
H20A H -0.129052 0.573949 0.793580 0.040 Uiso 1 1 calc R U . . .
C21A C 0.4890(4) 0.4043(3) 0.7611(2) 0.0189(8) Uani 1 1 d . . . . .
C22A C 0.4085(4) 0.3132(3) 0.7285(3) 0.0308(10) Uani 1 1 d . . . . .
H22A H 0.462508 0.265849 0.708650 0.046 Uiso 1 1 calc R U . . .
H22B H 0.334813 0.324075 0.682321 0.046 Uiso 1 1 calc R U . . .
H22C H 0.376908 0.291726 0.773946 0.046 Uiso 1 1 calc R U . . .
C23A C 0.5406(4) 0.4427(3) 0.6918(2) 0.0203(8) Uani 1 1 d . . . . .
C24A C 0.5915(4) 0.3828(4) 0.6368(3) 0.0330(11) Uani 1 1 d . . . . .
H24A H 0.591591 0.318042 0.640935 0.040 Uiso 1 1 calc R U . . .
C25A C 0.6419(5) 0.4169(5) 0.5762(3) 0.0486(16) Uani 1 1 d . . . . .
H25A H 0.675973 0.375452 0.539117 0.058 Uiso 1 1 calc R U . . .
C26A C 0.6424(5) 0.5111(5) 0.5699(3) 0.0480(15) Uani 1 1 d . . . . .
H26A H 0.675341 0.534281 0.527789 0.058 Uiso 1 1 calc R U . . .
C27A C 0.5954(5) 0.5710(4) 0.6243(3) 0.0405(12) Uani 1 1 d . . . . .
H27A H 0.597211 0.635815 0.620715 0.049 Uiso 1 1 calc R U . . .
C28A C 0.5451(4) 0.5369(3) 0.6849(3) 0.0287(10) Uani 1 1 d . . . . .
H28A H 0.513033 0.579059 0.722446 0.034 Uiso 1 1 calc R U . . .
C29A C 0.6112(4) 0.3856(3) 0.8296(2) 0.0207(8) Uani 1 1 d . . . . .
C30A C 0.6284(5) 0.3018(3) 0.8646(3) 0.0288(10) Uani 1 1 d . . . . .
H30A H 0.561139 0.255396 0.848531 0.035 Uiso 1 1 calc R U . . .
C31A C 0.7417(5) 0.2856(4) 0.9219(3) 0.0371(12) Uani 1 1 d . . . . .
H31A H 0.751392 0.227937 0.944460 0.044 Uiso 1 1 calc R U . . .
C32A C 0.8407(5) 0.3516(4) 0.9470(3) 0.0397(13) Uani 1 1 d . . . . .
H32A H 0.918983 0.339287 0.985685 0.048 Uiso 1 1 calc R U . . .
C33A C 0.8247(4) 0.4360(4) 0.9152(3) 0.0347(11) Uani 1 1 d . . . . .
H33A H 0.891575 0.482678 0.932992 0.042 Uiso 1 1 calc R U . . .
C34A C 0.7108(4) 0.4528(3) 0.8571(3) 0.0271(9) Uani 1 1 d . . . . .
H34A H 0.700791 0.511160 0.835856 0.033 Uiso 1 1 calc R U . . .
N1B N 0.7510(4) 0.0770(3) 0.6697(2) 0.0262(8) Uani 1 1 d . . . . .
H1B H 0.824(6) 0.089(4) 0.655(4) 0.044(16) Uiso 1 1 d . . . . .
H2B H 0.700(6) 0.030(4) 0.640(4) 0.046(16) Uiso 1 1 d . . . . .
C1B C 0.7854(4) 0.0670(3) 0.7558(2) 0.0198(8) Uani 1 1 d . . . . .
C2B C 0.9019(4) 0.1100(3) 0.8077(2) 0.0179(8) Uani 1 1 d . . . . .
C3B C 0.9327(4) 0.0999(3) 0.8924(2) 0.0202(8) Uani 1 1 d . . . . .
H3B H 1.010187 0.128642 0.927633 0.024 Uiso 1 1 calc R U . . .
C4B C 0.8537(4) 0.0490(3) 0.9275(3) 0.0236(9) Uani 1 1 d . . . . .
H4B H 0.877224 0.042395 0.985549 0.028 Uiso 1 1 calc R U . . .
C5B C 0.7392(4) 0.0079(3) 0.8755(3) 0.0209(8) Uani 1 1 d . . . . .
H5B H 0.684585 -0.026591 0.899044 0.025 Uiso 1 1 calc R U . . .
C6B C 0.7027(4) 0.0159(3) 0.7903(2) 0.0185(8) Uani 1 1 d . . . . .
C7B C 0.5718(4) -0.0273(3) 0.7359(3) 0.0199(8) Uani 1 1 d . . . . .
C8B C 0.4846(4) 0.0545(3) 0.7069(3) 0.0303(10) Uani 1 1 d . . . . .
H8BA H 0.395678 0.030973 0.682039 0.045 Uiso 1 1 calc R U . . .
H8BB H 0.516757 0.083502 0.665182 0.045 Uiso 1 1 calc R U . . .
H8BC H 0.486364 0.100588 0.755181 0.045 Uiso 1 1 calc R U . . .
C9B C 0.5052(4) -0.0845(3) 0.7869(3) 0.0212(8) Uani 1 1 d . . . . .
C10B C 0.4286(5) -0.0421(4) 0.8360(4) 0.0422(13) Uani 1 1 d . . . . .
H10B H 0.414452 0.022526 0.835743 0.051 Uiso 1 1 calc R U . . .
C11B C 0.3720(5) -0.0916(4) 0.8854(4) 0.0464(14) Uani 1 1 d . . . . .
H11B H 0.320386 -0.060602 0.918362 0.056 Uiso 1 1 calc R U . . .
C12B C 0.3904(4) -0.1846(3) 0.8867(3) 0.0331(11) Uani 1 1 d . . . . .
H12B H 0.351525 -0.218803 0.920041 0.040 Uiso 1 1 calc R U . . .
C13B C 0.4652(5) -0.2273(3) 0.8394(3) 0.0309(10) Uani 1 1 d . . . . .
H13B H 0.478087 -0.292032 0.839999 0.037 Uiso 1 1 calc R U . . .
C14B C 0.5233(4) -0.1790(3) 0.7904(3) 0.0265(9) Uani 1 1 d . . . . .
H14B H 0.576153 -0.210859 0.758831 0.032 Uiso 1 1 calc R U . . .
C15B C 0.5920(4) -0.0919(3) 0.6596(3) 0.0219(9) Uani 1 1 d . . . . .
C16B C 0.4982(4) -0.1027(3) 0.5835(3) 0.0299(10) Uani 1 1 d . . . . .
H16B H 0.420598 -0.069595 0.578275 0.036 Uiso 1 1 calc R U . . .
C17B C 0.5163(5) -0.1608(4) 0.5155(3) 0.0400(12) Uani 1 1 d . . . . .
H17B H 0.451576 -0.166936 0.464065 0.048 Uiso 1 1 calc R U . . .
C18B C 0.6279(6) -0.2099(4) 0.5222(3) 0.0417(13) Uani 1 1 d . . . . .
H18B H 0.640431 -0.249931 0.475629 0.050 Uiso 1 1 calc R U . . .
C19B C 0.7218(5) -0.2003(3) 0.5974(3) 0.0347(11) Uani 1 1 d . . . . .
H19B H 0.799206 -0.233622 0.602183 0.042 Uiso 1 1 calc R U . . .
C20B C 0.7037(4) -0.1427(3) 0.6656(3) 0.0258(9) Uani 1 1 d . . . . .
H20B H 0.768190 -0.137707 0.717123 0.031 Uiso 1 1 calc R U . . .
C21B C 0.9917(4) 0.1684(3) 0.7715(2) 0.0192(8) Uani 1 1 d . . . . .
C22B C 0.9143(4) 0.2507(3) 0.7346(3) 0.0264(9) Uani 1 1 d . . . . .
H22D H 0.971420 0.291419 0.715536 0.040 Uiso 1 1 calc R U . . .
H22E H 0.879802 0.285849 0.777771 0.040 Uiso 1 1 calc R U . . .
H22F H 0.842797 0.226787 0.687166 0.040 Uiso 1 1 calc R U . . .
C23B C 1.0419(4) 0.1085(3) 0.7035(3) 0.0219(8) Uani 1 1 d . . . . .
C24B C 1.0407(4) 0.0120(3) 0.6977(3) 0.0281(10) Uani 1 1 d . . . . .
H24B H 1.007311 -0.018358 0.735943 0.034 Uiso 1 1 calc R U . . .
C25B C 1.0874(5) -0.0405(4) 0.6371(3) 0.0389(12) Uani 1 1 d . . . . .
H25B H 1.085836 -0.106290 0.634436 0.047 Uiso 1 1 calc R U . . .
C26B C 1.1358(5) 0.0016(4) 0.5812(3) 0.0381(12) Uani 1 1 d . . . . .
H26B H 1.165291 -0.034532 0.538616 0.046 Uiso 1 1 calc R U . . .
C27B C 1.1412(5) 0.0970(4) 0.5875(3) 0.0406(13) Uani 1 1 d . . . . .
H27B H 1.177350 0.126650 0.550093 0.049 Uiso 1 1 calc R U . . .
C28B C 1.0947(4) 0.1502(3) 0.6475(3) 0.0295(10) Uani 1 1 d . . . . .
H28B H 1.098794 0.215980 0.650499 0.035 Uiso 1 1 calc R U . . .
C29B C 1.1117(4) 0.2072(3) 0.8395(3) 0.0202(8) Uani 1 1 d . . . . .
C30B C 1.2114(4) 0.1490(3) 0.8700(3) 0.0279(10) Uani 1 1 d . . . . .
H30B H 1.204453 0.085181 0.848330 0.033 Uiso 1 1 calc R U . . .
C31B C 1.3212(4) 0.1822(4) 0.9316(3) 0.0373(11) Uani 1 1 d . . . . .
H31B H 1.387297 0.140852 0.951929 0.045 Uiso 1 1 calc R U . . .
C32B C 1.3343(5) 0.2748(4) 0.9631(3) 0.0367(12) Uani 1 1 d . . . . .
H32B H 1.409422 0.297642 1.004771 0.044 Uiso 1 1 calc R U . . .
C33B C 1.2373(5) 0.3336(3) 0.9334(3) 0.0332(11) Uani 1 1 d . . . . .
H33B H 1.246075 0.397719 0.954221 0.040 Uiso 1 1 calc R U . . .
C34B C 1.1264(4) 0.2999(3) 0.8730(3) 0.0277(10) Uani 1 1 d . . . . .
H34B H 1.059395 0.341240 0.854355 0.033 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
N1A C1A 1.412(5) . ?
N1A H1A 0.87(5) . ?
N1A H2A 0.98(6) . ?
C1A C6A 1.417(5) . ?
C1A C2A 1.420(6) . ?
C2A C3A 1.396(5) . ?
C2A C21A 1.547(5) . ?
C3A C4A 1.371(5) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.388(6) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.393(5) . ?
C5A H5A 0.9500 . ?
C6A C7A 1.539(5) . ?
C7A C9A 1.542(5) . ?
C7A C15A 1.545(5) . ?
C7A C8A 1.552(5) . ?
C8A H8AA 0.9800 . ?
C8A H8AB 0.9800 . ?
C8A H8AC 0.9800 . ?
C9A C10A 1.395(6) . ?
C9A C14A 1.395(6) . ?
C10A C11A 1.383(6) . ?
C10A H10A 0.9500 . ?
C11A C12A 1.386(7) . ?
C11A H11A 0.9500 . ?
C12A C13A 1.373(7) . ?
C12A H12A 0.9500 . ?
C13A C14A 1.397(6) . ?
C13A H13A 0.9500 . ?
C14A H14A 0.9500 . ?
C15A C20A 1.386(6) . ?
C15A C16A 1.397(6) . ?
C16A C17A 1.380(6) . ?
C16A H16A 0.9500 . ?
C17A C18A 1.391(7) . ?
C17A H17A 0.9500 . ?
C18A C19A 1.367(8) . ?
C18A H18A 0.9500 . ?
C19A C20A 1.385(7) . ?
C19A H19A 0.9500 . ?
C20A H20A 0.9500 . ?
C21A C22A 1.542(6) . ?
C21A C29A 1.551(6) . ?
C21A C23A 1.551(6) . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C23A C28A 1.385(6) . ?
C23A C24A 1.398(6) . ?
C24A C25A 1.390(7) . ?
C24A H24A 0.9500 . ?
C25A C26A 1.383(9) . ?
C25A H25A 0.9500 . ?
C26A C27A 1.369(8) . ?
C26A H26A 0.9500 . ?
C27A C28A 1.389(6) . ?
C27A H27A 0.9500 . ?
C28A H28A 0.9500 . ?
C29A C34A 1.394(6) . ?
C29A C30A 1.399(6) . ?
C30A C31A 1.381(7) . ?
C30A H30A 0.9500 . ?
C31A C32A 1.377(8) . ?
C31A H31A 0.9500 . ?
C32A C33A 1.384(8) . ?
C32A H32A 0.9500 . ?
C33A C34A 1.394(6) . ?
C33A H33A 0.9500 . ?
C34A H34A 0.9500 . ?
N1B C1B 1.411(5) . ?
N1B H1B 0.90(6) . ?
N1B H2B 0.89(6) . ?
C1B C6B 1.417(5) . ?
C1B C2B 1.421(6) . ?
C2B C3B 1.388(6) . ?
C2B C21B 1.551(5) . ?
C3B C4B 1.393(6) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.397(6) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.389(6) . ?
C5B H5B 0.9500 . ?
C6B C7B 1.549(5) . ?
C7B C9B 1.542(6) . ?
C7B C15B 1.548(6) . ?
C7B C8B 1.557(6) . ?
C8B H8BA 0.9800 . ?
C8B H8BB 0.9800 . ?
C8B H8BC 0.9800 . ?
C9B C10B 1.391(6) . ?
C9B C14B 1.392(6) . ?
C10B C11B 1.392(7) . ?
C10B H10B 0.9500 . ?
C11B C12B 1.366(7) . ?
C11B H11B 0.9500 . ?
C12B C13B 1.359(7) . ?
C12B H12B 0.9500 . ?
C13B C14B 1.386(6) . ?
C13B H13B 0.9500 . ?
C14B H14B 0.9500 . ?
C15B C20B 1.394(6) . ?
C15B C16B 1.396(6) . ?
C16B C17B 1.385(7) . ?
C16B H16B 0.9500 . ?
C17B C18B 1.379(8) . ?
C17B H17B 0.9500 . ?
C18B C19B 1.386(8) . ?
C18B H18B 0.9500 . ?
C19B C20B 1.383(6) . ?
C19B H19B 0.9500 . ?
C20B H20B 0.9500 . ?
C21B C29B 1.537(6) . ?
C21B C23B 1.550(6) . ?
C21B C22B 1.550(6) . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 0.9800 . ?
C23B C24B 1.392(6) . ?
C23B C28B 1.393(6) . ?
C24B C25B 1.386(6) . ?
C24B H24B 0.9500 . ?
C25B C26B 1.369(8) . ?
C25B H25B 0.9500 . ?
C26B C27B 1.375(8) . ?
C26B H26B 0.9500 . ?
C27B C28B 1.382(7) . ?
C27B H27B 0.9500 . ?
C28B H28B 0.9500 . ?
C29B C34B 1.388(6) . ?
C29B C30B 1.393(6) . ?
C30B C31B 1.392(6) . ?
C30B H30B 0.9500 . ?
C31B C32B 1.378(7) . ?
C31B H31B 0.9500 . ?
C32B C33B 1.376(7) . ?
C32B H32B 0.9500 . ?
C33B C34B 1.394(6) . ?
C33B H33B 0.9500 . ?
C34B H34B 0.9500 . ?

