# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2021
#######################################################################
#
# 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.
#
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data_shelx
_database_code_depnum_ccdc_archive 'CCDC 2031638'
loop_
_audit_author_name
_audit_author_address
'Rik Rani koner'
;IIT Mandi
India
;
_audit_update_record
;
2020-12-16 deposited with the CCDC. 2020-12-21 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014/6
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C20 H26 N4 O3'
_chemical_formula_weight 370.45
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system orthorhombic
_space_group_IT_number 18
_space_group_name_H-M_alt 'P 21 21 2'
_space_group_name_Hall 'P 2 2ab'
_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'
_cell_length_a 8.3715(6)
_cell_length_b 33.178(3)
_cell_length_c 7.1858(4)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 1995.9(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 150(2)
_cell_measurement_reflns_used 1331
_cell_measurement_theta_min 5.3180
_cell_measurement_theta_max 66.0560
_exptl_crystal_description Triangle
_exptl_crystal_colour colorless
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.233
_exptl_crystal_F_000 792
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.320
_exptl_crystal_size_mid 0.210
_exptl_crystal_size_min 0.120
_exptl_absorpt_coefficient_mu 0.685
_shelx_estimated_absorpt_T_min 0.811
_shelx_estimated_absorpt_T_max 0.922
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.36324
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_process_details SADABS
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 150(2)
_diffrn_radiation_wavelength 1.54184
_diffrn_radiation_type CuK\a
_diffrn_source 'SuperNova (Cu) X-ray Source'
_diffrn_measurement_device_type 'four-circle diffractometer'
_diffrn_measurement_method ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 2470
_diffrn_reflns_av_unetI/netI 0.0543
_diffrn_reflns_av_R_equivalents 0.0443
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_k_min -30
_diffrn_reflns_limit_k_max 39
_diffrn_reflns_limit_l_min -5
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_theta_min 6.159
_diffrn_reflns_theta_max 66.904
_diffrn_reflns_theta_full 67.684
_diffrn_measured_fraction_theta_max 0.649
_diffrn_measured_fraction_theta_full 0.640
_diffrn_reflns_Laue_measured_fraction_max 0.649
_diffrn_reflns_Laue_measured_fraction_full 0.640
_diffrn_reflns_point_group_measured_fraction_max 0.510
_diffrn_reflns_point_group_measured_fraction_full 0.502
_reflns_number_total 1811
_reflns_number_gt 1541
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.338
_reflns_Friedel_fraction_max 0.311
_reflns_Friedel_fraction_full 0.306
_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 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution 'SIR97 (Giacovazzo et al, 1999)'
_computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics 'Mercury CSD 3.5.1, 2008'
_computing_publication_material 'WinGX publication routines (Farrugia, 1999)'
_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/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens mixed
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_abs_structure_details
;
Flack x determined using 356 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.3(4)
_chemical_absolute_configuration unk
_refine_ls_number_reflns 1811
_refine_ls_number_parameters 223
_refine_ls_number_restraints 42
_refine_ls_R_factor_all 0.1351
_refine_ls_R_factor_gt 0.1243
_refine_ls_wR_factor_ref 0.3646
_refine_ls_wR_factor_gt 0.3434
_refine_ls_goodness_of_fit_ref 1.520
_refine_ls_restrained_S_all 1.501
_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
O2 O -0.6129(8) -0.4485(2) -0.0386(10) 0.0441(16) Uani 1 1 d . . . . .
O1 O -0.8023(9) -0.4285(2) -0.2365(10) 0.0451(17) Uani 1 1 d . . . . .
O3 O -0.3027(10) -0.4742(3) -0.9490(12) 0.058(2) Uani 1 1 d G . . . .
N2 N 0.0124(10) -0.4477(2) -0.8797(11) 0.0403(18) Uani 1 1 d . . . . .
H2A H -0.0859 -0.4570 -0.8834 0.048 Uiso 1 1 calc R U . . .
H2B H 0.0669 -0.4446 -0.9834 0.048 Uiso 1 1 calc R U . . .
N4 N -0.5912(9) -0.3808(2) -0.4298(11) 0.0356(17) Uani 1 1 d . . . . .
H4 H -0.5901 -0.3846 -0.5510 0.043 Uiso 1 1 calc R U . . .
N3 N 0.0052(10) -0.4419(2) -0.5600(11) 0.0415(19) Uani 1 1 d . . . . .
H3 H 0.0588 -0.4341 -0.4609 0.050 Uiso 1 1 calc R U . . .
N1 N 0.2284(10) -0.4236(3) -0.7239(13) 0.046(2) Uani 1 1 d . . . . .
H1A H 0.2793 -0.4164 -0.6220 0.055 Uiso 1 1 calc R U . . .
H1B H 0.2756 -0.4214 -0.8329 0.055 Uiso 1 1 calc R U . . .
C1 C 0.0801(10) -0.4379(3) -0.7132(14) 0.0338(19) Uani 1 1 d . . . . .
C4 C -0.4274(10) -0.4422(3) -0.3952(12) 0.038(2) Uani 1 1 d . . . . .
H4A H -0.4088 -0.4647 -0.3069 0.045 Uiso 1 1 calc R U . . .
H4B H -0.4868 -0.4530 -0.5035 0.045 Uiso 1 1 calc R U . . .
C6 C -0.6630(11) -0.4301(3) -0.1845(13) 0.037(2) Uani 1 1 d . . . . .
C5 C -0.5256(11) -0.4092(3) -0.3005(12) 0.0370(19) Uani 1 1 d . . . . .
H5 H -0.4544 -0.3943 -0.2123 0.044 Uiso 1 1 calc R U . . .
C2 C -0.1520(12) -0.4569(3) -0.5221(13) 0.038(2) Uani 1 1 d . . . . .
H2C H -0.1446 -0.4779 -0.4245 0.046 Uiso 1 1 calc R U . . .
H2D H -0.1943 -0.4698 -0.6361 0.046 Uiso 1 1 calc R U . . .
C3 C -0.2676(12) -0.4250(4) -0.4594(16) 0.050(3) Uani 1 1 d . . . . .
H3A H -0.2867 -0.4061 -0.5634 0.060 Uiso 1 1 calc R U . . .
H3B H -0.2192 -0.4096 -0.3558 0.060 Uiso 1 1 calc R U . . .
C7 C -0.6597(15) -0.3450(4) -0.3437(17) 0.056(3) Uani 1 1 d . . . . .
H7A H -0.5885 -0.3354 -0.2431 0.067 Uiso 1 1 calc R U . . .
H7B H -0.7645 -0.3518 -0.2880 0.067 Uiso 1 1 calc R U . . .
C8 C -0.6823(13) -0.3096(2) -0.4997(12) 0.065(3) Uani 1 1 d G . . . .
