 
data_1_sq
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          
'C78 H84 N4' 
_chemical_formula_sum
 'C78 H84 N4' 
_chemical_formula_weight          1077.49

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       trigonal
_space_group_IT_number            148
_space_group_name_H-M_alt         'R -3'
_space_group_name_Hall            '-R 3'
 
_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'
 '-y, x-y, z'
 '-x+y, -x, z'
 'x+2/3, y+1/3, z+1/3'
 '-y+2/3, x-y+1/3, z+1/3'
 '-x+y+2/3, -x+1/3, z+1/3'
 'x+1/3, y+2/3, z+2/3'
 '-y+1/3, x-y+2/3, z+2/3'
 '-x+y+1/3, -x+2/3, z+2/3'
 '-x, -y, -z'
 'y, -x+y, -z'
 'x-y, x, -z'
 '-x+2/3, -y+1/3, -z+1/3'
 'y+2/3, -x+y+1/3, -z+1/3'
 'x-y+2/3, x+1/3, -z+1/3'
 '-x+1/3, -y+2/3, -z+2/3'
 'y+1/3, -x+y+2/3, -z+2/3'
 'x-y+1/3, x+2/3, -z+2/3'
 
_cell_length_a                    23.201(3)
_cell_length_b                    23.201(3)
_cell_length_c                    21.302(4)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      9930(3)
_cell_formula_units_Z             6
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     8581
_cell_measurement_theta_min       1.3932
_cell_measurement_theta_max       27.4778
 
_exptl_crystal_description        block
_exptl_crystal_colour             colorless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.081          
_exptl_crystal_F_000              3480
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.26
_exptl_crystal_size_mid           0.24
_exptl_crystal_size_min           0.23
_exptl_absorpt_coefficient_mu     0.062
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'multiwire proportional'
_diffrn_measurement_method        'phi and omega scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             26895
_diffrn_reflns_av_unetI/netI      0.0298
_diffrn_reflns_av_R_equivalents   0.0468
_diffrn_reflns_limit_h_min        -30
_diffrn_reflns_limit_h_max        30
_diffrn_reflns_limit_k_min        -28
_diffrn_reflns_limit_k_max        30
_diffrn_reflns_limit_l_min        -27
_diffrn_reflns_limit_l_max        27
_diffrn_reflns_theta_min          1.393
_diffrn_reflns_theta_max          27.486
_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              5042
_reflns_number_gt                 4852
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_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)+(0.1477P)²+18.2787P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          5053
_refine_ls_number_parameters      293
_refine_ls_number_restraints      636
_refine_ls_R_factor_all           0.1144
_refine_ls_R_factor_gt            0.1075
_refine_ls_wR_factor_ref          0.3111
_refine_ls_wR_factor_gt           0.2998
_refine_ls_goodness_of_fit_ref    1.242
_refine_ls_restrained_S_all       1.228
_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 0.000000 0.000000 0.40552(18) 0.0336(8) Uani 1 3 d S TU P . .
N2 N 0.18307(11) 0.27607(10) 0.41191(12) 0.0413(6) Uani 1 1 d . U . . .
C1 C 0.04664(12) 0.06922(12) 0.40646(11) 0.0322(5) Uani 1 1 d . U . . .
C2' C 0.10777(11) 0.09443(11) 0.43802(11) 0.0301(5) Uani 1 1 d . U . . .
H2' H 0.118257 0.065310 0.458210 0.036 Uiso 1 1 calc R U . . .
C3' C 0.15245(12) 0.16206(12) 0.43933(12) 0.0335(5) Uani 1 1 d . U . . .
H3' H 0.193213 0.177998 0.459451 0.040 Uiso 1 1 calc R U . . .
C4' C 0.13682(13) 0.20638(12) 0.41076(13) 0.0366(6) Uani 1 1 d . U . . .
C5' C 0.07663(14) 0.18216(14) 0.38008(14) 0.0419(6) Uani 1 1 d . U . . .
H5' H 0.065694 0.211548 0.361145 0.050 Uiso 1 1 calc R U . . .