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
C1A N1A H1A 113(3) . . ?
C1A N1A H2A 112(3) . . ?
H1A N1A H2A 107(4) . . ?
N1A C1A C6A 119.8(3) . . ?
N1A C1A C2A 120.2(3) . . ?
C6A C1A C2A 120.0(3) . . ?
C3A C2A C1A 118.3(3) . . ?
C3A C2A C21A 120.8(4) . . ?
C1A C2A C21A 120.8(3) . . ?
C4A C3A C2A 122.2(4) . . ?
C4A C3A H3A 118.9 . . ?
C2A C3A H3A 118.9 . . ?
C3A C4A C5A 119.1(4) . . ?
C3A C4A H4A 120.5 . . ?
C5A C4A H4A 120.5 . . ?
C4A C5A C6A 121.9(4) . . ?
C4A C5A H5A 119.1 . . ?
C6A C5A H5A 119.1 . . ?
C5A C6A C1A 118.5(4) . . ?
C5A C6A C7A 119.7(3) . . ?
C1A C6A C7A 121.7(3) . . ?
C6A C7A C9A 112.0(3) . . ?
C6A C7A C15A 110.9(3) . . ?
C9A C7A C15A 107.0(3) . . ?
C6A C7A C8A 106.5(3) . . ?
C9A C7A C8A 111.0(3) . . ?
C15A C7A C8A 109.5(3) . . ?
C7A C8A H8AA 109.5 . . ?
C7A C8A H8AB 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
C7A C8A H8AC 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
C10A C9A C14A 117.9(4) . . ?
C10A C9A C7A 120.9(4) . . ?
C14A C9A C7A 121.1(4) . . ?
C11A C10A C9A 121.3(4) . . ?
C11A C10A H10A 119.4 . . ?
C9A C10A H10A 119.4 . . ?
C10A C11A C12A 120.2(4) . . ?
C10A C11A H11A 119.9 . . ?
C12A C11A H11A 119.9 . . ?
C13A C12A C11A 119.4(4) . . ?
C13A C12A H12A 120.3 . . ?
C11A C12A H12A 120.3 . . ?
C12A C13A C14A 120.7(4) . . ?
C12A C13A H13A 119.6 . . ?
C14A C13A H13A 119.6 . . ?
C9A C14A C13A 120.4(4) . . ?
C9A C14A H14A 119.8 . . ?
C13A C14A H14A 119.8 . . ?
C20A C15A C16A 116.8(4) . . ?
C20A C15A C7A 122.1(4) . . ?
C16A C15A C7A 121.1(3) . . ?
C17A C16A C15A 121.9(4) . . ?
C17A C16A H16A 119.1 . . ?
C15A C16A H16A 119.1 . . ?
C16A C17A C18A 120.1(4) . . ?
C16A C17A H17A 119.9 . . ?
C18A C17A H17A 119.9 . . ?
C19A C18A C17A 118.6(4) . . ?
C19A C18A H18A 120.7 . . ?
C17A C18A H18A 120.7 . . ?
C18A C19A C20A 121.2(4) . . ?
C18A C19A H19A 119.4 . . ?
C20A C19A H19A 119.4 . . ?
C19A C20A C15A 121.4(4) . . ?
C19A C20A H20A 119.3 . . ?
C15A C20A H20A 119.3 . . ?
C22A C21A C2A 107.3(3) . . ?
C22A C21A C29A 109.6(3) . . ?
C2A C21A C29A 111.5(3) . . ?
C22A C21A C23A 112.1(3) . . ?
C2A C21A C23A 111.2(3) . . ?
C29A C21A C23A 105.2(3) . . ?
C21A C22A H22A 109.5 . . ?
C21A C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
C21A C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C28A C23A C24A 117.7(4) . . ?
C28A C23A C21A 121.9(4) . . ?
C24A C23A C21A 120.3(4) . . ?
C25A C24A C23A 120.8(5) . . ?
C25A C24A H24A 119.6 . . ?
C23A C24A H24A 119.6 . . ?
C26A C25A C24A 120.0(5) . . ?
C26A C25A H25A 120.0 . . ?
C24A C25A H25A 120.0 . . ?
C27A C26A C25A 120.0(5) . . ?
C27A C26A H26A 120.0 . . ?
C25A C26A H26A 120.0 . . ?
C26A C27A C28A 120.0(5) . . ?
C26A C27A H27A 120.0 . . ?
C28A C27A H27A 120.0 . . ?
C23A C28A C27A 121.5(5) . . ?
C23A C28A H28A 119.2 . . ?
C27A C28A H28A 119.2 . . ?
C34A C29A C30A 117.4(4) . . ?
C34A C29A C21A 120.0(4) . . ?
C30A C29A C21A 122.6(4) . . ?
C31A C30A C29A 121.0(5) . . ?
C31A C30A H30A 119.5 . . ?
C29A C30A H30A 119.5 . . ?
C32A C31A C30A 121.0(5) . . ?
C32A C31A H31A 119.5 . . ?
C30A C31A H31A 119.5 . . ?
C31A C32A C33A 119.1(4) . . ?
C31A C32A H32A 120.5 . . ?
C33A C32A H32A 120.4 . . ?
C32A C33A C34A 120.2(5) . . ?
C32A C33A H33A 119.9 . . ?
C34A C33A H33A 119.9 . . ?
C29A C34A C33A 121.2(4) . . ?
C29A C34A H34A 119.4 . . ?
C33A C34A H34A 119.4 . . ?
C1B N1B H1B 108(4) . . ?
C1B N1B H2B 112(4) . . ?
H1B N1B H2B 117(5) . . ?
N1B C1B C6B 120.0(4) . . ?
N1B C1B C2B 119.5(4) . . ?
C6B C1B C2B 120.5(4) . . ?
C3B C2B C1B 118.4(4) . . ?
C3B C2B C21B 120.4(3) . . ?
C1B C2B C21B 121.2(3) . . ?
C2B C3B C4B 122.1(4) . . ?
C2B C3B H3B 118.9 . . ?
C4B C3B H3B 118.9 . . ?
C3B C4B C5B 118.6(4) . . ?
C3B C4B H4B 120.7 . . ?
C5B C4B H4B 120.7 . . ?
C6B C5B C4B 122.0(4) . . ?
C6B C5B H5B 119.0 . . ?
C4B C5B H5B 119.0 . . ?
C5B C6B C1B 118.4(4) . . ?
C5B C6B C7B 120.1(3) . . ?
C1B C6B C7B 121.5(3) . . ?
C9B C7B C15B 108.4(3) . . ?
C9B C7B C6B 111.0(3) . . ?
C15B C7B C6B 110.6(3) . . ?
C9B C7B C8B 108.9(3) . . ?
C15B C7B C8B 110.8(3) . . ?
C6B C7B C8B 107.1(3) . . ?
C7B C8B H8BA 109.5 . . ?
C7B C8B H8BB 109.5 . . ?
H8BA C8B H8BB 109.5 . . ?
C7B C8B H8BC 109.5 . . ?
H8BA C8B H8BC 109.5 . . ?
H8BB C8B H8BC 109.5 . . ?
C10B C9B C14B 116.5(4) . . ?
C10B C9B C7B 120.9(4) . . ?
C14B C9B C7B 122.5(4) . . ?
C9B C10B C11B 121.9(4) . . ?
C9B C10B H10B 119.1 . . ?
C11B C10B H10B 119.1 . . ?
C12B C11B C10B 120.3(4) . . ?
C12B C11B H11B 119.9 . . ?
C10B C11B H11B 119.9 . . ?
C13B C12B C11B 118.8(4) . . ?
C13B C12B H12B 120.6 . . ?
C11B C12B H12B 120.6 . . ?
C12B C13B C14B 121.8(4) . . ?
C12B C13B H13B 119.1 . . ?
C14B C13B H13B 119.1 . . ?
C13B C14B C9B 120.8(4) . . ?
C13B C14B H14B 119.6 . . ?
C9B C14B H14B 119.6 . . ?
C20B C15B C16B 118.0(4) . . ?
C20B C15B C7B 120.7(4) . . ?
C16B C15B C7B 121.3(4) . . ?
C17B C16B C15B 121.1(5) . . ?
C17B C16B H16B 119.4 . . ?
C15B C16B H16B 119.4 . . ?
C18B C17B C16B 120.2(5) . . ?
C18B C17B H17B 119.9 . . ?
C16B C17B H17B 119.9 . . ?
C17B C18B C19B 119.4(5) . . ?
C17B C18B H18B 120.3 . . ?
C19B C18B H18B 120.3 . . ?
C20B C19B C18B 120.5(5) . . ?
C20B C19B H19B 119.7 . . ?
C18B C19B H19B 119.7 . . ?
C19B C20B C15B 120.7(4) . . ?
C19B C20B H20B 119.6 . . ?
C15B C20B H20B 119.6 . . ?
C29B C21B C23B 106.5(3) . . ?
C29B C21B C22B 108.8(3) . . ?
C23B C21B C22B 110.7(3) . . ?
C29B C21B C2B 111.6(3) . . ?
C23B C21B C2B 111.0(3) . . ?
C22B C21B C2B 108.2(3) . . ?
C21B C22B H22D 109.5 . . ?
C21B C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
C21B C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
C24B C23B C28B 117.4(4) . . ?
C24B C23B C21B 121.9(4) . . ?
C28B C23B C21B 120.6(4) . . ?
C25B C24B C23B 121.2(4) . . ?
C25B C24B H24B 119.4 . . ?
C23B C24B H24B 119.4 . . ?
C26B C25B C24B 120.5(5) . . ?
C26B C25B H25B 119.7 . . ?
C24B C25B H25B 119.7 . . ?
C25B C26B C27B 119.1(4) . . ?
C25B C26B H26B 120.5 . . ?
C27B C26B H26B 120.5 . . ?
C26B C27B C28B 121.0(5) . . ?
C26B C27B H27B 119.5 . . ?
C28B C27B H27B 119.5 . . ?
C27B C28B C23B 120.7(5) . . ?
C27B C28B H28B 119.6 . . ?
C23B C28B H28B 119.6 . . ?
C34B C29B C30B 117.1(4) . . ?
C34B C29B C21B 122.6(4) . . ?
C30B C29B C21B 120.3(4) . . ?
C31B C30B C29B 121.5(4) . . ?
C31B C30B H30B 119.2 . . ?
C29B C30B H30B 119.2 . . ?
C32B C31B C30B 120.3(5) . . ?
C32B C31B H31B 119.9 . . ?
C30B C31B H31B 119.9 . . ?
C33B C32B C31B 119.2(4) . . ?
C33B C32B H32B 120.4 . . ?
C31B C32B H32B 120.4 . . ?
C32B C33B C34B 120.4(4) . . ?
C32B C33B H33B 119.8 . . ?
C34B C33B H33B 119.8 . . ?
C29B C34B C33B 121.4(4) . . ?
C29B C34B H34B 119.3 . . ?
C33B C34B H34B 119.3 . . ?