C9 C -0.6204(13) -0.2707(3) -0.4955(14) 0.115(7) Uani 1 1 d G U . . .
H9 H -0.5538 -0.2625 -0.3954 0.138 Uiso 1 1 calc R U . . .
C10 C -0.6559(14) -0.2438(2) -0.6380(15) 0.059(3) Uani 1 1 d G . . . .
C18 C -0.7533(17) -0.2558(3) -0.7845(14) 0.116(7) Uani 1 1 d G U . . .
C19 C -0.8153(16) -0.2947(3) -0.7887(13) 0.106(6) Uani 1 1 d G . . . .
H19 H -0.8818 -0.3028 -0.8889 0.127 Uiso 1 1 calc R U . . .
C20 C -0.7798(12) -0.3216(2) -0.6463(13) 0.063(3) Uani 1 1 d G . . . .
H20 H -0.8221 -0.3481 -0.6491 0.076 Uiso 1 1 calc R U . . .
C12 C -0.6556(16) -0.1865(3) -0.8230(14) 0.065(3) Uani 1 1 d G U . . .
C13 C -0.6493(16) -0.1493(3) -0.9121(16) 0.086(4) Uani 1 1 d G U . . .
H13 H -0.5899 -0.1278 -0.8588 0.103 Uiso 1 1 calc R U . . .
C14 C -0.7300(19) -0.1436(3) -1.0791(17) 0.101(6) Uani 1 1 d G U . . .
H14 H -0.7257 -0.1182 -1.1399 0.121 Uiso 1 1 calc R U . . .
C15 C -0.8169(18) -0.1750(4) -1.1570(15) 0.093(5) Uani 1 1 d G . . . .
H15 H -0.8721 -0.1711 -1.2712 0.111 Uiso 1 1 calc R U . . .
C16 C -0.823(2) -0.2122(4) -1.0680(19) 0.110(6) Uani 1 1 d G U . . .
H16 H -0.8827 -0.2337 -1.1213 0.132 Uiso 1 1 calc R U . . .
C17 C -0.743(2) -0.2179(3) -0.9010(19) 0.148(10) Uani 1 1 d G U . . .
C11 C -0.586(3) -0.2017(6) -0.648(3) 0.091(5) Uani 1 1 d . . . . .
H11A H -0.6185 -0.1851 -0.5401 0.109 Uiso 1 1 calc R U . . .
H11B H -0.4674 -0.2025 -0.6546 0.109 Uiso 1 1 calc R U . . .
H3C H -0.3338 -0.4979 -0.9637 0.136 Uiso 1 1 d R U . . .
H3D H -0.3848 -0.4591 -0.9343 0.136 Uiso 1 1 d R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O2 0.035(3) 0.055(4) 0.042(3) 0.006(3) 0.001(3) 0.005(3)
O1 0.040(4) 0.050(4) 0.045(3) 0.002(3) -0.003(3) -0.002(3)
O3 0.050(4) 0.056(4) 0.066(4) 0.004(4) -0.013(4) -0.004(3)
N2 0.036(4) 0.046(4) 0.039(3) 0.003(3) 0.003(3) -0.004(3)
N4 0.026(3) 0.040(4) 0.041(4) 0.000(3) 0.001(3) -0.001(3)
N3 0.034(4) 0.047(4) 0.044(4) -0.005(3) 0.000(3) 0.003(3)
N1 0.035(4) 0.055(5) 0.047(4) -0.011(4) 0.002(4) -0.008(3)
C1 0.026(4) 0.030(4) 0.045(4) -0.007(4) -0.003(3) 0.009(3)
C4 0.026(4) 0.052(6) 0.034(3) -0.003(4) 0.001(4) -0.002(4)
C6 0.031(4) 0.041(5) 0.041(4) 0.000(4) -0.003(4) 0.006(4)
C5 0.034(4) 0.043(5) 0.034(3) 0.003(4) -0.002(4) 0.003(4)
C2 0.038(4) 0.036(4) 0.040(4) 0.001(4) 0.005(4) 0.001(4)
C3 0.032(5) 0.068(7) 0.050(5) 0.002(5) -0.001(4) 0.003(5)
C7 0.050(6) 0.060(6) 0.057(5) -0.002(6) -0.006(5) 0.006(5)
C8 0.061(7) 0.044(6) 0.090(8) -0.006(7) 0.013(7) -0.005(5)
C9 0.115(7) 0.115(7) 0.115(7) -0.0003(13) 0.0000(13) 0.0000(13)
C10 0.060(7) 0.048(6) 0.070(7) -0.009(5) 0.020(6) 0.000(5)
C18 0.116(7) 0.116(7) 0.116(7) -0.0004(13) -0.0003(13) 0.0001(13)
C19 0.101(14) 0.126(16) 0.091(11) 0.017(12) 0.002(12) 0.015(12)
C20 0.068(7) 0.059(7) 0.062(6) -0.001(6) 0.009(7) 0.022(6)
C12 0.065(3) 0.066(3) 0.065(3) 0.0003(12) 0.0001(12) 0.0002(12)
C13 0.085(4) 0.086(4) 0.086(4) -0.0001(13) 0.0002(13) 0.0001(13)
C14 0.101(6) 0.101(6) 0.101(6) -0.0001(13) 0.0006(13) -0.0001(13)
C15 0.104(13) 0.087(11) 0.088(10) 0.025(10) 0.020(11) 0.017(10)
C16 0.109(6) 0.110(6) 0.110(6) -0.0003(13) 0.0001(13) -0.0003(13)
C17 0.148(10) 0.148(10) 0.148(10) 0.0002(13) 0.0003(13) 0.0002(13)
C11 0.097(12) 0.086(11) 0.089(10) 0.017(9) 0.013(11) 0.009(9)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2 C6 1.284(12) . ?
O1 C6 1.226(12) . ?
O3 H3C 0.8366 . ?
O3 H3D 0.8568 . ?
N2 C1 1.363(13) . ?
N2 H2A 0.8800 . ?
N2 H2B 0.8800 . ?
N4 C5 1.433(12) . ?
N4 C7 1.455(15) . ?
N4 H4 0.8800 . ?
N3 C1 1.274(14) . ?
N3 C2 1.433(13) . ?
N3 H3 0.8800 . ?
N1 C1 1.331(12) . ?
N1 H1A 0.8800 . ?
N1 H1B 0.8800 . ?
C4 C3 1.526(13) . ?
C4 C5 1.530(14) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C6 C5 1.580(14) . ?
C5 H5 1.0000 . ?
C2 C3 1.503(15) . ?
C2 H2C 0.9900 . ?
C2 H2D 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C7 C8 1.636(14) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.3900 . ?
C8 C20 1.3900 . ?
C9 C10 1.3900 . ?
C9 H9 0.9500 . ?