C6 C 0.03250(13) 0.11431(13) 0.37739(13) 0.0381(6) Uani 1 1 d . U . . .
H6 H -0.007370 0.098641 0.355702 0.046 Uiso 1 1 calc R U . . .
C7 C 0.24796(13) 0.30619(12) 0.38882(13) 0.0379(6) Uani 1 1 d . U . . .
C8 C 0.28078(14) 0.27758(13) 0.35999(15) 0.0448(7) Uani 1 1 d . U . . .
H8 H 0.261889 0.231589 0.357912 0.054 Uiso 1 1 calc R U . . .
C9 C 0.34307(15) 0.31977(14) 0.33411(16) 0.0496(7) Uani 1 1 d . U . . .
H9 H 0.365312 0.301049 0.313877 0.059 Uiso 1 1 calc R U . . .
C10 C 0.37363(14) 0.38906(14) 0.33724(16) 0.0465(7) Uani 1 1 d . U . . .
C11 C 0.34074(14) 0.41637(12) 0.36954(14) 0.0428(6) Uani 1 1 d . U . . .
H11 H 0.361144 0.462289 0.374306 0.051 Uiso 1 1 calc R U . . .
C12 C 0.27753(14) 0.37567(12) 0.39484(13) 0.0391(6) Uani 1 1 d . U . . .
C13 C 0.22758(15) 0.38801(13) 0.42220(13) 0.0427(6) Uani 1 1 d . U . . .
C14 C 0.22690(19) 0.44614(15) 0.43874(15) 0.0539(8) Uani 1 1 d . U . . .
H14 H 0.265174 0.487361 0.433804 0.065 Uiso 1 1 calc R U . . .
C15 C 0.1694(2) 0.44260(18) 0.46248(16) 0.0641(10) Uani 1 1 d . U . . .
C16 C 0.1132(2) 0.37966(19) 0.46914(18) 0.0674(11) Uani 1 1 d . U . . .
H16 H 0.074416 0.376834 0.484592 0.081 Uiso 1 1 calc R U . . .
C17 C 0.11234(18) 0.32141(17) 0.45401(17) 0.0576(9) Uani 1 1 d . U . . .
H17 H 0.074100 0.280290 0.459535 0.069 Uiso 1 1 calc R U . . .
C18 C 0.16998(15) 0.32598(13) 0.43037(13) 0.0427(6) Uani 1 1 d . U . . .
C19 C 0.43977(15) 0.43437(17) 0.30310(18) 0.0570(8) Uani 1 1 d . U . . .
C20 C 0.4628(3) 0.3960(3) 0.2642(3) 0.117(2) Uani 1 1 d . U . . .
H20A H 0.502610 0.426378 0.242046 0.176 Uiso 1 1 calc R U . . .
H20B H 0.428742 0.368800 0.234567 0.176 Uiso 1 1 calc R U . . .
H20C H 0.471795 0.368139 0.290985 0.176 Uiso 1 1 calc R U . . .
C21 C 0.4926(2) 0.4738(3) 0.3503(3) 0.126(2) Uani 1 1 d . U . . .
H21A H 0.532469 0.505534 0.329113 0.190 Uiso 1 1 calc R U . . .
H21B H 0.501458 0.444451 0.374899 0.190 Uiso 1 1 calc R U . . .
H21C H 0.477713 0.496903 0.377401 0.190 Uiso 1 1 calc R U . . .
C22 C 0.4318(3) 0.4836(3) 0.2620(3) 0.1022(16) Uani 1 1 d . U . . .
H22A H 0.472788 0.511742 0.240477 0.153 Uiso 1 1 calc R U . . .
H22B H 0.420431 0.510439 0.287838 0.153 Uiso 1 1 calc R U . . .
H22C H 0.397024 0.459759 0.231923 0.153 Uiso 1 1 calc R U . . .