_refine_diff_density_max         0.474
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.088

####################################################################### 
# 
# 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_jvr190225N2
_database_code_depnum_ccdc_archive 'CCDC 1956675'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2019-09-30 deposited with the CCDC.	2020-01-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H59 N'
_chemical_formula_weight         746.04

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_H-M_alt        'A b a 2'
_space_group_name_Hall           'A 2 -2ac'

_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'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, z+1/2'

_cell_length_a                   15.828(6)
_cell_length_b                   16.995(6)
_cell_length_c                   16.819(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4524(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5285
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      27.32

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_F_000             1608
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.519
_exptl_crystal_size_mid          0.398
_exptl_crystal_size_min          0.295
_exptl_absorpt_coefficient_mu    0.062
_shelx_estimated_absorpt_T_min   0.969
_shelx_estimated_absorpt_T_max   0.982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8359
_exptl_absorpt_correction_T_max  0.9590
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_absorpt_special_details   
;
The ratio of minimum to maximum
apparent transmission was 0.872
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            19658
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.574
_diffrn_reflns_theta_max         27.530
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             5150
_reflns_number_gt                4089
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.921
_reflns_Friedel_fraction_max     0.981
_reflns_Friedel_fraction_full    0.987

_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       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'APEX3 v2016.9-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0561P)²+1.7478P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1538 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
  The Flack parameter was deleted because the 
 value (-4.0(10)) does not match the valid range
;
_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5150
_refine_ls_number_parameters     269
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0544
_refine_ls_wR_factor_ref         0.1219
_refine_ls_wR_factor_gt          0.1118
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_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
N1 N 0.500000 0.500000 0.4502(2) 0.0215(7) Uani 1 2 d S T P . .
H1 H 0.523(2) 0.460(2) 0.425(2) 0.043(11) Uiso 1 1 d . . . . .
C1 C 0.500000 0.500000 0.5321(2) 0.0163(8) Uani 1 2 d S T P . .
C2 C 0.46471(16) 0.56478(16) 0.57463(16) 0.0167(6) Uani 1 1 d . . . . .
C3 C 0.46446(19) 0.56202(17) 0.65729(18) 0.0241(7) Uani 1 1 d . . . . .
H3 H 0.439213 0.603837 0.686278 0.029 Uiso 1 1 calc R U . . .
C4 C 0.500000 0.500000 0.6980(3) 0.0324(11) Uani 1 2 d S T P . .
H4 H 0.500000 0.500000 0.754522 0.039 Uiso 1 2 calc R U P . .
C5 C 0.42191(15) 0.63435(16) 0.53081(17) 0.0162(6) Uani 1 1 d . . . . .
C6 C 0.39087(16) 0.69835(16) 0.59071(16) 0.0174(6) Uani 1 1 d . . . . .
C8 C 0.28301(19) 0.7786(2) 0.6538(2) 0.0293(7) Uani 1 1 d . . . . .
C7 C 0.30687(18) 0.71802(18) 0.60204(18) 0.0223(6) Uani 1 1 d . . . . .
H7 H 0.264453 0.689800 0.574043 0.027 Uiso 1 1 calc R U . . .
C9 C 0.34463(19) 0.81990(19) 0.69433(19) 0.0269(7) Uani 1 1 d . . . . .
H9 H 0.328665 0.860496 0.730138 0.032 Uiso 1 1 calc R U . . .
C10 C 0.43015(19) 0.80272(17) 0.68323(18) 0.0252(7) Uani 1 1 d . . . . .
C11 C 0.45152(17) 0.74236(17) 0.63154(18) 0.0217(6) Uani 1 1 d . . . . .
H11 H 0.509553 0.730489 0.623576 0.026 Uiso 1 1 calc R U . . .
C12 C 0.1914(2) 0.7988(3) 0.6647(3) 0.0502(11) Uani 1 1 d . . . . .
H12A H 0.183370 0.855456 0.656899 0.075 Uiso 1 1 calc R U . . .
H12B H 0.173502 0.784302 0.718529 0.075 Uiso 1 1 calc R U . . .
H12C H 0.157398 0.769835 0.625735 0.075 Uiso 1 1 calc R U . . .
C13 C 0.4968(2) 0.8496(2) 0.7262(2) 0.0394(9) Uani 1 1 d . . . . .
H13A H 0.549474 0.819439 0.728043 0.059 Uiso 1 1 calc R U . . .
H13B H 0.477714 0.860689 0.780539 0.059 Uiso 1 1 calc R U . . .
H13C H 0.506440 0.899326 0.698083 0.059 Uiso 1 1 calc R U . . .
C14 C 0.34627(16) 0.59888(16) 0.48433(17) 0.0189(6) Uani 1 1 d . . . . .
C15 C 0.28746(18) 0.55359(19) 0.52644(19) 0.0252(7) Uani 1 1 d . . . . .
H15 H 0.295480 0.545388 0.581802 0.030 Uiso 1 1 calc R U . . .
C16 C 0.21803(18) 0.52053(19) 0.4895(2) 0.0294(7) Uani 1 1 d . . . . .
C17 C 0.20876(18) 0.52932(18) 0.4079(2) 0.0290(7) Uani 1 1 d . . . . .
H17 H 0.161425 0.506235 0.382172 0.035 Uiso 1 1 calc R U . . .
C18 C 0.26698(19) 0.57098(18) 0.36319(19) 0.0253(7) Uani 1 1 d . . . . .
C19 C 0.33518(16) 0.60643(17) 0.40293(18) 0.0198(6) Uani 1 1 d . . . . .
H19 H 0.374775 0.636398 0.373187 0.024 Uiso 1 1 calc R U . . .
C20 C 0.1526(2) 0.4757(3) 0.5380(3) 0.0484(10) Uani 1 1 d . . . . .
H20A H 0.145076 0.422937 0.515588 0.073 Uiso 1 1 calc R U . . .
H20B H 0.098613 0.503972 0.536493 0.073 Uiso 1 1 calc R U . . .
H20C H 0.171844 0.471349 0.593217 0.073 Uiso 1 1 calc R U . . .
C21 C 0.2587(2) 0.5782(2) 0.2740(2) 0.0405(9) Uani 1 1 d . . . . .
H21A H 0.312959 0.565594 0.248988 0.061 Uiso 1 1 calc R U . . .
H21B H 0.242470 0.632170 0.260285 0.061 Uiso 1 1 calc R U . . .
H21C H 0.215400 0.541592 0.254993 0.061 Uiso 1 1 calc R U . . .
C22 C 0.48421(17) 0.68006(16) 0.47686(17) 0.0182(6) Uani 1 1 d . . . . .
C23 C 0.45417(18) 0.74687(18) 0.43781(18) 0.0225(6) Uani 1 1 d . . . . .
H23 H 0.396040 0.760093 0.442196 0.027 Uiso 1 1 calc R U . . .
C24 C 0.5069(2) 0.79460(17) 0.3927(2) 0.0273(7) Uani 1 1 d . . . . .
C25 C 0.5920(2) 0.77450(19) 0.3868(2) 0.0308(8) Uani 1 1 d . . . . .
H25 H 0.628673 0.806498 0.355947 0.037 Uiso 1 1 calc R U . . .
C26 C 0.62401(18) 0.70897(19) 0.42487(19) 0.0261(7) Uani 1 1 d . . . . .
C27 C 0.56977(17) 0.66271(17) 0.47058(18) 0.0217(6) Uani 1 1 d . . . . .
H27 H 0.591793 0.618365 0.498030 0.026 Uiso 1 1 calc R U . . .
C28 C 0.4723(3) 0.8661(2) 0.3519(2) 0.0440(10) Uani 1 1 d . . . . .
H28A H 0.506327 0.912114 0.366349 0.066 Uiso 1 1 calc R U . . .
H28B H 0.413678 0.874474 0.368582 0.066 Uiso 1 1 calc R U . . .
H28C H 0.474344 0.858417 0.294210 0.066 Uiso 1 1 calc R U . . .
C29 C 0.71619(19) 0.6871(2) 0.4173(2) 0.0401(9) Uani 1 1 d . . . . .
H29A H 0.720987 0.634141 0.394724 0.060 Uiso 1 1 calc R U . . .
H29B H 0.742720 0.688143 0.469944 0.060 Uiso 1 1 calc R U . . .
H29C H 0.744647 0.724869 0.382345 0.060 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
N1 C1 1.377(5) . ?
N1 H1 0.88(4) . ?
N1 H1 0.88(4) 2_665 ?
C1 C2 1.427(3) . ?
C1 C2 1.427(3) 2_665 ?
C2 C3 1.391(4) . ?
C2 C5 1.549(4) . ?
C3 C4 1.377(4) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 C22 1.549(4) . ?
C5 C14 1.552(4) . ?
C5 C6 1.562(4) . ?
C6 C7 1.384(4) . ?
C6 C11 1.397(4) . ?
C8 C9 1.382(5) . ?
C8 C7 1.400(4) . ?
C8 C12 1.502(5) . ?
C7 H7 0.9500 . ?
C9 C10 1.397(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.387(4) . ?
C10 C13 1.507(4) . ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C19 1.386(4) . ?
C14 C15 1.400(4) . ?
C15 C16 1.382(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.388(5) . ?
C16 C20 1.524(5) . ?
C17 C18 1.384(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.405(4) . ?
C18 C21 1.510(5) . ?
C19 H19 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C27 1.390(4) . ?
C22 C23 1.395(4) . ?
C23 C24 1.390(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.392(5) . ?
C24 C28 1.498(5) . ?
C25 C26 1.381(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.395(4) . ?
C26 C29 1.511(4) . ?
C27 H27 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 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 N1 H1 119(2) . . ?
C1 N1 H1 119(2) . 2_665 ?
H1 N1 H1 123(5) . 2_665 ?
N1 C1 C2 120.10(17) . . ?
N1 C1 C2 120.10(17) . 2_665 ?
C2 C1 C2 119.8(3) . 2_665 ?
C3 C2 C1 118.4(3) . . ?
C3 C2 C5 120.0(3) . . ?
C1 C2 C5 121.4(2) . . ?
C4 C3 C2 121.5(3) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C3 120.3(4) 2_665 . ?
C3 C4 H4 119.8 2_665 . ?
C3 C4 H4 119.8 . . ?
C22 C5 C2 112.5(2) . . ?
C22 C5 C14 113.0(2) . . ?
C2 C5 C14 106.3(2) . . ?
C22 C5 C6 103.2(2) . . ?
C2 C5 C6 111.2(2) . . ?
C14 C5 C6 110.7(2) . . ?
C7 C6 C11 117.6(3) . . ?
C7 C6 C5 124.0(2) . . ?
C11 C6 C5 118.3(2) . . ?
C9 C8 C7 119.3(3) . . ?
C9 C8 C12 120.3(3) . . ?
C7 C8 C12 120.3(3) . . ?
C6 C7 C8 121.5(3) . . ?
C6 C7 H7 119.3 . . ?
C8 C7 H7 119.3 . . ?
C8 C9 C10 120.8(3) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 H9 119.6 . . ?
C11 C10 C9 118.3(3) . . ?
C11 C10 C13 121.5(3) . . ?
C9 C10 C13 120.2(3) . . ?
C10 C11 C6 122.5(3) . . ?
C10 C11 H11 118.8 . . ?
C6 C11 H11 118.8 . . ?
C8 C12 H12A 109.5 . . ?
C8 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C8 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C19 C14 C15 117.8(3) . . ?
C19 C14 C5 124.0(2) . . ?
C15 C14 C5 118.2(3) . . ?
C16 C15 C14 121.6(3) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C15 C16 C17 119.0(3) . . ?
C15 C16 C20 120.2(3) . . ?
C17 C16 C20 120.8(3) . . ?
C18 C17 C16 121.4(3) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
C17 C18 C19 118.2(3) . . ?
C17 C18 C21 121.6(3) . . ?
C19 C18 C21 120.2(3) . . ?
C14 C19 C18 121.8(3) . . ?
C14 C19 H19 119.1 . . ?
C18 C19 H19 119.1 . . ?
C16 C20 H20A 109.5 . . ?
C16 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C16 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C27 C22 C23 118.0(3) . . ?
C27 C22 C5 123.9(2) . . ?
C23 C22 C5 117.8(2) . . ?
C24 C23 C22 121.8(3) . . ?
C24 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
C23 C24 C25 118.5(3) . . ?
C23 C24 C28 120.2(3) . . ?
C25 C24 C28 121.3(3) . . ?
C26 C25 C24 121.3(3) . . ?
C26 C25 H25 119.3 . . ?
C24 C25 H25 119.3 . . ?
C25 C26 C27 118.9(3) . . ?
C25 C26 C29 120.9(3) . . ?
C27 C26 C29 120.1(3) . . ?
C22 C27 C26 121.5(3) . . ?
C22 C27 H27 119.3 . . ?
C26 C27 H27 119.3 . . ?
C24 C28 H28A 109.5 . . ?
C24 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C24 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?