C10 C18 1.3900 . ?
C10 C11 1.52(2) . ?
C18 C19 1.3900 . ?
C18 C17 1.513(11) . ?
C19 C20 1.3900 . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C12 C13 1.3900 . ?
C12 C17 1.3900 . ?
C12 C11 1.48(2) . ?
C13 C14 1.3900 . ?
C13 H13 0.9500 . ?
C14 C15 1.3900 . ?
C14 H14 0.9500 . ?
C15 C16 1.3900 . ?
C15 H15 0.9500 . ?
C16 C17 1.3900 . ?
C16 H16 0.9500 . ?
C11 H11A 0.9900 . ?
C11 H11B 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
H3C O3 H3D 108.3 . . ?
C1 N2 H2A 120.0 . . ?
C1 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C5 N4 C7 114.3(8) . . ?
C5 N4 H4 122.9 . . ?
C7 N4 H4 122.9 . . ?
C1 N3 C2 130.7(9) . . ?
C1 N3 H3 114.6 . . ?
C2 N3 H3 114.6 . . ?
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
N3 C1 N1 123.1(9) . . ?
N3 C1 N2 121.9(8) . . ?
N1 C1 N2 115.0(9) . . ?
C3 C4 C5 109.7(9) . . ?
C3 C4 H4A 109.7 . . ?
C5 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
C5 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
O1 C6 O2 125.4(9) . . ?
O1 C6 C5 120.8(8) . . ?
O2 C6 C5 113.7(8) . . ?
N4 C5 C4 112.9(7) . . ?
N4 C5 C6 110.6(8) . . ?
C4 C5 C6 108.1(7) . . ?
N4 C5 H5 108.4 . . ?
C4 C5 H5 108.4 . . ?
C6 C5 H5 108.4 . . ?
N3 C2 C3 113.8(9) . . ?
N3 C2 H2C 108.8 . . ?
C3 C2 H2C 108.8 . . ?
N3 C2 H2D 108.8 . . ?
C3 C2 H2D 108.8 . . ?
H2C C2 H2D 107.7 . . ?
C2 C3 C4 113.1(10) . . ?
C2 C3 H3A 109.0 . . ?
C4 C3 H3A 109.0 . . ?
C2 C3 H3B 109.0 . . ?
C4 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
N4 C7 C8 109.9(9) . . ?
N4 C7 H7A 109.7 . . ?
C8 C7 H7A 109.7 . . ?
N4 C7 H7B 109.7 . . ?
C8 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
C9 C8 C20 120.0 . . ?
C9 C8 C7 127.5(7) . . ?
C20 C8 C7 112.5(7) . . ?
C8 C9 C10 120.0 . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C18 C10 C9 120.0 . . ?
C18 C10 C11 117.0(10) . . ?
C9 C10 C11 122.9(10) . . ?
C10 C18 C19 120.0 . . ?
C10 C18 C17 98.4(9) . . ?
C19 C18 C17 141.4(9) . . ?
C20 C19 C18 120.0 . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C19 C20 C8 120.0 . . ?
C19 C20 H20 120.0 . . ?
C8 C20 H20 120.0 . . ?
C13 C12 C17 120.0 . . ?
C13 C12 C11 132.9(11) . . ?
C17 C12 C11 107.1(11) . . ?
C14 C13 C12 120.0 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C15 C14 C13 120.0 . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C16 C15 C14 120.0 . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C16 C17 120.0 . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 C12 120.0 . . ?
C16 C17 C18 124.2(9) . . ?
C12 C17 C18 115.6(9) . . ?
C12 C11 C10 101.7(15) . . ?
C12 C11 H11A 111.4 . . ?
C10 C11 H11A 111.4 . . ?
C12 C11 H11B 111.4 . . ?
C10 C11 H11B 111.4 . . ?
H11A C11 H11B 109.3 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N3 C1 N1 -179.2(9) . . . . ?
C2 N3 C1 N2 1.5(15) . . . . ?
C7 N4 C5 C4 -169.2(8) . . . . ?
C7 N4 C5 C6 69.5(10) . . . . ?
C3 C4 C5 N4 74.1(10) . . . . ?
C3 C4 C5 C6 -163.2(7) . . . . ?
O1 C6 C5 N4 16.5(12) . . . . ?
O2 C6 C5 N4 -164.7(8) . . . . ?
O1 C6 C5 C4 -107.6(10) . . . . ?
O2 C6 C5 C4 71.3(10) . . . . ?
C1 N3 C2 C3 -110.2(11) . . . . ?
N3 C2 C3 C4 -172.4(8) . . . . ?
C5 C4 C3 C2 169.5(8) . . . . ?
C5 N4 C7 C8 163.5(8) . . . . ?
N4 C7 C8 C9 -123.4(8) . . . . ?
N4 C7 C8 C20 58.5(11) . . . . ?
C20 C8 C9 C10 0.0 . . . . ?
C7 C8 C9 C10 -177.9(11) . . . . ?
C8 C9 C10 C18 0.0 . . . . ?
C8 C9 C10 C11 -176.6(13) . . . . ?
C9 C10 C18 C19 0.0 . . . . ?
C11 C10 C18 C19 176.8(12) . . . . ?
C9 C10 C18 C17 -176.0(11) . . . . ?
C11 C10 C18 C17 0.8(14) . . . . ?
C10 C18 C19 C20 0.0 . . . . ?
C17 C18 C19 C20 173.7(18) . . . . ?
C18 C19 C20 C8 0.0 . . . . ?
C9 C8 C20 C19 0.0 . . . . ?
C7 C8 C20 C19 178.2(10) . . . . ?
C17 C12 C13 C14 0.0 . . . . ?
C11 C12 C13 C14 -179.6(16) . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C13 C14 C15 C16 0.0 . . . . ?
C14 C15 C16 C17 0.0 . . . . ?
C15 C16 C17 C12 0.0 . . . . ?
C15 C16 C17 C18 174.4(16) . . . . ?
C13 C12 C17 C16 0.0 . . . . ?
C11 C12 C17 C16 179.7(13) . . . . ?
C13 C12 C17 C18 -174.9(14) . . . . ?
C11 C12 C17 C18 4.9(14) . . . . ?
C10 C18 C17 C16 -178.1(8) . . . . ?
C19 C18 C17 C16 7.4(19) . . . . ?
C10 C18 C17 C12 -3.5(12) . . . . ?
C19 C18 C17 C12 -178.0(9) . . . . ?
C13 C12 C11 C10 175.9(11) . . . . ?
C17 C12 C11 C10 -3.8(14) . . . . ?
C18 C10 C11 C12 1.8(16) . . . . ?
C9 C10 C11 C12 178.5(9) . . . . ?
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
N2 H2A O3 0.88 1.96 2.825(12) 167.4 .