C2_1 C 0.1858(9) 0.5138(11) 0.4859(10) 0.067(4) Uani 0.264(8) 1 d D U P A 2
C3_1 C 0.2531(9) 0.5769(7) 0.4722(10) 0.093(6) Uani 0.264(8) 1 d D U P A 2
H3A_1 H 0.245990 0.613524 0.463867 0.139 Uiso 0.264(8) 1 calc R U P A 2
H3B_1 H 0.273371 0.569264 0.436205 0.139 Uiso 0.264(8) 1 calc R U P A 2
H3C_1 H 0.281885 0.587102 0.507849 0.139 Uiso 0.264(8) 1 calc R U P A 2
C4_1 C 0.1798(12) 0.5137(12) 0.5569(9) 0.079(5) Uani 0.264(8) 1 d D U P A 2
H4A_1 H 0.166969 0.545518 0.569246 0.118 Uiso 0.264(8) 1 calc R U P A 2
H4B_1 H 0.221827 0.525260 0.575661 0.118 Uiso 0.264(8) 1 calc R U P A 2
H4C_1 H 0.146653 0.470136 0.570811 0.118 Uiso 0.264(8) 1 calc R U P A 2
C5_1 C 0.1309(11) 0.5220(11) 0.4560(12) 0.105(6) Uani 0.264(8) 1 d D U P A 2
H5A_1 H 0.108209 0.532370 0.487887 0.157 Uiso 0.264(8) 1 calc R U P A 2
H5B_1 H 0.099787 0.481331 0.435430 0.157 Uiso 0.264(8) 1 calc R U P A 2
H5C_1 H 0.149827 0.557436 0.425810 0.157 Uiso 0.264(8) 1 calc R U P A 2
C23_1 C 0.1624(4) 0.5036(4) 0.4780(4) 0.0669(17) Uani 0.736(8) 1 d . U P A 1
C24_1 C 0.1923(4) 0.5542(3) 0.4240(3) 0.084(2) Uani 0.736(8) 1 d . U P A 1
H24A_1 H 0.192855 0.594469 0.435455 0.126 Uiso 0.736(8) 1 calc R U P A 1
H24B_1 H 0.165851 0.535911 0.386884 0.126 Uiso 0.736(8) 1 calc R U P A 1
H24C_1 H 0.236984 0.563771 0.415933 0.126 Uiso 0.736(8) 1 calc R U P A 1
C25_1 C 0.0911(4) 0.4882(4) 0.4890(4) 0.090(2) Uani 0.736(8) 1 d . U P A 1
H25A_1 H 0.090584 0.529125 0.493829 0.134 Uiso 0.736(8) 1 calc R U P A 1
H25B_1 H 0.073846 0.461896 0.526340 0.134 Uiso 0.736(8) 1 calc R U P A 1
H25C_1 H 0.063981 0.464050 0.453746 0.134 Uiso 0.736(8) 1 calc R U P A 1
C26_1 C 0.2039(6) 0.5334(5) 0.5357(4) 0.110(3) Uani 0.736(8) 1 d . U P A 1
H26A_1 H 0.201648 0.571969 0.548086 0.165 Uiso 0.736(8) 1 calc R U P A 1
H26B_1 H 0.249274 0.545946 0.526832 0.165 Uiso 0.736(8) 1 calc R U P A 1
H26C_1 H 0.187368 0.501251 0.569051 0.165 Uiso 0.736(8) 1 calc R U P A 1
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
N1 C1 1.419(2) . ?
N1 C1 1.419(2) 2 ?
N1 C1 1.419(2) 3 ?
N2 C18 1.393(3) . ?
N2 C7 1.394(3) . ?
N2 C4' 1.425(3) . ?
C1 C6 1.389(3) . ?
C1 C2' 1.406(3) . ?
C2' C3' 1.382(3) . ?
C3' C4' 1.390(3) . ?
C4' C5' 1.382(4) . ?
C5' C6 1.385(4) . ?
C7 C8 1.380(4) . ?
C7 C12 1.407(3) . ?
C8 C9 1.391(4) . ?
C9 C10 1.397(4) . ?
C10 C11 1.393(4) . ?
C10 C19 1.541(4) . ?
C11 C12 1.396(4) . ?
C12 C13 1.448(4) . ?
C13 C18 1.401(4) . ?