_refine_diff_density_max         0.197
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.043

####################################################################### 
# 
# 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_jvr190924N1a
_database_code_depnum_ccdc_archive 'CCDC 1956677'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2019-09-30 deposited with the CCDC.	2020-01-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H47 N'
_chemical_formula_weight         565.80

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'

_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                   6.3152(2)
_cell_length_b                   10.7638(3)
_cell_length_c                   24.7246(8)
_cell_angle_alpha                85.9667(13)
_cell_angle_beta                 87.0612(15)
_cell_angle_gamma                88.1823(14)
_cell_volume                     1673.63(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9953
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      28.35

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_F_000             612
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.506
_exptl_crystal_size_mid          0.371
_exptl_crystal_size_min          0.246
_exptl_absorpt_coefficient_mu    0.064
_shelx_estimated_absorpt_T_min   0.969
_shelx_estimated_absorpt_T_max   0.985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8154
_exptl_absorpt_correction_T_max  0.9593
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_absorpt_special_details   
;
The ratio of minimum to maximum
apparent transmission was 0.850
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            53939
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.430
_diffrn_reflns_theta_max         28.381
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             8344
_reflns_number_gt                7123
_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       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'APEX3 v2016.9-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0634P)²+0.7984P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8344
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0523
_refine_ls_wR_factor_ref         0.1384
_refine_ls_wR_factor_gt          0.1320
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_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
N1 N 0.95033(17) 0.78287(10) 0.24289(4) 0.0221(2) Uani 1 1 d . . . . .
H1 H 0.939(3) 0.8537(16) 0.2582(7) 0.027(4) Uiso 1 1 d . . . . .
H2 H 0.947(3) 0.7949(16) 0.2071(8) 0.035(4) Uiso 1 1 d . . . . .
C1 C 0.80591(18) 0.69417(10) 0.26504(4) 0.0163(2) Uani 1 1 d . . . . .
C2 C 0.72219(17) 0.70053(10) 0.31919(4) 0.0155(2) Uani 1 1 d . . . . .
C3 C 0.56588(18) 0.61782(11) 0.33809(5) 0.0182(2) Uani 1 1 d . . . . .
H3 H 0.505621 0.622773 0.373903 0.022 Uiso 1 1 calc R U . . .
C4 C 0.49580(19) 0.52841(11) 0.30606(5) 0.0207(2) Uani 1 1 d . . . . .
H4 H 0.384188 0.475475 0.319159 0.025 Uiso 1 1 calc R U . . .
C5 C 0.59016(18) 0.51691(11) 0.25467(5) 0.0182(2) Uani 1 1 d . . . . .
H5 H 0.546095 0.453212 0.233386 0.022 Uiso 1 1 calc R U . . .
C6 C 0.74771(17) 0.59646(10) 0.23362(4) 0.0157(2) Uani 1 1 d . . . . .
C7 C 0.85856(18) 0.57686(11) 0.17743(5) 0.0178(2) Uani 1 1 d . . . . .
C8 C 1.10055(19) 0.55851(13) 0.18452(6) 0.0264(3) Uani 1 1 d . . . . .
H8A H 1.167929 0.525019 0.151825 0.040 Uiso 1 1 calc R U . . .
H8B H 1.124820 0.500098 0.215960 0.040 Uiso 1 1 calc R U . . .
H8C H 1.161704 0.638812 0.190248 0.040 Uiso 1 1 calc R U . . .
C9 C 0.77787(19) 0.45872(11) 0.15372(5) 0.0197(2) Uani 1 1 d . . . . .
C10 C 0.8627(2) 0.34116(12) 0.16910(5) 0.0255(3) Uani 1 1 d . . . . .
H10 H 0.970673 0.334044 0.194616 0.031 Uiso 1 1 calc R U . . .
C11 C 0.7929(2) 0.23342(12) 0.14788(6) 0.0296(3) Uani 1 1 d . . . . .
C12 C 0.6336(2) 0.24510(13) 0.11108(6) 0.0314(3) Uani 1 1 d . . . . .
H12 H 0.585598 0.172486 0.096319 0.038 Uiso 1 1 calc R U . . .
C13 C 0.5428(2) 0.35995(13) 0.09533(6) 0.0292(3) Uani 1 1 d . . . . .
C14 C 0.6175(2) 0.46624(12) 0.11656(5) 0.0234(3) Uani 1 1 d . . . . .
H14 H 0.558026 0.545564 0.105483 0.028 Uiso 1 1 calc R U . . .
C15 C 0.8914(3) 0.10799(14) 0.16437(8) 0.0444(4) Uani 1 1 d . . . . .
H15A H 0.837244 0.044846 0.142370 0.067 Uiso 1 1 calc R U . . .
H15B H 0.855032 0.086413 0.202819 0.067 Uiso 1 1 calc R U . . .
H15C H 1.045862 0.111147 0.158635 0.067 Uiso 1 1 calc R U . . .
C16 C 0.3663(3) 0.37156(18) 0.05599(7) 0.0470(4) Uani 1 1 d . . . . .
H16A H 0.356269 0.457419 0.040089 0.070 Uiso 1 1 calc R U . . .
H16B H 0.231606 0.349991 0.075311 0.070 Uiso 1 1 calc R U . . .
H16C H 0.396569 0.314791 0.027097 0.070 Uiso 1 1 calc R U . . .
C17 C 0.81102(19) 0.68754(11) 0.13659(5) 0.0198(2) Uani 1 1 d . . . . .
C18 C 0.9405(2) 0.70892(13) 0.08960(5) 0.0271(3) Uani 1 1 d . . . . .
H18 H 1.067128 0.660004 0.084888 0.033 Uiso 1 1 calc R U . . .
C19 C 0.8881(2) 0.80033(14) 0.04953(5) 0.0321(3) Uani 1 1 d . . . . .
C20 C 0.7028(3) 0.87132(13) 0.05662(5) 0.0318(3) Uani 1 1 d . . . . .
H20 H 0.665467 0.933243 0.029194 0.038 Uiso 1 1 calc R U . . .
C21 C 0.5702(2) 0.85353(12) 0.10323(5) 0.0257(3) Uani 1 1 d . . . . .
C22 C 0.6274(2) 0.76154(11) 0.14279(5) 0.0211(2) Uani 1 1 d . . . . .
H22 H 0.538899 0.748969 0.174816 0.025 Uiso 1 1 calc R U . . .
C23 C 1.0322(3) 0.81900(19) -0.00096(6) 0.0481(5) Uani 1 1 d . . . . .
H23A H 0.966985 0.880731 -0.026516 0.072 Uiso 1 1 calc R U . . .
H23B H 1.053638 0.739746 -0.017973 0.072 Uiso 1 1 calc R U . . .
H23C H 1.169236 0.848631 0.008887 0.072 Uiso 1 1 calc R U . . .
C24 C 0.3693(2) 0.92990(13) 0.11136(6) 0.0345(3) Uani 1 1 d . . . . .
H24A H 0.249245 0.874417 0.117985 0.052 Uiso 1 1 calc R U . . .
H24B H 0.346899 0.985062 0.078783 0.052 Uiso 1 1 calc R U . . .
H24C H 0.380647 0.980035 0.142618 0.052 Uiso 1 1 calc R U . . .
C25 C 0.80941(18) 0.79258(11) 0.35747(5) 0.0171(2) Uani 1 1 d . . . . .
C26 C 1.04976(19) 0.76152(13) 0.36217(5) 0.0254(3) Uani 1 1 d . . . . .
H26A H 1.102136 0.802490 0.392824 0.038 Uiso 1 1 calc R U . . .
H26B H 1.126951 0.791316 0.328594 0.038 Uiso 1 1 calc R U . . .
H26C H 1.071939 0.671158 0.368042 0.038 Uiso 1 1 calc R U . . .
C27 C 0.69839(18) 0.77551(11) 0.41479(5) 0.0182(2) Uani 1 1 d . . . . .
C28 C 0.52243(19) 0.84935(12) 0.43011(5) 0.0204(2) Uani 1 1 d . . . . .
H28 H 0.471464 0.912734 0.404963 0.025 Uiso 1 1 calc R U . . .
C29 C 0.4195(2) 0.83267(13) 0.48125(5) 0.0245(3) Uani 1 1 d . . . . .
C30 C 0.4961(2) 0.74016(14) 0.51793(5) 0.0285(3) Uani 1 1 d . . . . .
H30 H 0.428433 0.728653 0.553060 0.034 Uiso 1 1 calc R U . . .
C31 C 0.6694(2) 0.66447(13) 0.50415(5) 0.0282(3) Uani 1 1 d . . . . .
C32 C 0.7688(2) 0.68313(12) 0.45261(5) 0.0246(3) Uani 1 1 d . . . . .
H32 H 0.887664 0.631478 0.443027 0.030 Uiso 1 1 calc R U . . .
C33 C 0.2288(2) 0.91300(15) 0.49609(6) 0.0349(3) Uani 1 1 d . . . . .
H33A H 0.228739 0.928436 0.534687 0.052 Uiso 1 1 calc R U . . .
H33B H 0.099327 0.870345 0.489004 0.052 Uiso 1 1 calc R U . . .
H33C H 0.234325 0.992521 0.474250 0.052 Uiso 1 1 calc R U . . .
C34 C 0.7489(3) 0.56219(16) 0.54373(6) 0.0429(4) Uani 1 1 d . . . . .
H34A H 0.902445 0.568377 0.546352 0.064 Uiso 1 1 calc R U . . .
H34B H 0.717481 0.480916 0.530967 0.064 Uiso 1 1 calc R U . . .
H34C H 0.678200 0.570965 0.579538 0.064 Uiso 1 1 calc R U . . .
C35 C 0.7712(2) 0.92906(11) 0.33661(5) 0.0209(2) Uani 1 1 d . . . . .
C36 C 0.6016(2) 0.96381(12) 0.30423(5) 0.0244(3) Uani 1 1 d . . . . .
H36 H 0.515592 0.901139 0.292412 0.029 Uiso 1 1 calc R U . . .
C37 C 0.5556(3) 1.08837(14) 0.28887(6) 0.0353(3) Uani 1 1 d . . . . .
C38 C 0.6822(3) 1.17896(14) 0.30679(7) 0.0447(4) Uani 1 1 d . . . . .
H38 H 0.651299 1.264217 0.296843 0.054 Uiso 1 1 calc R U . . .
C39 C 0.8521(3) 1.14794(14) 0.33875(7) 0.0410(4) Uani 1 1 d . . . . .
C40 C 0.8966(2) 1.02284(13) 0.35314(6) 0.0302(3) Uani 1 1 d . . . . .
H40 H 1.014359 1.000767 0.374593 0.036 Uiso 1 1 calc R U . . .
C41 C 0.9878(4) 1.24778(18) 0.35854(9) 0.0661(7) Uani 1 1 d . . . . .
H41A H 1.135975 1.217926 0.358794 0.099 Uiso 1 1 calc R U . . .
H41B H 0.938134 1.266462 0.395372 0.099 Uiso 1 1 calc R U . . .
H41C H 0.976821 1.323412 0.334243 0.099 Uiso 1 1 calc R U . . .
C42 C 0.3741(3) 1.12266(18) 0.25288(7) 0.0507(5) Uani 1 1 d . . . . .
H42A H 0.306566 1.201181 0.263377 0.076 Uiso 1 1 calc R U . . .
H42B H 0.270001 1.056645 0.256892 0.076 Uiso 1 1 calc R U . . .
H42C H 0.427929 1.132452 0.214979 0.076 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
N1 C1 1.4049(14) . ?
N1 H1 0.874(17) . ?
N1 H2 0.887(19) . ?
C1 C6 1.4190(15) . ?
C1 C2 1.4193(15) . ?
C2 C3 1.3912(16) . ?
C2 C25 1.5496(15) . ?
C3 C4 1.3855(16) . ?
C3 H3 0.9500 . ?
C4 C5 1.3871(16) . ?
C4 H4 0.9500 . ?
C5 C6 1.3901(16) . ?
C5 H5 0.9500 . ?
C6 C7 1.5480(15) . ?
C7 C17 1.5388(17) . ?
C7 C9 1.5482(16) . ?
C7 C8 1.5520(16) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.3940(18) . ?
C9 C14 1.3984(17) . ?
C10 C11 1.3987(18) . ?
C10 H10 0.9500 . ?
C11 C12 1.388(2) . ?
C11 C15 1.507(2) . ?
C12 C13 1.385(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.3971(17) . ?
C13 C16 1.513(2) . ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C22 1.3936(18) . ?
C17 C18 1.3959(16) . ?
C18 C19 1.391(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.387(2) . ?
C19 C23 1.5121(19) . ?
C20 C21 1.3950(19) . ?
C20 H20 0.9500 . ?
C21 C22 1.3945(18) . ?
C21 C24 1.502(2) . ?
C22 H22 0.9500 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C35 1.5381(16) . ?
C25 C27 1.5503(15) . ?
C25 C26 1.5523(16) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C32 1.3945(17) . ?
C27 C28 1.3976(16) . ?
C28 C29 1.3944(17) . ?
C28 H28 0.9500 . ?
C29 C30 1.391(2) . ?
C29 C33 1.5053(18) . ?
C30 C31 1.386(2) . ?
C30 H30 0.9500 . ?
C31 C32 1.3958(18) . ?
C31 C34 1.512(2) . ?
C32 H32 0.9500 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.3962(18) . ?
C35 C40 1.3980(17) . ?
C36 C37 1.3933(18) . ?
C36 H36 0.9500 . ?
C37 C38 1.390(3) . ?
C37 C42 1.507(2) . ?
C38 C39 1.384(3) . ?
C38 H38 0.9500 . ?
C39 C40 1.392(2) . ?
C39 C41 1.518(2) . ?
C40 H40 0.9500 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 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 N1 H1 113.6(11) . . ?
C1 N1 H2 113.0(11) . . ?
H1 N1 H2 110.9(15) . . ?
N1 C1 C6 119.88(10) . . ?
N1 C1 C2 120.07(10) . . ?
C6 C1 C2 120.03(10) . . ?
C3 C2 C1 118.35(10) . . ?
C3 C2 C25 120.41(10) . . ?
C1 C2 C25 121.17(10) . . ?
C4 C3 C2 121.72(10) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C5 119.37(11) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C4 C5 C6 121.52(10) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C5 C6 C1 118.56(10) . . ?
C5 C6 C7 120.31(10) . . ?
C1 C6 C7 121.12(10) . . ?
C17 C7 C6 110.99(9) . . ?
C17 C7 C9 107.10(9) . . ?
C6 C7 C9 110.75(9) . . ?
C17 C7 C8 111.22(10) . . ?
C6 C7 C8 108.63(9) . . ?
C9 C7 C8 108.10(9) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C14 117.94(11) . . ?
C10 C9 C7 120.77(11) . . ?
C14 C9 C7 121.29(11) . . ?
C9 C10 C11 121.62(13) . . ?
C9 C10 H10 119.2 . . ?
C11 C10 H10 119.2 . . ?
C12 C11 C10 118.56(13) . . ?
C12 C11 C15 121.12(13) . . ?
C10 C11 C15 120.32(14) . . ?
C13 C12 C11 121.68(12) . . ?
C13 C12 H12 119.2 . . ?
C11 C12 H12 119.2 . . ?
C12 C13 C14 118.59(13) . . ?
C12 C13 C16 121.32(13) . . ?
C14 C13 C16 120.09(14) . . ?
C13 C14 C9 121.60(12) . . ?
C13 C14 H14 119.2 . . ?
C9 C14 H14 119.2 . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C22 C17 C18 118.14(12) . . ?
C22 C17 C7 121.01(10) . . ?
C18 C17 C7 120.56(11) . . ?
C19 C18 C17 121.40(13) . . ?
C19 C18 H18 119.3 . . ?
C17 C18 H18 119.3 . . ?
C20 C19 C18 119.02(12) . . ?
C20 C19 C23 121.53(14) . . ?
C18 C19 C23 119.45(15) . . ?
C19 C20 C21 121.29(13) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 H20 119.4 . . ?
C22 C21 C20 118.36(13) . . ?
C22 C21 C24 119.89(12) . . ?
C20 C21 C24 121.75(13) . . ?
C17 C22 C21 121.78(12) . . ?
C17 C22 H22 119.1 . . ?
C21 C22 H22 119.1 . . ?
C19 C23 H23A 109.5 . . ?
C19 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C19 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C35 C25 C2 111.88(9) . . ?
C35 C25 C27 107.29(9) . . ?
C2 C25 C27 110.48(9) . . ?
C35 C25 C26 111.14(10) . . ?
C2 C25 C26 107.40(9) . . ?
C27 C25 C26 108.62(9) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C32 C27 C28 117.60(11) . . ?
C32 C27 C25 120.68(10) . . ?
C28 C27 C25 121.71(10) . . ?
C29 C28 C27 121.89(11) . . ?
C29 C28 H28 119.1 . . ?
C27 C28 H28 119.1 . . ?
C30 C29 C28 118.66(12) . . ?
C30 C29 C33 120.94(12) . . ?
C28 C29 C33 120.40(12) . . ?
C31 C30 C29 121.18(12) . . ?
C31 C30 H30 119.4 . . ?
C29 C30 H30 119.4 . . ?
C30 C31 C32 118.87(12) . . ?
C30 C31 C34 120.95(13) . . ?
C32 C31 C34 120.18(13) . . ?
C27 C32 C31 121.80(12) . . ?
C27 C32 H32 119.1 . . ?
C31 C32 H32 119.1 . . ?
C29 C33 H33A 109.5 . . ?
C29 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C29 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 C40 118.24(12) . . ?
C36 C35 C25 121.12(11) . . ?
C40 C35 C25 120.46(12) . . ?
C37 C36 C35 121.46(13) . . ?
C37 C36 H36 119.3 . . ?
C35 C36 H36 119.3 . . ?
C38 C37 C36 118.53(15) . . ?
C38 C37 C42 121.29(15) . . ?
C36 C37 C42 120.17(16) . . ?
C39 C38 C37 121.60(14) . . ?
C39 C38 H38 119.2 . . ?
C37 C38 H38 119.2 . . ?
C38 C39 C40 118.91(14) . . ?
C38 C39 C41 121.09(17) . . ?
C40 C39 C41 119.99(19) . . ?
C39 C40 C35 121.25(15) . . ?
C39 C40 H40 119.4 . . ?
C35 C40 H40 119.4 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C37 C42 H42A 109.5 . . ?
C37 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C37 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?