N2 H2B O1 0.88 2.19 3.064(10) 172.5 1_654
N4 H4 N1 0.88 2.35 2.961(11) 126.6 1_455
N1 H1A N4 0.88 2.12 2.961(11) 160.4 1_655
N1 H1B O2 0.88 1.97 2.750(12) 147.4 1_654
C2 H2D O3 0.99 2.43 3.366(13) 157.7 .
C7 H7B O1 0.99 2.59 3.112(15) 112.8 .
O3 H3C O2 0.84 1.91 2.736(12) 170.0 2_444
O3 H3D O2 0.86 2.08 2.808(11) 142.3 1_554
N2 H2A O3 0.88 1.96 2.825(12) 167.4 .
N2 H2B O1 0.88 2.19 3.064(10) 172.5 1_654
N4 H4 N1 0.88 2.35 2.961(11) 126.6 1_455
N1 H1A N4 0.88 2.12 2.961(11) 160.4 1_655
N1 H1B O2 0.88 1.97 2.750(12) 147.4 1_654
C2 H2D O3 0.99 2.43 3.366(13) 157.7 .
C7 H7B O1 0.99 2.59 3.112(15) 112.8 .
O3 H3C O2 0.84 1.91 2.736(12) 170.0 2_444
O3 H3D O2 0.86 2.08 2.808(11) 142.3 1_554
_refine_diff_density_max 0.608
_refine_diff_density_min -0.344
_refine_diff_density_rms 0.092
_shelxl_version_number 2014/6
_shelx_res_file
;
TITL fa_a_lt_cu_a.res in P2(1)2(1)2
CELL 1.54184 8.3715 33.1780 7.1858 90.000 90.000 90.000
ZERR 4.00 0.0006 0.0030 0.0004 0.000 0.000 0.000
LATT -1
SYMM - X, - Y, Z
SYMM 1/2 - X, 1/2 + Y, - Z
SYMM 1/2 + X, 1/2 - Y, - Z
SFAC C H N O
UNIT 80 104 16 12
MERG 2
OMIT 0 0 2
OMIT 8 8 4
OMIT 0 4 0
OMIT 0 4 2
OMIT 2 19 5
OMIT 5 12 5
OMIT 0 22 5
OMIT 8 1 5
OMIT 1 1 0
OMIT 1 29 3
OMIT 2 25 4
OMIT 5 4 6
OMIT 4 33 3
OMIT 4 27 4
OMIT 0 23 5
OMIT 2 4 0
OMIT 0 4 1
OMIT 2 26 4
OMIT 7 3 5
OMIT 3 28 5
OMIT 6 8 6
OMIT 2 7 0
OMIT 2 33 3
OMIT 1 30 3
OMIT 6 12 6
OMIT 6 14 5
OMIT 5 15 5
OMIT 3 11 6
OMIT 8 10 4
OMIT 3 33 3
OMIT 2 3 3
OMIT 7 0 5
OMIT 0 28 3
OMIT 2 30 5
OMIT 5 11 5
OMIT 5 13 4
OMIT 6 10 5
OMIT 1 33 3
OMIT 1 28 4
OMIT -2 3 3
OMIT 5 10 6
OMIT -4 4 7
OMIT 0 35 2
OMIT -1 30 5
OMIT 4 28 4
OMIT 2 28 5
OMIT -1 25 4
OMIT 1 33 4
OMIT 0 10 1
OMIT 0 2 5
OMIT 4 7 0
OMIT 1 30 0
OMIT 1 24 0
OMIT 3 0 4
OMIT 3 27 0
OMIT 4 9 5
OMIT 2 34 4
OMIT 1 25 4
OMIT 7 2 5
OMIT -1 7 3
OMIT 8 0 5
OMIT 8 2 5
OMIT 0 30 4
OMIT -2 27 3
OMIT 0 29 3
OMIT 2 32 0
OMIT 3 30 4
OMIT 0 7 3
OMIT 8 0 2
OMIT 4 14 0
OMIT 2 27 4
OMIT 2 32 3
OMIT 7 19 0
OMIT -1 28 4
OMIT 3 28 4
OMIT 0 26 2
OMIT 5 0 3
OMIT 5 0 1
OMIT 8 8 3
OMIT 1 29 4
OMIT 0 24 2
OMIT -8 8 3
OMIT 7 0 4
OMIT -3 29 3
OMIT 7 5 5
OMIT 6 2 6
OMIT 2 16 0
OMIT 0 8 2
OMIT 4 8 0
OMIT 7 11 5
OMIT -1 27 4
OMIT 5 32 0
OMIT 4 4 2
OMIT 2 30 0
OMIT 0 36 2
OMIT 5 21 0
OMIT -8 8 4
OMIT 4 30 4
OMIT -4 4 2
OMIT 3 29 5
OMIT 0 38 1
OMIT -7 10 1
OMIT 2 23 0
OMIT 3 2 3
OMIT -6 13 3
OMIT -3 2 3
OMIT 2 7 1
OMIT 9 13 2
OMIT 0 26 3
OMIT 4 30 0
OMIT 5 23 0
OMIT 2 28 4
OMIT 1 28 0
OMIT 1 28 5
OMIT -3 24 3
OMIT 0 24 3
OMIT 4 2 1
OMIT -8 8 1
OMIT 4 10 6
OMIT 0 24 5
OMIT 0 36 0
OMIT 0 7 5
OMIT 2 13 0
OMIT 0 16 2
OMIT 5 34 0
OMIT 4 28 0
OMIT -4 2 1
OMIT -3 29 1
OMIT 6 7 5
OMIT 2 29 1
OMIT -2 12 2
OMIT 2 18 1
OMIT 5 1 0
OMIT 0 0 8
OMIT 3 32 0
OMIT -4 7 2
OMIT 2 12 2
OMIT 7 10 1
OMIT 5 6 6
OMIT -1 12 7
OMIT -8 13 3
OMIT -5 2 1
OMIT 3 35 3
OMIT -5 14 1
OMIT 2 36 2
OMIT 0 6 7
OMIT 2 29 5
OMIT -8 7 3
OMIT 9 4 2
OMIT 1 31 0
OMIT 0 18 1
OMIT 4 4 0
OMIT 8 6 0
OMIT -9 8 2
OMIT 0 20 0
OMIT 9 8 2
OMIT -8 9 3
OMIT 8 9 3
OMIT 3 24 3
OMIT 1 31 3
OMIT 9 8 1
OMIT 4 0 7
OMIT -8 22 1
OMIT 8 0 1
OMIT -1 8 6
OMIT 0 27 1
OMIT -9 4 2
OMIT 0 0 4
OMIT 8 13 3
OMIT -5 20 4