C13 C14 1.402(4) . ?
C14 C15 1.391(5) . ?
C15 C16 1.395(6) . ?
C15 C23_1 1.539(8) . ?
C15 C2_1 1.58(2) . ?
C16 C17 1.379(5) . ?
C17 C18 1.383(4) . ?
C19 C21 1.493(6) . ?
C19 C20 1.497(6) . ?
C19 C22 1.522(5) . ?
C2_1 C5_1 1.519(17) . ?
C2_1 C4_1 1.520(18) . ?
C2_1 C3_1 1.543(17) . ?
C23_1 C26_1 1.499(12) . ?
C23_1 C25_1 1.526(10) . ?
C23_1 C24_1 1.540(9) . ?
 
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 C1 119.978(10) . 2 ?
C1 N1 C1 119.982(10) . 3 ?
C1 N1 C1 119.980(10) 2 3 ?
C18 N2 C7 108.2(2) . . ?
C18 N2 C4' 126.5(2) . . ?
C7 N2 C4' 125.1(2) . . ?
C6 C1 C2' 118.0(2) . . ?
C6 C1 N1 120.8(2) . . ?
C2' C1 N1 121.2(2) . . ?
C3' C2' C1 120.7(2) . . ?
C2' C3' C4' 120.4(2) . . ?
C5' C4' C3' 119.4(2) . . ?
C5' C4' N2 120.3(2) . . ?
C3' C4' N2 120.3(2) . . ?
C4' C5' C6 120.3(2) . . ?
C5' C6 C1 121.3(2) . . ?
C8 C7 N2 129.3(2) . . ?
C8 C7 C12 121.4(2) . . ?
N2 C7 C12 109.1(2) . . ?
C7 C8 C9 117.8(2) . . ?
C8 C9 C10 122.8(3) . . ?
C11 C10 C9 117.9(3) . . ?
C11 C10 C19 120.5(3) . . ?
C9 C10 C19 121.5(3) . . ?
C10 C11 C12 120.8(2) . . ?
C11 C12 C7 119.1(2) . . ?
C11 C12 C13 134.1(2) . . ?
C7 C12 C13 106.5(2) . . ?
C18 C13 C14 119.5(3) . . ?
C18 C13 C12 107.1(2) . . ?
C14 C13 C12 133.4(3) . . ?
C15 C14 C13 120.4(3) . . ?
C14 C15 C16 117.7(3) . . ?
C14 C15 C23_1 124.3(4) . . ?
C16 C15 C23_1 117.9(4) . . ?
C14 C15 C2_1 109.3(7) . . ?
C16 C15 C2_1 132.3(7) . . ?
C17 C16 C15 123.4(3) . . ?
C16 C17 C18 118.0(3) . . ?
C17 C18 N2 130.1(3) . . ?
C17 C18 C13 120.9(3) . . ?
N2 C18 C13 109.0(2) . . ?
C21 C19 C20 108.1(5) . . ?
C21 C19 C22 107.3(4) . . ?
C20 C19 C22 110.0(4) . . ?
C21 C19 C10 109.4(3) . . ?
C20 C19 C10 112.6(3) . . ?
C22 C19 C10 109.2(3) . . ?
C5_1 C2_1 C4_1 109.6(18) . . ?
C5_1 C2_1 C3_1 108.5(17) . . ?
C4_1 C2_1 C3_1 103.9(16) . . ?
C5_1 C2_1 C15 102.7(14) . . ?
C4_1 C2_1 C15 109.7(15) . . ?
C3_1 C2_1 C15 122.2(14) . . ?
C26_1 C23_1 C25_1 110.7(8) . . ?
C26_1 C23_1 C15 105.2(6) . . ?
C25_1 C23_1 C15 114.8(6) . . ?
C26_1 C23_1 C24_1 108.7(7) . . ?
C25_1 C23_1 C24_1 108.4(6) . . ?
C15 C23_1 C24_1 109.0(5) . . ?
 
_refine_diff_density_max    0.429
_refine_diff_density_min   -0.429
_refine_diff_density_rms    0.103