_refine_diff_density_max         0.290
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.043

####################################################################### 
# 
# 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_jvr181015N1
_database_code_depnum_ccdc_archive 'CCDC 1956670'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2019-09-30 deposited with the CCDC.	2020-01-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H37 Cl2 N'
_chemical_formula_weight         662.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_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'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   8.7550(4)
_cell_length_b                   20.6545(11)
_cell_length_c                   9.7582(5)
_cell_angle_alpha                90
_cell_angle_beta                 106.074(2)
_cell_angle_gamma                90
_cell_volume                     1695.59(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7463
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      26.30

_exptl_crystal_description       stick
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_F_000             696
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.382
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.158
_exptl_absorpt_coefficient_mu    0.226
_shelx_estimated_absorpt_T_min   0.919
_shelx_estimated_absorpt_T_max   0.965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7886
_exptl_absorpt_correction_T_max  0.8371
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_absorpt_special_details   
;
The ratio of minimum to maximum
apparent transmission was 0.942
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            23655
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.385
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             3424
_reflns_number_gt                2765
_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       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'APEX3 v2016.9-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0588P)²+1.8447P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3424
_refine_ls_number_parameters     245
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0560
_refine_ls_wR_factor_ref         0.1433
_refine_ls_wR_factor_gt          0.1345
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.112
_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
Cl1 Cl 0.1344(9) 0.250000 0.5241(6) 0.0647(14) Uani 0.5 2 d DS T P A 1
Cl2 Cl 0.2652(4) 0.250000 0.8363(3) 0.0564(6) Uani 0.5 2 d DS TU P A 1
C1S C 0.3117(15) 0.250000 0.6698(9) 0.048(4) Uani 0.5 2 d DS TU P A 1
H1SA H 0.375908 0.211211 0.663543 0.058 Uiso 0.25 1 calc R U P A 1
H1SB H 0.375908 0.288789 0.663543 0.058 Uiso 0.25 1 calc R U P A 1
Cl1' Cl 0.1652(10) 0.2715(6) 0.5395(7) 0.0647(14) Uani 0.25 1 d D . P B -2
Cl2' Cl 0.2764(5) 0.27563(18) 0.8393(4) 0.0564(6) Uani 0.25 1 d D U P B -2
C1S' C 0.2950(17) 0.2302(6) 0.6890(11) 0.037(3) Uani 0.25 1 d D U P B -2
H1SC H 0.260824 0.184759 0.694122 0.045 Uiso 0.25 1 calc R U P B -2
H1SD H 0.406023 0.230549 0.682977 0.045 Uiso 0.25 1 calc R U P B -2
N1 N 0.4719(3) 0.250000 0.4062(3) 0.0175(5) Uani 1 2 d S T P . .
C1 C 0.5862(3) 0.250000 0.3314(3) 0.0145(5) Uani 1 2 d S T P . .
C2 C 0.6468(2) 0.30975(9) 0.29657(19) 0.0144(4) Uani 1 1 d . . . . .
C3 C 0.7714(2) 0.30787(10) 0.2334(2) 0.0191(4) Uani 1 1 d . . . . .
H3 H 0.815088 0.347376 0.211537 0.023 Uiso 1 1 calc R U . . .
C4 C 0.8328(3) 0.250000 0.2018(3) 0.0226(6) Uani 1 2 d S T P . .
H4 H 0.917438 0.249999 0.158355 0.027 Uiso 1 2 calc R U P . .
C5 C 0.5886(2) 0.37461(9) 0.3442(2) 0.0146(4) Uani 1 1 d . . . . .
C6 C 0.6296(2) 0.37107(9) 0.5102(2) 0.0171(4) Uani 1 1 d . . . . .
C7 C 0.5273(3) 0.38818(11) 0.5899(2) 0.0240(5) Uani 1 1 d . . . . .
H7 H 0.424212 0.403990 0.542896 0.029 Uiso 1 1 calc R U . . .
C8 C 0.5736(3) 0.38252(12) 0.7388(2) 0.0306(5) Uani 1 1 d . . . . .
H8 H 0.502368 0.395258 0.791697 0.037 Uiso 1 1 calc R U . . .
C9 C 0.7214(3) 0.35868(12) 0.8093(2) 0.0335(6) Uani 1 1 d . . . . .
H9 H 0.751616 0.354112 0.910093 0.040 Uiso 1 1 calc R U . . .
C10 C 0.8260(3) 0.34134(11) 0.7310(2) 0.0292(5) Uani 1 1 d . . . . .
H10 H 0.928640 0.325123 0.778175 0.035 Uiso 1 1 calc R U . . .
C11 C 0.7798(3) 0.34784(11) 0.5837(2) 0.0239(5) Uani 1 1 d . . . . .
H11 H 0.852401 0.336170 0.531358 0.029 Uiso 1 1 calc R U . . .
C12 C 0.6732(2) 0.43371(9) 0.2992(2) 0.0160(4) Uani 1 1 d . . . . .
C13 C 0.7682(2) 0.47620(10) 0.3965(2) 0.0196(4) Uani 1 1 d . . . . .
H13 H 0.789292 0.467840 0.495738 0.023 Uiso 1 1 calc R U . . .
C14 C 0.8332(2) 0.53101(10) 0.3506(2) 0.0246(5) Uani 1 1 d . . . . .
H14 H 0.897376 0.559676 0.418863 0.029 Uiso 1 1 calc R U . . .
C15 C 0.8052(2) 0.54394(10) 0.2074(3) 0.0260(5) Uani 1 1 d . . . . .
H15 H 0.850046 0.581179 0.176452 0.031 Uiso 1 1 calc R U . . .
C16 C 0.7101(2) 0.50165(11) 0.1081(2) 0.0240(5) Uani 1 1 d . . . . .
H16 H 0.690688 0.509906 0.009025 0.029 Uiso 1 1 calc R U . . .
C17 C 0.6441(2) 0.44786(10) 0.1535(2) 0.0193(4) Uani 1 1 d . . . . .
H17 H 0.577798 0.419928 0.084937 0.023 Uiso 1 1 calc R U . . .
C18 C 0.4096(2) 0.38715(9) 0.2710(2) 0.0164(4) Uani 1 1 d . . . . .
C19 C 0.3172(2) 0.34591(10) 0.1680(2) 0.0203(4) Uani 1 1 d . . . . .
H19 H 0.363156 0.307591 0.142924 0.024 Uiso 1 1 calc R U . . .
C20 C 0.1582(2) 0.36008(11) 0.1011(2) 0.0246(5) Uani 1 1 d . . . . .
H20 H 0.096313 0.330709 0.033163 0.030 Uiso 1 1 calc R U . . .
C21 C 0.0900(2) 0.41623(12) 0.1326(2) 0.0263(5) Uani 1 1 d . . . . .
H21 H -0.018654 0.425440 0.087648 0.032 Uiso 1 1 calc R U . . .
C22 C 0.1821(2) 0.45925(11) 0.2311(2) 0.0253(5) Uani 1 1 d . . . . .
H22 H 0.137175 0.498622 0.252094 0.030 Uiso 1 1 calc R U . . .
C23 C 0.3395(2) 0.44458(10) 0.2984(2) 0.0209(4) Uani 1 1 d . . . . .
H23 H 0.401340 0.474459 0.365136 0.025 Uiso 1 1 calc R U . . .
H1 H 0.423(3) 0.2861(12) 0.408(3) 0.030(7) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C1S 1.791(9) . ?
Cl2 C1S 1.781(8) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
Cl1' C1S' 1.797(9) . ?
Cl2' C1S' 1.787(9) . ?
C1S' H1SC 0.9900 . ?
C1S' H1SD 0.9900 . ?
N1 C1 1.392(3) . ?
N1 H1 0.86(2) . ?
N1 H1 0.86(2) 4_565 ?
C1 C2 1.421(2) 4_565 ?
C1 C2 1.421(2) . ?
C2 C3 1.394(3) . ?
C2 C5 1.550(3) . ?
C3 C4 1.380(2) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 C12 1.553(3) . ?
C5 C18 1.554(2) . ?
C5 C6 1.561(3) . ?
C6 C7 1.385(3) . ?
C6 C11 1.397(3) . ?
C7 C8 1.401(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.377(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.392(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.387(3) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.388(3) . ?
C12 C17 1.403(3) . ?
C13 C14 1.395(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.377(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.395(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.381(3) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 C19 1.393(3) . ?
C18 C23 1.395(3) . ?
C19 C20 1.395(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.377(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.390(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.386(3) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?