OMIT 5 7 5
OMIT -4 13 2
OMIT 0 18 0
OMIT -7 16 5
OMIT 6 1 6
OMIT -3 9 1
OMIT -8 10 3
OMIT 0 3 5
OMIT 1 25 0
OMIT 2 8 1
OMIT 0 6 8
OMIT 9 10 0
OMIT -6 11 3
OMIT 9 6 0
OMIT -2 32 2
OMIT 0 7 4
OMIT -1 26 4
OMIT 0 8 5
OMIT 8 10 3
OMIT -3 18 3
OMIT 8 11 3
OMIT 3 9 1
OMIT -5 17 4
OMIT 7 4 2
OMIT 8 8 1
OMIT 1 38 0
OMIT 3 34 3
OMIT 1 0 4
OMIT 1 27 4
OMIT -1 22 5
OMIT 4 5 0
OMIT 6 29 0
OMIT 0 13 5
OMIT 4 31 0
OMIT -7 4 2
OMIT -4 26 4
OMIT 4 19 1
OMIT 0 13 2
OMIT 0 5 4
OMIT 4 0 2
OMIT -1 29 4
OMIT 2 11 0
OMIT 1 34 0
OMIT -7 12 1
OMIT 5 2 1
OMIT -8 6 2
OMIT 7 21 0
OMIT 9 12 1
OMIT 4 26 4
OMIT 1 4 6
OMIT 8 22 1
OMIT 0 6 3
OMIT -2 32 3
OMIT 2 3 0
OMIT 0 9 4
OMIT -1 17 6
OMIT -3 20 4
OMIT 2 16 1
OMIT -3 6 6
OMIT -5 10 4
OMIT -6 1 6
OMIT 7 12 3
OMIT 1 9 8
OMIT -6 23 1
OMIT -2 16 1
OMIT 0 9 5
OMIT -6 3 1
OMIT 3 29 1
OMIT 9 0 2
OMIT 1 2 0
OMIT 0 27 5
OMIT -9 12 1
OMIT -7 18 4
OMIT -2 3 8
OMIT 3 10 6
OMIT 8 0 3
OMIT 8 6 2
OMIT -6 24 1
OMIT -1 33 3
OMIT 0 2 2
OMIT 0 7 7
OMIT 2 8 0
OMIT 0 34 4
OMIT -5 12 4
OMIT -8 15 3
OMIT -1 10 6
OMIT 1 17 6
OMIT 4 20 1
OMIT 5 28 2
OMIT 2 21 1
OMIT 5 7 0
OMIT 4 1 0
OMIT 8 20 1
OMIT 6 19 0
OMIT 3 4 6
OMIT -4 12 7
OMIT 8 9 4
OMIT 0 11 7
OMIT 5 10 5
OMIT 2 3 8
OMIT 1 8 6
OMIT -2 21 1
OMIT -3 4 6
OMIT 1 19 2
OMIT 7 9 0
OMIT 1 35 1
OMIT 3 36 2
OMIT -8 4 1
OMIT 0 33 2
OMIT 3 31 0
OMIT -1 33 1
OMIT -6 8 6
OMIT 1 19 0
OMIT 2 33 0
OMIT -1 20 4
OMIT -2 28 4
OMIT -9 3 3
OMIT -7 21 4
OMIT 7 19 2
OMIT -8 2 4
OMIT -6 9 2
OMIT -2 11 2
OMIT 1 15 1
OMIT 2 11 2
OMIT 0 16 1
OMIT -4 30 3
OMIT 7 26 2
OMIT -6 13 6
OMIT -8 16 2
OMIT 4 32 2
OMIT -1 9 8
OMIT -1 19 2
OMIT 4 4 5
OMIT -4 16 7
OMIT -5 14 6
OMIT 0 22 6
OMIT -4 9 6
OMIT 2 34 3
OMIT -8 1 5
OMIT 1 20 4
OMIT -2 5 3
OMIT 5 27 1
OMIT -1 23 6
OMIT 6 31 0
OMIT 8 4 1
OMIT 0 36 3
OMIT 9 14 2
OMIT -5 8 6
OMIT 1 17 3
OMIT -2 30 3
OMIT -1 15 1
OMIT 2 14 0
OMIT -3 6 4
OMIT 4 28 1
OMIT 1 36 2
OMIT 9 9 1
OMIT 4 5 2
OMIT -3 29 2
OMIT 4 33 0
OMIT -6 18 5
OMIT 2 31 3
OMIT 6 5 0
OMIT -7 4 4
OMIT -3 5 8
OMIT 9 3 3
OMIT -5 6 7
OMIT 7 8 3
OMIT 8 16 2
OMIT -5 9 2
OMIT 8 2 4
OMIT 1 23 1
OMIT 8 22 0
OMIT 4 10 0
OMIT 1 29 1
OMIT 0 30 2
OMIT 5 26 2
OMIT 0 15 2
OMIT -7 19 2
OMIT 1 33 1
OMIT -2 3 7
OMIT 4 0 0
OMIT -5 13 6
OMIT 3 0 6
OMIT 3 34 1
OMIT 0 19 1
OMIT -2 25 5
OMIT 7 4 4
OMIT 0 16 4
OMIT -2 18 1
OMIT -4 12 3
OMIT 0 20 2
OMIT 0 12 1
OMIT -4 14 5
OMIT 1 26 0
OMIT 0 21 5
OMIT 2 5 3
OMIT -6 9 6
OMIT -8 14 4
OMIT 0 11 5
OMIT 2 10 0
OMIT 0 13 3
OMIT 4 7 6
OMIT -7 19 4
OMIT -2 18 7
OMIT -7 12 3
OMIT -3 19 5
OMIT 5 0 6
OMIT 2 37 0
OMIT -6 4 4
OMIT -4 25 4
OMIT -1 31 4
OMIT -6 2 3
OMIT -4 29 1
OMIT -1 5 3
OMIT -3 31 1
OMIT 0 18 5
OMIT -4 4 1
OMIT -5 17 5
OMIT 0 25 4
OMIT 5 2 4
OMIT 0 8 1
OMIT 8 7 3
OMIT 0 21 3
OMIT 6 22 2
OMIT -6 25 4
OMIT -5 8 5
OMIT 0 37 1
OMIT -8 6 3
OMIT 7 10 0
OMIT -1 29 1
OMIT 1 7 8
OMIT -3 26 5
OMIT -1 35 1
OMIT 0 35 1
OMIT -1 13 1
OMIT 1 20 0
OMIT -4 10 2
OMIT -4 4 5
OMIT -5 29 1
OMIT -3 7 8
OMIT -6 12 3
OMIT -5 2 6
OMIT -2 29 3
OMIT -7 8 3
OMIT 5 25 2
OMIT 2 32 2
OMIT 0 38 0
OMIT 0 32 0
OMIT 1 10 7
OMIT 5 5 1
OMIT 6 5 5
OMIT 0 4 4
OMIT -1 23 1
OMIT 0 20 5
OMIT -6 8 2
OMIT 7 11 3
OMIT -4 3 3
OMIT -3 32 1