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
Cl2 C1S Cl1 110.9(6) . . ?
Cl2 C1S H1SA 109.5 . . ?
Cl1 C1S H1SA 109.5 . . ?
Cl2 C1S H1SB 109.5 . . ?
Cl1 C1S H1SB 109.5 . . ?
H1SA C1S H1SB 108.0 . . ?
Cl2' C1S' Cl1' 103.6(6) . . ?
Cl2' C1S' H1SC 111.0 . . ?
Cl1' C1S' H1SC 111.0 . . ?
Cl2' C1S' H1SD 111.0 . . ?
Cl1' C1S' H1SD 111.0 . . ?
H1SC C1S' H1SD 109.0 . . ?
H1SA C1S' H1SB 81.8 4_565 4_565 ?
C1 N1 H1 116.4(17) . . ?
C1 N1 H1 116.4(17) . 4_565 ?
H1 N1 H1 119(3) . 4_565 ?
N1 C1 C2 119.73(12) . 4_565 ?
N1 C1 C2 119.72(12) . . ?
C2 C1 C2 120.5(2) 4_565 . ?
C3 C2 C1 118.14(18) . . ?
C3 C2 C5 121.26(17) . . ?
C1 C2 C5 120.21(16) . . ?
C4 C3 C2 121.58(19) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C3 C4 C3 120.0(3) . 4_565 ?
C3 C4 H4 120.0 . . ?
C3 C4 H4 120.0 4_565 . ?
C2 C5 C12 111.90(15) . . ?
C2 C5 C18 112.33(15) . . ?
C12 C5 C18 103.79(15) . . ?
C2 C5 C6 105.68(15) . . ?
C12 C5 C6 109.87(15) . . ?
C18 C5 C6 113.41(15) . . ?
C7 C6 C11 117.56(18) . . ?
C7 C6 C5 124.90(17) . . ?
C11 C6 C5 117.53(17) . . ?
C6 C7 C8 121.0(2) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
C9 C8 C7 120.6(2) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C8 C9 C10 119.2(2) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C11 C10 C9 119.8(2) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C10 C11 C6 121.9(2) . . ?
C10 C11 H11 119.1 . . ?
C6 C11 H11 119.1 . . ?
C13 C12 C17 117.88(18) . . ?
C13 C12 C5 123.07(17) . . ?
C17 C12 C5 118.89(17) . . ?
C12 C13 C14 120.91(19) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C15 C14 C13 120.6(2) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C14 C15 C16 119.17(19) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 H15 120.4 . . ?
C17 C16 C15 120.23(19) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C12 121.17(19) . . ?
C16 C17 H17 119.4 . . ?
C12 C17 H17 119.4 . . ?
C19 C18 C23 117.41(18) . . ?
C19 C18 C5 122.67(17) . . ?
C23 C18 C5 119.66(17) . . ?
C18 C19 C20 120.92(19) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 H19 119.5 . . ?
C21 C20 C19 120.7(2) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C20 C21 C22 119.21(19) . . ?
C20 C21 H21 120.4 . . ?
C22 C21 H21 120.4 . . ?
C23 C22 C21 119.9(2) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C18 121.81(19) . . ?
C22 C23 H23 119.1 . . ?
C18 C23 H23 119.1 . . ?

_refine_diff_density_max         0.812
_refine_diff_density_min         -1.126
_refine_diff_density_rms         0.059

####################################################################### 
# 
# 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_jvr190225N3
_database_code_depnum_ccdc_archive 'CCDC 1956676'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2019-09-30 deposited with the CCDC.	2020-01-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C68 H83 N'
_chemical_formula_sum            'C68 H83 N'
_chemical_formula_weight         914.35

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'

_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                   19.1224(7)
_cell_length_b                   13.9671(5)
_cell_length_c                   20.7356(7)
_cell_angle_alpha                90
_cell_angle_beta                 93.2520(10)
_cell_angle_gamma                90
_cell_volume                     5529.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    65521
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_F_000             1992
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.226
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.7137
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_absorpt_special_details   
;
The ratio of minimum to maximum
apparent transmission was 0.957
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            65521
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.627
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6349
_reflns_number_gt                5359
_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       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'APEX3 v2016.5-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Platon (Spek, 2009)'
_computing_publication_material  'Platon (Spek, 2009)'

_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)+(0.0596P)²+5.9680P] 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         6349
_refine_ls_number_parameters     326
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0503
_refine_ls_wR_factor_ref         0.1300
_refine_ls_wR_factor_gt          0.1233
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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
N1 N 0.5000 0.46394(11) 0.7500 0.0185(3) Uani 1 2 d S T P . .
H1 H 0.5024(10) 0.4965(14) 0.7863(9) 0.038(5) Uiso 1 1 d . . . . .
C1 C 0.5000 0.36488(12) 0.7500 0.0141(3) Uani 1 2 d S T P . .
C2 C 0.50078(6) 0.31399(9) 0.69054(6) 0.0142(2) Uani 1 1 d . . . . .
C3 C 0.49963(7) 0.21439(9) 0.69214(6) 0.0193(3) Uani 1 1 d . . . . .
H3 H 0.4986 0.1798 0.6527 0.023 Uiso 1 1 calc R U . . .
C5 C 0.50233(6) 0.36937(9) 0.62539(6) 0.0141(2) Uani 1 1 d . . . . .
C4 C 0.5000 0.16445(13) 0.7500 0.0237(4) Uani 1 2 d S T P . .
H4 H 0.5000 0.0964 0.7500 0.028 Uiso 1 2 calc R U P . .
C7 C 0.54553(7) 0.24311(10) 0.54645(6) 0.0200(3) Uani 1 1 d . . . . .
H7 H 0.5883 0.2409 0.5720 0.024 Uiso 1 1 calc R U . . .
C6 C 0.49137(7) 0.30231(9) 0.56568(6) 0.0154(2) Uani 1 1 d . . . . .
C9 C 0.47672(7) 0.18895(9) 0.45094(6) 0.0193(3) Uani 1 1 d . . . . .
C8 C 0.53812(7) 0.18765(10) 0.49104(6) 0.0216(3) Uani 1 1 d . . . . .
H8 H 0.5758 0.1476 0.4800 0.026 Uiso 1 1 calc R U . . .
C10 C 0.42326(7) 0.24690(11) 0.47029(7) 0.0241(3) Uani 1 1 d . . . . .
H10 H 0.3805 0.2494 0.4446 0.029 Uiso 1 1 calc R U . . .
C11 C 0.43021(7) 0.30193(10) 0.52652(6) 0.0210(3) Uani 1 1 d . . . . .
H11 H 0.3919 0.3402 0.5383 0.025 Uiso 1 1 calc R U . . .
C12 C 0.46972(8) 0.12820(10) 0.38902(6) 0.0246(3) Uani 1 1 d . . . . .
C13 C 0.47453(9) 0.02198(11) 0.40744(8) 0.0341(4) Uani 1 1 d . . . . .
H13A H 0.4697 -0.0173 0.3683 0.051 Uiso 1 1 calc R U . . .
H13B H 0.4369 0.0061 0.4358 0.051 Uiso 1 1 calc R U . . .
H13C H 0.5200 0.0093 0.4300 0.051 Uiso 1 1 calc R U . . .
C14 C 0.39977(9) 0.14453(13) 0.35095(8) 0.0392(4) Uani 1 1 d . . . . .
H14A H 0.3954 0.2122 0.3390 0.059 Uiso 1 1 calc R U . . .
H14B H 0.3612 0.1266 0.3777 0.059 Uiso 1 1 calc R U . . .
H14C H 0.3979 0.1052 0.3118 0.059 Uiso 1 1 calc R U . . .
C15 C 0.52895(10) 0.15282(14) 0.34519(8) 0.0407(4) Uani 1 1 d . . . . .
H15A H 0.5261 0.1108 0.3073 0.061 Uiso 1 1 calc R U . . .
H15B H 0.5742 0.1437 0.3690 0.061 Uiso 1 1 calc R U . . .
H15C H 0.5244 0.2197 0.3312 0.061 Uiso 1 1 calc R U . . .
C16 C 0.44140(6) 0.44331(9) 0.62400(6) 0.0149(2) Uani 1 1 d . . . . .
C17 C 0.37586(7) 0.41430(9) 0.64381(6) 0.0180(3) Uani 1 1 d . . . . .