OMIT 8 6 3
OMIT -6 14 6
OMIT -4 7 5
OMIT -4 28 1
OMIT -8 18 3
OMIT -1 4 3
OMIT 4 26 0
OMIT 7 9 3
OMIT 3 1 1
OMIT 0 16 0
OMIT -7 11 3
OMIT -4 6 7
OMIT 8 8 2
OMIT -3 20 3
OMIT -7 8 1
OMIT -2 7 1
OMIT -2 34 4
OMIT -3 9 7
OMIT -1 13 3
OMIT 2 1 1
OMIT 2 37 2
OMIT 7 7 0
OMIT -4 8 2
OMIT -1 10 7
OMIT 1 26 5
OMIT -8 8 2
OMIT -3 1 1
OMIT 4 8 6
OMIT 0 37 2
OMIT 4 19 0
OMIT -5 10 6
OMIT 2 14 7
OMIT -5 18 5
OMIT -3 16 5
OMIT 0 34 0
OMIT -6 6 2
OMIT 0 11 4
OMIT 7 23 0
OMIT -4 25 3
OMIT 0 10 2
OMIT 3 32 1
OMIT -5 27 1
OMIT 3 25 3
OMIT -8 9 4
OMIT 4 3 3
OMIT -7 12 4
OMIT -7 25 1
OMIT 2 21 4
OMIT 5 19 0
OMIT 0 5 5
OMIT -5 2 4
OMIT 4 4 1
OMIT -6 10 2
OMIT 7 8 1
OMIT 5 26 0
OMIT -2 9 6
OMIT -7 15 1
OMIT -2 25 4
OMIT 6 7 6
OMIT 4 6 2
OMIT 6 4 5
OMIT 2 0 2
OMIT 9 15 0
OMIT -2 14 7
OMIT -4 5 2
OMIT -1 20 5
OMIT 0 17 2
OMIT 4 3 2
OMIT -4 15 6
OMIT -6 6 6
OMIT -6 7 3
OMIT 5 32 1
OMIT -1 17 3
OMIT -4 3 2
OMIT 7 10 5
OMIT -5 31 1
OMIT 3 35 0
OMIT -3 24 6
OMIT 9 10 2
OMIT -4 14 6
OMIT 2 7 7
OMIT 2 7 5
OMIT 0 2 3
OMIT -4 26 3
OMIT -8 11 3
OMIT 7 11 4
OMIT 2 15 2
OMIT 2 18 7
OMIT 7 15 1
OMIT 7 7 2
OMIT -2 22 3
OMIT -7 13 5
OMIT 8 10 0
OMIT -5 26 3
OMIT 7 9 2
OMIT 3 31 1
OMIT -3 4 2
OMIT 0 35 4
OMIT -2 28 5
OMIT 4 9 0
OMIT -7 11 4
OMIT 0 10 4
OMIT 3 35 1
OMIT 3 4 2
OMIT 4 21 1
OMIT -2 18 5
OMIT -5 28 3
OMIT -2 2 5
OMIT 0 14 2
OMIT -1 30 1
OMIT 8 9 2
OMIT 0 11 1
OMIT -6 1 3
OMIT -7 8 2
OMIT 1 30 1
OMIT -8 9 2
OMIT -3 21 1
OMIT -1 21 7
OMIT -1 19 4
OMIT -1 3 2
OMIT 3 34 0
OMIT -2 1 1
OMIT -7 19 3
OMIT -1 11 2
OMIT 0 6 0
OMIT 4 17 0
OMIT -7 7 2
OMIT 0 23 4
OMIT 3 21 1
OMIT 4 21 0
OMIT -3 34 1
OMIT -1 31 5
OMIT -4 21 3
OMIT 2 7 2
OMIT -8 17 1
OMIT -2 8 1
OMIT 9 5 0
OMIT 7 8 2
OMIT 1 19 4
OMIT 1 27 0
OMIT 8 3 0
OMIT -4 27 5
OMIT -8 11 2
OMIT -3 4 1
OMIT 1 11 2
OMIT 7 18 2
OMIT 3 0 3
OMIT 8 11 2
OMIT 6 1 3
OMIT 5 32 2
OMIT -2 21 4
OMIT -3 2 7
OMIT 9 9 0
OMIT -6 2 5
OMIT -3 8 7
OMIT -1 24 4
OMIT 6 31 1
OMIT -4 6 2
OMIT -8 16 1
OMIT -9 1 2
OMIT -7 18 2
OMIT -5 6 1
OMIT 1 24 4
OMIT 6 25 0
OMIT 3 6 0
OMIT 2 14 2
OMIT 0 14 3
OMIT -3 12 2
OMIT 7 7 3
OMIT 6 12 0
OMIT 3 3 0
OMIT -7 7 3
OMIT -7 5 4
OMIT -5 26 1
OMIT 7 12 4
OMIT 0 25 1
OMIT 5 9 5
OMIT 9 1 2
OMIT 7 2 3
OMIT 4 1 2
OMIT -4 1 2
OMIT -7 2 3
OMIT 1 39 1
OMIT 4 6 1
OMIT -7 9 2
OMIT -3 16 3
OMIT 6 29 2
OMIT 9 5 2
OMIT 4 1 4
OMIT 7 8 5
OMIT 0 28 6
OMIT -7 15 4
OMIT 7 12 2
OMIT -1 36 2
OMIT 8 1 3
OMIT 8 17 1
OMIT -2 7 2
OMIT 6 0 1
OMIT 8 3 2
OMIT -2 11 4
OMIT -7 12 2
OMIT 2 17 0
OMIT -4 1 4
OMIT -2 20 1
OMIT -2 6 3
OMIT 6 24 1
OMIT -9 2 3
OMIT -6 14 5
OMIT -1 30 4
OMIT -6 4 6
OMIT 6 17 0
OMIT 2 20 1
OMIT -8 3 2
OMIT 2 6 3
OMIT 3 6 6
OMIT 0 15 3
OMIT -1 18 4
OMIT -6 11 4
OMIT -7 4 1
OMIT 5 29 1
OMIT 9 14 0
OMIT -7 1 5
OMIT -9 5 2
OMIT 2 9 6
OMIT -4 33 1
OMIT 7 4 1
OMIT -8 1 3
OMIT -3 22 3
OMIT 9 2 3
OMIT 2 22 3
OMIT 8 14 3
OMIT 4 8 5
OMIT 5 7 6
OMIT 5 6 1
OMIT -4 6 1
OMIT 2 9 5
OMIT -5 2 5
OMIT 4 24 0
OMIT -7 3 2
OMIT -7 5 3
OMIT -3 17 1
OMIT 1 3 2
OMIT -2 31 1
OMIT -7 7 5
OMIT -6 25 3
OMIT -1 8 3
OMIT -2 23 3
OMIT -7 23 1
OMIT -6 5 4
OMIT 0 24 1
OMIT 8 18 0
OMIT 4 29 1
OMIT 1 17 0
OMIT 4 5 3
OMIT 8 16 1
OMIT -1 22 3
OMIT -4 26 5