H17 H 0.3689 0.3491 0.6547 0.022 Uiso 1 1 calc R U . . .
C18 C 0.32068(7) 0.47838(10) 0.64793(6) 0.0198(3) Uani 1 1 d . . . . .
H18 H 0.2769 0.4558 0.6612 0.024 Uiso 1 1 calc R U . . .
C19 C 0.32824(7) 0.57519(9) 0.63302(6) 0.0183(3) Uani 1 1 d . . . . .
C20 C 0.39297(7) 0.60315(9) 0.61155(6) 0.0195(3) Uani 1 1 d . . . . .
H20 H 0.3995 0.6681 0.5996 0.023 Uiso 1 1 calc R U . . .
C21 C 0.44841(7) 0.53936(9) 0.60699(6) 0.0172(3) Uani 1 1 d . . . . .
H21 H 0.4916 0.5615 0.5921 0.021 Uiso 1 1 calc R U . . .
C22 C 0.27121(7) 0.65045(10) 0.64349(7) 0.0242(3) Uani 1 1 d . . . . .
C23 C 0.19987(8) 0.60429(12) 0.65365(9) 0.0341(4) Uani 1 1 d . . . . .
H23A H 0.1854 0.5657 0.6157 0.051 Uiso 1 1 calc R U . . .
H23B H 0.1650 0.6545 0.6597 0.051 Uiso 1 1 calc R U . . .
H23C H 0.2036 0.5632 0.6920 0.051 Uiso 1 1 calc R U . . .
C24 C 0.26286(9) 0.71802(13) 0.58544(9) 0.0376(4) Uani 1 1 d . . . . .
H24A H 0.2497 0.6810 0.5465 0.056 Uiso 1 1 calc R U . . .
H24B H 0.3073 0.7511 0.5797 0.056 Uiso 1 1 calc R U . . .
H24C H 0.2263 0.7652 0.5929 0.056 Uiso 1 1 calc R U . . .
C25 C 0.29376(9) 0.70869(13) 0.70432(9) 0.0380(4) Uani 1 1 d . . . . .
H25A H 0.3380 0.7417 0.6975 0.057 Uiso 1 1 calc R U . . .
H25B H 0.3001 0.6654 0.7414 0.057 Uiso 1 1 calc R U . . .
H25C H 0.2575 0.7560 0.7127 0.057 Uiso 1 1 calc R U . . .
C26 C 0.57477(6) 0.41781(9) 0.61955(6) 0.0156(2) Uani 1 1 d . . . . .
C27 C 0.59150(7) 0.45828(10) 0.56051(6) 0.0201(3) Uani 1 1 d . . . . .
H27 H 0.5578 0.4563 0.5250 0.024 Uiso 1 1 calc R U . . .
C28 C 0.65561(7) 0.50097(10) 0.55247(7) 0.0224(3) Uani 1 1 d . . . . .
H28 H 0.6651 0.5267 0.5115 0.027 Uiso 1 1 calc R U . . .
C29 C 0.70688(7) 0.50723(10) 0.60308(7) 0.0204(3) Uani 1 1 d . . . . .
C30 C 0.69094(7) 0.46533(10) 0.66112(7) 0.0226(3) Uani 1 1 d . . . . .
H30 H 0.7248 0.4671 0.6965 0.027 Uiso 1 1 calc R U . . .
C31 C 0.62667(7) 0.42062(10) 0.66922(6) 0.0198(3) Uani 1 1 d . . . . .
H31 H 0.6183 0.3916 0.7095 0.024 Uiso 1 1 calc R U . . .
C32 C 0.77633(7) 0.55862(11) 0.59295(7) 0.0264(3) Uani 1 1 d . . . . .
C33 C 0.76166(10) 0.66521(13) 0.57929(12) 0.0489(5) Uani 1 1 d . . . . .
H33A H 0.8060 0.6987 0.5738 0.073 Uiso 1 1 calc R U . . .
H33B H 0.7382 0.6934 0.6156 0.073 Uiso 1 1 calc R U . . .
H33C H 0.7314 0.6715 0.5397 0.073 Uiso 1 1 calc R U . . .
C34 C 0.81077(9) 0.51501(15) 0.53479(9) 0.0416(4) Uani 1 1 d . . . . .
H34A H 0.7796 0.5227 0.4960 0.062 Uiso 1 1 calc R U . . .
H34B H 0.8195 0.4468 0.5426 0.062 Uiso 1 1 calc R U . . .
H34C H 0.8552 0.5477 0.5286 0.062 Uiso 1 1 calc R U . . .
C35 C 0.82758(9) 0.55193(16) 0.65206(9) 0.0454(5) Uani 1 1 d . . . . .
H35A H 0.8369 0.4845 0.6623 0.068 Uiso 1 1 calc R U . . .
H35B H 0.8072 0.5831 0.6890 0.068 Uiso 1 1 calc R U . . .
H35C H 0.8715 0.5839 0.6428 0.068 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
N1 C1 1.384(2) . ?
N1 H1 0.878(19) . ?
C1 C2 1.4240(14) . ?
C1 C2 1.4241(14) 2_656 ?
C2 C3 1.3917(18) . ?
C2 C5 1.5583(16) . ?
C3 C4 1.3875(16) . ?
C3 H3 0.9500 . ?
C5 C26 1.5525(17) . ?
C5 C16 1.5560(17) . ?
C5 C6 1.5572(16) . ?
C4 C3 1.3875(16) 2_656 ?
C4 H4 0.9500 . ?
C7 C8 1.3861(18) . ?
C7 C6 1.4009(18) . ?
C7 H7 0.9500 . ?
C6 C11 1.3854(18) . ?
C9 C10 1.3811(19) . ?
C9 C8 1.3998(19) . ?
C9 C12 1.5385(18) . ?
C8 H8 0.9500 . ?
C10 C11 1.3965(18) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C15 1.531(2) . ?
C12 C14 1.531(2) . ?
C12 C13 1.533(2) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C21 1.3954(18) . ?
C16 C17 1.4008(17) . ?
C17 C18 1.3899(18) . ?
C17 H17 0.9500 . ?
C18 C19 1.3965(19) . ?
C18 H18 0.9500 . ?
C19 C20 1.3948(18) . ?
C19 C22 1.5387(18) . ?
C20 C21 1.3922(18) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C24 1.531(2) . ?
C22 C23 1.534(2) . ?
C22 C25 1.542(2) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C31 1.3897(18) . ?
C26 C27 1.4017(17) . ?
C27 C28 1.3820(19) . ?
C27 H27 0.9500 . ?
C28 C29 1.3976(19) . ?
C28 H28 0.9500 . ?
C29 C30 1.3878(19) . ?
C29 C32 1.5344(18) . ?
C30 C31 1.3970(18) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 C35 1.528(2) . ?
C32 C34 1.533(2) . ?
C32 C33 1.538(2) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 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 N1 H1 121.2(13) . . ?
N1 C1 C2 119.95(8) . . ?
N1 C1 C2 119.95(8) . 2_656 ?
C2 C1 C2 120.11(15) . 2_656 ?
C3 C2 C1 118.51(12) . . ?
C3 C2 C5 121.19(11) . . ?
C1 C2 C5 120.29(11) . . ?
C4 C3 C2 121.59(12) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C26 C5 C16 112.32(10) . . ?
C26 C5 C6 106.29(9) . . ?
C16 C5 C6 108.51(9) . . ?
C26 C5 C2 110.18(10) . . ?
C16 C5 C2 107.13(9) . . ?
C6 C5 C2 112.49(10) . . ?
C3 C4 C3 119.64(17) . 2_656 ?
C3 C4 H4 120.2 . . ?
C3 C4 H4 120.2 2_656 . ?
C8 C7 C6 121.55(12) . . ?
C8 C7 H7 119.2 . . ?
C6 C7 H7 119.2 . . ?
C11 C6 C7 116.37(11) . . ?
C11 C6 C5 122.65(11) . . ?
C7 C6 C5 120.86(11) . . ?
C10 C9 C8 116.41(12) . . ?
C10 C9 C12 122.33(12) . . ?
C8 C9 C12 121.26(12) . . ?
C7 C8 C9 121.87(12) . . ?
C7 C8 H8 119.1 . . ?
C9 C8 H8 119.1 . . ?
C9 C10 C11 121.88(12) . . ?
C9 C10 H10 119.1 . . ?
C11 C10 H10 119.1 . . ?
C6 C11 C10 121.91(12) . . ?
C6 C11 H11 119.0 . . ?
C10 C11 H11 119.0 . . ?
C15 C12 C14 108.33(13) . . ?
C15 C12 C13 109.22(14) . . ?
C14 C12 C13 108.11(13) . . ?
C15 C12 C9 109.84(12) . . ?
C14 C12 C9 112.35(12) . . ?
C13 C12 C9 108.94(12) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C16 C17 116.91(12) . . ?
C21 C16 C5 124.07(11) . . ?
C17 C16 C5 118.95(11) . . ?
C18 C17 C16 121.79(12) . . ?
C18 C17 H17 119.1 . . ?
C16 C17 H17 119.1 . . ?
C17 C18 C19 121.43(12) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 H18 119.3 . . ?
C20 C19 C18 116.52(12) . . ?
C20 C19 C22 120.18(12) . . ?
C18 C19 C22 123.17(12) . . ?
C21 C20 C19 122.38(12) . . ?
C21 C20 H20 118.8 . . ?
C19 C20 H20 118.8 . . ?
C20 C21 C16 120.91(12) . . ?
C20 C21 H21 119.5 . . ?
C16 C21 H21 119.5 . . ?
C24 C22 C23 108.24(13) . . ?
C24 C22 C19 110.69(12) . . ?
C23 C22 C19 112.03(12) . . ?
C24 C22 C25 109.26(14) . . ?
C23 C22 C25 108.61(13) . . ?
C19 C22 C25 107.96(11) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C31 C26 C27 116.56(11) . . ?
C31 C26 C5 123.87(11) . . ?
C27 C26 C5 119.52(11) . . ?
C28 C27 C26 121.83(12) . . ?
C28 C27 H27 119.1 . . ?
C26 C27 H27 119.1 . . ?
C27 C28 C29 121.71(12) . . ?
C27 C28 H28 119.1 . . ?
C29 C28 H28 119.1 . . ?
C30 C29 C28 116.46(12) . . ?
C30 C29 C32 123.39(12) . . ?
C28 C29 C32 120.14(12) . . ?
C29 C30 C31 122.05(12) . . ?
C29 C30 H30 119.0 . . ?
C31 C30 H30 119.0 . . ?
C26 C31 C30 121.31(12) . . ?
C26 C31 H31 119.3 . . ?
C30 C31 H31 119.3 . . ?
C35 C32 C34 108.79(13) . . ?
C35 C32 C29 112.48(13) . . ?
C34 C32 C29 109.61(13) . . ?
C35 C32 C33 107.99(15) . . ?
C34 C32 C33 108.76(15) . . ?
C29 C32 C33 109.13(12) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?