OMIT 2 31 1
OMIT 7 5 3
OMIT 1 27 5
OMIT 1 13 1
OMIT 7 12 1
OMIT 7 0 2
OMIT 8 23 0
OMIT 7 3 2
OMIT 1 9 2
OMIT 6 6 0
OMIT -8 21 1
OMIT 3 6 5
OMIT -2 6 6
OMIT -1 19 1
OMIT 0 25 3
OMIT 2 36 0
OMIT 5 2 5
OMIT -9 6 3
OMIT 5 31 1
OMIT 2 11 5
OMIT -7 18 1
OMIT 6 6 5
OMIT 1 32 3
OMIT -7 9 3
OMIT -2 9 7
OMIT -1 24 1
OMIT 2 8 6
OMIT 1 2 5
OMIT -8 13 1
OMIT -6 27 3
OMIT 0 19 3
OMIT 3 0 8
OMIT -2 7 7
OMIT -7 8 4
OMIT 7 18 1
OMIT -3 14 7
OMIT -4 9 2
OMIT 3 22 3
OMIT 3 29 2
OMIT 0 25 6
OMIT -2 14 2
OMIT 6 12 5
OMIT 0 7 2
OMIT -7 16 4
OMIT 0 8 7
OMIT 9 4 3
OMIT -2 12 6
OMIT -2 24 1
OMIT -1 33 4
OMIT -5 9 4
OMIT 0 8 8
OMIT -5 4 7
OMIT -3 6 5
OMIT 0 13 8
OMIT -1 22 1
OMIT 0 2 1
OMIT 1 19 1
OMIT -2 20 6
OMIT -3 24 4
OMIT 2 2 5
OMIT -5 16 3
OMIT 8 4 0
OMIT -2 14 1
OMIT -3 34 3
OMIT -4 21 4
OMIT -1 20 3
OMIT 5 1 3
OMIT -5 10 5
OMIT -5 7 6
OMIT 0 19 2
OMIT -1 7 7
OMIT -3 5 3
OMIT -5 23 3
OMIT 5 8 0
OMIT 8 13 0
OMIT -4 30 1
OMIT 1 13 3
OMIT -2 20 7
OMIT 3 24 0
OMIT -4 28 3
OMIT -5 19 3
OMIT -4 16 3
OMIT -4 26 2
OMIT 5 0 5
OMIT -5 30 3
OMIT -4 5 1
OMIT 9 6 3
OMIT 1 5 5
OMIT 1 15 2
OMIT 1 7 7
OMIT 3 11 1
OMIT -5 25 1
OMIT 9 12 2
OMIT 1 30 5
OMIT -1 5 5
OMIT 1 0 3
OMIT -6 18 4
OMIT -1 9 2
OMIT -3 3 5
OMIT -1 16 4
OMIT -3 23 2
OMIT -5 15 5
OMIT -4 5 3
OMIT 4 5 1
OMIT 7 13 5
OMIT -8 10 4
OMIT 0 21 6
OMIT 2 17 2
OMIT -3 19 7
OMIT 2 9 1
OMIT 3 0 1
OMIT -5 1 7
OMIT 0 14 1
OMIT 2 7 8
OMIT -8 5 4
OMIT -1 26 3
OMIT -2 23 2
OMIT 7 1 5
OMIT 1 20 3
OMIT -2 10 3
OMIT 0 29 2
OMIT -1 16 6
OMIT -4 19 5
OMIT 0 22 0
OMIT -1 3 8
OMIT 5 30 2
OMIT 9 13 1
OMIT 1 22 1
OMIT 5 0 4
OMIT 2 35 3
OMIT 2 14 1
OMIT -6 12 2
OMIT -6 19 3
OMIT -7 2 2
OMIT -2 17 2
OMIT -3 6 7
OMIT 1 3 8
OMIT -2 13 6
OMIT -3 16 6
OMIT -3 8 4
OMIT 0 10 5
OMIT 1 19 6
OMIT -4 15 5
OMIT -2 2 6
OMIT -1 15 2
OMIT 3 16 2
OMIT 2 10 3
OMIT 5 8 5
OMIT -3 17 4
OMIT -7 24 1
OMIT -3 16 2
OMIT -5 8 2
OMIT 1 16 6
OMIT -6 9 3
OMIT 8 19 1
OMIT -5 1 1
OMIT -4 18 3
OMIT 5 13 6
OMIT 2 2 0
OMIT -2 27 6
OMIT -1 19 6
OMIT -6 9 4
OMIT 2 24 1
OMIT 6 22 0
OMIT 5 11 6
OMIT -6 16 1
OMIT 8 1 2
OMIT -8 1 2
OMIT 0 8 6
OMIT 0 18 3
OMIT 0 33 4
OMIT -4 17 6
OMIT -3 30 1
OMIT 4 29 0
OMIT -3 11 1
OMIT 0 13 7
OMIT -5 24 4
OMIT -4 21 5
OMIT 0 34 1
OMIT -8 4 4
OMIT 1 14 5
OMIT 6 28 0
OMIT -6 6 1
OMIT 7 15 0
OMIT -1 4 2
OMIT 2 14 5
OMIT 4 9 6
OMIT -4 21 6
OMIT 3 9 0
OMIT 6 6 6
OMIT 3 7 0
OMIT -1 1 2
OMIT 8 1 0
OMIT -3 33 3
OMIT 2 0 3
OMIT 1 13 2
OMIT 7 12 5
OMIT 5 14 5
OMIT -6 7 4
OMIT 5 5 0
OMIT 0 31 4
OMIT -6 20 4
OMIT 1 15 0
OMIT 0 4 7
OMIT 4 2 4
OMIT 5 16 0
OMIT -2 34 1
OMIT -6 10 6
OMIT -4 6 6
OMIT -4 28 4
OMIT 5 29 2
OMIT 2 16 3
OMIT -3 13 5
OMIT 8 3 5
OMIT 2 23 2
OMIT -4 12 6
OMIT -2 12 1
OMIT -4 30 4
OMIT -3 9 2
OMIT 3 20 3
OMIT -3 6 1
OMIT -1 23 4
OMIT 0 31 2
OMIT 7 24 1
OMIT -8 14 1
OMIT 2 12 1
OMIT -4 19 4
OMIT 2 5 0
OMIT 1 31 1
OMIT 7 27 1
OMIT -4 27 4
OMIT -4 24 3
OMIT 2 12 4
OMIT 1 4 2
OMIT -4 2 4
OMIT 0 17 3
OMIT 0 10 0
OMIT 1 13 0
OMIT -8 16 3
OMIT 0 1 1
OMIT 1 12 1
OMIT -3 11 2
OMIT 0 2 7
OMIT 1 10 4
OMIT 3 8 0
OMIT 0 3 2
OMIT 0 5 2
OMIT 6 11 5
OMIT -5 4 2
OMIT 9 0 1
OMIT 4 0 6
OMIT 0 34 2
OMIT -1 12 1
OMIT 0 5 3
OMIT -4 10 5
OMIT 7 1 6
OMIT 1 11 8