_refine_diff_density_max         0.302
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.045

####################################################################### 
# 
# 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_jvr190222N1
_database_code_depnum_ccdc_archive 'CCDC 1956674'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2019-09-30 deposited with the CCDC.	2020-01-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H43 N O2'
_chemical_formula_sum            'C40 H43 N O2'
_chemical_formula_weight         569.75

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                   10.3051(4)
_cell_length_b                   12.5154(6)
_cell_length_c                   13.8322(6)
_cell_angle_alpha                73.950(2)
_cell_angle_beta                 68.779(2)
_cell_angle_gamma                80.981(2)
_cell_volume                     1594.98(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    65626
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_F_000             612
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.514
_exptl_crystal_size_mid          0.387
_exptl_crystal_size_min          0.208
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7223
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_absorpt_special_details   
;
The ratio of minimum to maximum
apparent transmission was 0.967
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            65626
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.200
_diffrn_reflns_theta_max         34.023
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             11316
_reflns_number_gt                8469
_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       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'APEX3 v2016.5-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Platon (Spek, 2009)'
_computing_publication_material  'Platon (Spek, 2009)'

_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)+(0.0780P)²+0.6976P] 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         11316
_refine_ls_number_parameters     412
_refine_ls_number_restraints     357
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0587
_refine_ls_wR_factor_ref         0.1596
_refine_ls_wR_factor_gt          0.1450
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.016
_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
O1' O 0.57249(9) 0.13362(7) 0.32881(7) 0.01631(17) Uani 1 1 d . U . . .
H1' H 0.498(2) 0.1017(16) 0.3674(15) 0.036(5) Uiso 1 1 d . . . . .
H1B H 0.2762(19) 0.1676(15) 0.4028(15) 0.030(4) Uiso 1 1 d . . . . .
H1AA H 0.236(2) 0.0797(16) 0.5039(15) 0.033(5) Uiso 1 1 d . . . . .
N1 N 0.30378(11) 0.12567(9) 0.45770(8) 0.0179(2) Uani 1 1 d . U . . .
C1 C 0.34181(11) 0.19663(9) 0.50618(8) 0.0135(2) Uani 1 1 d . U . . .
C2 C 0.45713(11) 0.26152(9) 0.44398(8) 0.0134(2) Uani 1 1 d . U . . .
H2' H 0.251(2) -0.0143(16) 0.6835(15) 0.035(5) Uiso 1 1 d . . . . .
O2' O 0.17791(9) 0.01641(7) 0.66797(7) 0.01732(17) Uani 1 1 d . U . . .
C3 C 0.49096(12) 0.33787(10) 0.48636(9) 0.0155(2) Uani 1 1 d . U . . .
H3 H 0.5665 0.3837 0.4440 0.019 Uiso 1 1 calc R U . . .
C6 C 0.27057(11) 0.20119(9) 0.61333(9) 0.0138(2) Uani 1 1 d . U . . .
C5 C 0.30876(12) 0.27820(10) 0.65279(9) 0.0168(2) Uani 1 1 d . U . . .
H5 H 0.2604 0.2830 0.7245 0.020 Uiso 1 1 calc R U . . .
C4 C 0.41579(13) 0.34787(10) 0.58961(9) 0.0180(2) Uani 1 1 d . U . . .
H4 H 0.4375 0.4021 0.6169 0.022 Uiso 1 1 calc R U . . .
C9 C 0.37112(12) 0.40156(10) 0.26923(10) 0.0186(2) Uani 1 1 d . U . . .
H9 H 0.3526 0.4260 0.3324 0.022 Uiso 1 1 calc R U . . .
C8 C 0.45833(11) 0.30630(10) 0.25403(9) 0.0147(2) Uani 1 1 d . U . . .
C7 C 0.54080(11) 0.24995(9) 0.32943(9) 0.0132(2) Uani 1 1 d . U . . .
C10 C 0.31042(13) 0.46179(11) 0.19345(10) 0.0208(2) Uani 1 1 d . U . . .
C11 C 0.33760(13) 0.42435(11) 0.10222(10) 0.0228(2) Uani 1 1 d . U . . .
H11 H 0.2986 0.4658 0.0494 0.027 Uiso 1 1 calc R U . . .
C12 C 0.42068(14) 0.32746(12) 0.08614(10) 0.0226(2) Uani 1 1 d . U . . .
C13 C 0.48016(12) 0.26872(11) 0.16306(9) 0.0188(2) Uani 1 1 d . U . . .
H13 H 0.5364 0.2021 0.1533 0.023 Uiso 1 1 calc R U . . .
C14 C 0.21844(17) 0.56549(13) 0.21060(13) 0.0343(3) Uani 1 1 d . U . . .
H14A H 0.2002 0.6049 0.1445 0.051 Uiso 1 1 calc R U . . .
H14B H 0.2652 0.6140 0.2307 0.051 Uiso 1 1 calc R U . . .
H14C H 0.1300 0.5452 0.2678 0.051 Uiso 1 1 calc R U . . .
C15 C 0.4466(2) 0.28815(16) -0.01326(13) 0.0401(4) Uani 1 1 d . U . . .
H15A H 0.4616 0.3523 -0.0749 0.060 Uiso 1 1 calc R U . . .
H15B H 0.3655 0.2504 -0.0052 0.060 Uiso 1 1 calc R U . . .
H15C H 0.5294 0.2362 -0.0243 0.060 Uiso 1 1 calc R U . . .
C16 C 0.68283(11) 0.30064(10) 0.28863(9) 0.0147(2) Uani 1 1 d . U . . .
C17 C 0.70758(12) 0.40567(10) 0.21962(9) 0.0184(2) Uani 1 1 d . U . . .
H17 H 0.6348 0.4481 0.1965 0.022 Uiso 1 1 calc R U . . .
C18 C 0.83824(13) 0.44958(11) 0.18387(10) 0.0220(2) Uani 1 1 d . U . . .
C19 C 0.94396(13) 0.38517(12) 0.21662(11) 0.0245(3) Uani 1 1 d . U . . .
H19 H 1.0339 0.4132 0.1906 0.029 Uiso 1 1 calc R U . . .
C20 C 0.92173(13) 0.28072(12) 0.28644(11) 0.0225(2) Uani 1 1 d . U . . .
C21 C 0.78978(12) 0.23980(10) 0.32376(10) 0.0180(2) Uani 1 1 d . U . . .
H21 H 0.7724 0.1697 0.3737 0.022 Uiso 1 1 calc R U . . .
C22 C 0.86347(16) 0.56399(13) 0.11038(12) 0.0324(3) Uani 1 1 d . U . . .
H22A H 0.8879 0.5589 0.0364 0.049 Uiso 1 1 calc R U . . .
H22B H 0.9402 0.5945 0.1180 0.049 Uiso 1 1 calc R U . . .
H22C H 0.7787 0.6129 0.1290 0.049 Uiso 1 1 calc R U . . .
C23 C 1.03859(15) 0.21350(14) 0.32169(15) 0.0347(3) Uani 1 1 d . U . . .
H23A H 1.1211 0.2087 0.2588 0.052 Uiso 1 1 calc R U . . .
H23B H 1.0094 0.1384 0.3616 0.052 Uiso 1 1 calc R U . . .
H23C H 1.0611 0.2498 0.3675 0.052 Uiso 1 1 calc R U . . .
C24 C 0.14801(11) 0.12808(9) 0.68466(9) 0.0139(2) Uani 1 1 d . U . . .
C25 C 0.01627(11) 0.16927(10) 0.65452(9) 0.0154(2) Uani 1 1 d . U . . .
C26 C 0.00086(13) 0.27413(10) 0.59053(10) 0.0194(2) Uani 1 1 d . U . . .
H26 H 0.0740 0.3234 0.5639 0.023 Uiso 1 1 calc R U . . .
C27 C -0.12129(14) 0.30836(11) 0.56469(11) 0.0239(3) Uani 1 1 d . U . . .
C28 C -0.22735(14) 0.23578(12) 0.60536(11) 0.0263(3) Uani 1 1 d . U . . .
H28 H -0.3104 0.2584 0.5882 0.032 Uiso 1 1 calc R U . . .
C29 C -0.21528(13) 0.13068(12) 0.67068(11) 0.0241(3) Uani 1 1 d . U . . .
C30 C -0.09272(12) 0.09809(11) 0.69419(10) 0.0201(2) Uani 1 1 d . U . . .
H30 H -0.0828 0.0262 0.7380 0.024 Uiso 1 1 calc R U . . .
C31 C -0.13706(18) 0.42157(13) 0.49387(14) 0.0363(4) Uani 1 1 d . U . . .
H31A H -0.0481 0.4393 0.4364 0.055 Uiso 1 1 calc R U . . .
H31B H -0.1644 0.4777 0.5361 0.055 Uiso 1 1 calc R U . . .
H31C H -0.2089 0.4214 0.4630 0.055 Uiso 1 1 calc R U . . .
C32 C -0.33433(16) 0.05435(16) 0.71447(14) 0.0374(4) Uani 1 1 d . U . . .
H32A H -0.3693 0.0547 0.6573 0.056 Uiso 1 1 calc R U . . .
H32B H -0.4096 0.0806 0.7720 0.056 Uiso 1 1 calc R U . . .
H32C H -0.3011 -0.0216 0.7425 0.056 Uiso 1 1 calc R U . . .
C33 C 0.12161(11) 0.12156(9) 0.80249(9) 0.0148(2) Uani 1 1 d . U . . .
C34 C 0.00464(12) 0.17291(10) 0.86532(9) 0.0159(2) Uani 1 1 d . U . . .
H34 H -0.0644 0.2116 0.8356 0.019 Uiso 1 1 calc R U . . .
C35 C -0.01340(13) 0.16873(10) 0.97138(9) 0.0182(2) Uani 1 1 d . U . . .
C36 C 0.08885(13) 0.11231(11) 1.01353(9) 0.0211(2) Uani 1 1 d . U . . .
H36 H 0.0780 0.1096 1.0853 0.025 Uiso 1 1 calc R U . . .
C37 C 0.20698(13) 0.05959(11) 0.95254(10) 0.0204(2) Uani 1 1 d . U . . .
C38 C 0.22251(12) 0.06497(10) 0.84733(9) 0.0183(2) Uani 1 1 d . U . . .
H38 H 0.3030 0.0296 0.8050 0.022 Uiso 1 1 calc R U . . .
C39 C -0.14051(15) 0.22376(12) 1.03924(10) 0.0269(3) Uani 1 1 d . U . . .
H39A H -0.1174 0.2954 1.0425 0.040 Uiso 1 1 calc R U . . .
H39B H -0.1724 0.1757 1.1115 0.040 Uiso 1 1 calc R U . . .
H39C H -0.2147 0.2361 1.0080 0.040 Uiso 1 1 calc R U . . .
C40 C 0.31482(15) -0.00354(14) 1.00039(12) 0.0311(3) Uani 1 1 d . U . . .
H40A H 0.3952 -0.0274 0.9445 0.047 Uiso 1 1 calc R U . . .
H40B H 0.2745 -0.0691 1.0557 0.047 Uiso 1 1 calc R U . . .
H40C H 0.3449 0.0447 1.0322 0.047 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' C7 1.4430(13) . ?
O1' H1' 0.85(2) . ?
N1 C1 1.4215(15) . ?
N1 H1B 0.907(19) . ?
N1 H1AA 0.907(19) . ?
C1 C6 1.4089(15) . ?
C1 C2 1.4100(15) . ?
C2 C3 1.3930(16) . ?
C2 C7 1.5406(15) . ?
O2' C24 1.4469(14) . ?
O2' H2' 0.86(2) . ?
C3 C4 1.3867(16) . ?
C3 H3 0.9500 . ?
C6 C5 1.3954(16) . ?
C6 C24 1.5385(15) . ?
C5 C4 1.3867(16) . ?
C5 H5 0.9500 . ?
C4 H4 0.9500 . ?
C9 C8 1.3926(16) . ?
C9 C10 1.3958(16) . ?
C9 H9 0.9500 . ?
C8 C13 1.3943(16) . ?
C8 C7 1.5344(15) . ?
C7 C16 1.5357(15) . ?
C10 C11 1.3858(18) . ?
C10 C14 1.5036(18) . ?
C11 C12 1.3923(19) . ?
C11 H11 0.9500 . ?
C12 C13 1.3952(17) . ?
C12 C15 1.5070(19) . ?
C13 H13 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.3926(16) . ?
C16 C21 1.3967(15) . ?
C17 C18 1.3996(17) . ?
C17 H17 0.9500 . ?
C18 C19 1.3864(19) . ?
C18 C22 1.5072(19) . ?
C19 C20 1.389(2) . ?
C19 H19 0.9500 . ?
C20 C21 1.3935(17) . ?
C20 C23 1.5087(18) . ?
C21 H21 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C33 1.5329(15) . ?
C24 C25 1.5343(15) . ?
C25 C26 1.3874(16) . ?
C25 C30 1.3977(17) . ?
C26 C27 1.4028(17) . ?
C26 H26 0.9500 . ?
C27 C28 1.386(2) . ?
C27 C31 1.5063(19) . ?
C28 C29 1.391(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.3892(17) . ?
C29 C32 1.515(2) . ?
C30 H30 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.3888(16) . ?
C33 C38 1.4002(15) . ?
C34 C35 1.3974(16) . ?
C34 H34 0.9500 . ?
C35 C36 1.3902(17) . ?
C35 C39 1.5019(17) . ?
C36 C37 1.3934(18) . ?
C36 H36 0.9500 . ?
C37 C38 1.3887(17) . ?
C37 C40 1.5051(17) . ?
C38 H38 0.9500 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 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
C7 O1' H1' 105.8(13) . . ?
C1 N1 H1B 109.4(12) . . ?
C1 N1 H1AA 113.5(12) . . ?
H1B N1 H1AA 110.1(16) . . ?
C6 C1 C2 120.19(10) . . ?
C6 C1 N1 122.11(10) . . ?
C2 C1 N1 117.68(10) . . ?
C3 C2 C1 119.13(10) . . ?
C3 C2 C7 120.98(10) . . ?
C1 C2 C7 119.86(10) . . ?
C24 O2' H2' 110.7(13) . . ?
C4 C3 C2 120.87(11) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C5 C6 C1 118.47(10) . . ?
C5 C6 C24 119.96(10) . . ?
C1 C6 C24 121.49(10) . . ?
C4 C5 C6 121.47(10) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C5 C4 C3 119.55(11) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C8 C9 C10 121.28(11) . . ?
C8 C9 H9 119.4 . . ?
C10 C9 H9 119.4 . . ?
C9 C8 C13 118.78(10) . . ?
C9 C8 C7 120.95(10) . . ?
C13 C8 C7 119.99(10) . . ?
O1' C7 C8 110.29(9) . . ?
O1' C7 C16 105.39(8) . . ?
C8 C7 C16 109.91(9) . . ?
O1' C7 C2 109.72(9) . . ?
C8 C7 C2 110.48(9) . . ?
C16 C7 C2 110.95(9) . . ?
C11 C10 C9 118.59(11) . . ?
C11 C10 C14 120.99(11) . . ?
C9 C10 C14 120.42(12) . . ?
C10 C11 C12 121.59(11) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 H11 119.2 . . ?
C11 C12 C13 118.72(11) . . ?
C11 C12 C15 120.26(12) . . ?
C13 C12 C15 121.02(12) . . ?
C8 C13 C12 120.98(11) . . ?
C8 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C21 119.08(10) . . ?
C17 C16 C7 122.30(10) . . ?
C21 C16 C7 118.61(10) . . ?
C16 C17 C18 120.93(11) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C19 C18 C17 118.58(12) . . ?
C19 C18 C22 120.86(12) . . ?
C17 C18 C22 120.55(12) . . ?
C18 C19 C20 121.69(11) . . ?
C18 C19 H19 119.2 . . ?
C20 C19 H19 119.2 . . ?
C19 C20 C21 118.89(11) . . ?
C19 C20 C23 120.31(12) . . ?
C21 C20 C23 120.80(13) . . ?
C20 C21 C16 120.74(12) . . ?
C20 C21 H21 119.6 . . ?
C16 C21 H21 119.6 . . ?
C18 C22 H22A 109.5 . . ?
C18 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C18 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O2' C24 C33 108.69(9) . . ?
O2' C24 C25 103.68(9) . . ?
C33 C24 C25 111.84(9) . . ?
O2' C24 C6 110.71(9) . . ?
C33 C24 C6 109.95(9) . . ?
C25 C24 C6 111.78(9) . . ?
C26 C25 C30 119.00(10) . . ?
C26 C25 C24 122.71(10) . . ?
C30 C25 C24 118.29(10) . . ?
C25 C26 C27 120.85(12) . . ?
C25 C26 H26 119.6 . . ?
C27 C26 H26 119.6 . . ?
C28 C27 C26 118.68(12) . . ?
C28 C27 C31 120.50(12) . . ?
C26 C27 C31 120.82(13) . . ?
C27 C28 C29 121.64(12) . . ?
C27 C28 H28 119.2 . . ?
C29 C28 H28 119.2 . . ?
C30 C29 C28 118.66(12) . . ?
C30 C29 C32 121.37(13) . . ?
C28 C29 C32 119.98(12) . . ?
C29 C30 C25 121.16(12) . . ?
C29 C30 H30 119.4 . . ?
C25 C30 H30 119.4 . . ?
C27 C31 H31A 109.5 . . ?
C27 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C27 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C38 118.72(10) . . ?
C34 C33 C24 122.80(10) . . ?
C38 C33 C24 118.43(10) . . ?
C33 C34 C35 121.23(10) . . ?
C33 C34 H34 119.4 . . ?
C35 C34 H34 119.4 . . ?
C36 C35 C34 118.73(11) . . ?
C36 C35 C39 120.23(11) . . ?
C34 C35 C39 121.04(11) . . ?
C35 C36 C37 121.31(11) . . ?
C35 C36 H36 119.3 . . ?
C37 C36 H36 119.3 . . ?
C38 C37 C36 118.86(11) . . ?
C38 C37 C40 120.59(12) . . ?
C36 C37 C40 120.55(11) . . ?
C37 C38 C33 121.15(11) . . ?
C37 C38 H38 119.4 . . ?
C33 C38 H38 119.4 . . ?
C35 C39 H39A 109.5 . . ?
C35 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C35 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?

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
O1' H1' N1 0.85(2) 1.97(2) 2.6964(13) 144.0(18) .
N1 H1AA O2' 0.907(19) 2.075(19) 2.7636(14) 131.8(15) .
O2' H2' O1' 0.86(2) 2.16(2) 2.9438(12) 152.7(17) 2_656

_refine_diff_density_max         0.432
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.064