OMIT -4 1 6
OMIT 9 2 2
OMIT 4 12 0
OMIT 6 16 1
OMIT -2 17 6
OMIT 0 5 8
OMIT 1 22 3
OMIT 4 2 3
OMIT -6 14 2
OMIT -2 4 6
OMIT -3 21 5
OMIT 2 3 7
OMIT 1 35 0
OMIT 1 38 2
OMIT -2 10 1
OMIT -9 2 2
OMIT 6 0 3
OMIT -6 27 1
OMIT 7 18 0
OMIT -5 2 7
OMIT -1 1 4
OMIT 2 22 2
OMIT 1 11 1
OMIT -1 13 2
OMIT 5 31 2
OMIT 3 12 1
OMIT -5 19 6
OMIT 2 10 1
OMIT 6 13 4
OMIT 0 22 3
OMIT 0 13 6
OMIT -3 22 4
OMIT 3 13 0
OMIT -2 3 5
OMIT -3 12 1
OMIT 3 19 1
OMIT 2 0 6
OMIT 2 6 6
OMIT 3 34 2
OMIT 0 6 4
OMIT -2 29 5
OMIT -3 23 3
OMIT 5 31 0
OMIT -4 16 6
OMIT -5 14 5
OMIT 0 17 1
OMIT 4 30 1
OMIT -2 12 3
OMIT -2 10 6
OMIT -4 20 4
OMIT 3 21 0
OMIT -2 22 2
OMIT -5 7 3
OMIT 2 18 3
OMIT -4 23 3
OMIT -3 15 3
OMIT -5 20 3
OMIT 3 3 1
OMIT 3 27 2
OMIT 0 10 6
OMIT 1 16 4
OMIT 1 14 0
OMIT 5 1 1
OMIT 6 7 0
OMIT -3 10 7
OMIT 1 12 7
OMIT -3 8 5
OMIT 3 19 0
OMIT 0 3 1
OMIT -2 8 6
OMIT 3 20 1
OMIT 0 23 1
OMIT -6 21 3
OMIT -1 10 4
OMIT 1 17 4
OMIT 2 3 5
OMIT 7 27 0
OMIT -4 32 1
OMIT 1 27 1
MORE -1
ISOR 0.001 C9 C18 C16 C17
ISOR 0.00 0.20 C12
ISOR 0.001 C12 C13 C14
HTAB N2 O3
EQIV $1 x+1, y, z-1
HTAB N2 O1_$1
EQIV $2 x-1, y, z
HTAB N4 N1_$2
EQIV $3 x+1, y, z
HTAB N1 N4_$3
HTAB N1 O2_$1
HTAB C2 O3
HTAB C7 O1
EQIV $4 -x-1, -y-1, z-1
HTAB O3 O2_$4
EQIV $5 x, y, z-1
HTAB O3 O2_$5
HTAB N2 O3
HTAB N2 O1_$1
HTAB N4 N1_$2
HTAB N1 N4_$3
HTAB N1 O2_$1
HTAB C2 O3
HTAB C7 O1
HTAB O3 O2_$4
HTAB O3 O2_$5
FMAP 2
PLAN 50
SIZE 0.120 0.210 0.320
ACTA
BOND $H
CONF
LIST 6
L.S. 30
TEMP -123.00
WGHT 0.200000
FVAR 0.48321
O2 4 -0.612909 -0.448534 -0.038626 11.00000 0.03536 0.05492 =
0.04197 0.00643 0.00081 0.00536
O1 4 -0.802286 -0.428471 -0.236480 11.00000 0.04032 0.05005 =
0.04480 0.00227 -0.00330 -0.00152
AFIX 6
O3 4 -0.302674 -0.474188 -0.949000 11.00000 0.05017 0.05608 =
0.06631 0.00365 -0.01339 -0.00447
AFIX 0
N2 3 0.012365 -0.447662 -0.879661 11.00000 0.03625 0.04596 =
0.03882 0.00324 0.00337 -0.00446
AFIX 93
H2A 2 -0.085900 -0.457048 -0.883395 11.00000 -1.20000
H2B 2 0.066897 -0.444598 -0.983396 11.00000 -1.20000
AFIX 0
N4 3 -0.591192 -0.380766 -0.429811 11.00000 0.02601 0.04033 =
0.04058 -0.00040 0.00103 -0.00097
AFIX 43
H4 2 -0.590135 -0.384599 -0.550982 11.00000 -1.20000
AFIX 0
N3 3 0.005165 -0.441866 -0.559963 11.00000 0.03368 0.04675 =
0.04400 -0.00522 0.00014 0.00266
AFIX 43
H3 2 0.058816 -0.434104 -0.460936 11.00000 -1.20000
AFIX 0
N1 3 0.228418 -0.423593 -0.723896 11.00000 0.03522 0.05467 =
0.04743 -0.01061 0.00239 -0.00808
AFIX 93
H1A 2 0.279311 -0.416394 -0.622027 11.00000 -1.20000
H1B 2 0.275572 -0.421352 -0.832857 11.00000 -1.20000
AFIX 0
C1 1 0.080115 -0.437870 -0.713169 11.00000 0.02592 0.03046 =
0.04491 -0.00722 -0.00334 0.00882
C4 1 -0.427389 -0.442244 -0.395197 11.00000 0.02643 0.05233 =
0.03402 -0.00343 0.00089 -0.00235
AFIX 23
H4A 2 -0.408833 -0.464657 -0.306855 11.00000 -1.20000
H4B 2 -0.486829 -0.452987 -0.503482 11.00000 -1.20000
AFIX 0
C6 1 -0.662952 -0.430062 -0.184493 11.00000 0.03055 0.04123 =
0.04059 -0.00030 -0.00329 0.00586
C5 1 -0.525586 -0.409181 -0.300495 11.00000 0.03383 0.04340 =
0.03383 0.00322 -0.00216 0.00283
AFIX 13
H5 2 -0.454413 -0.394325 -0.212256 11.00000 -1.20000
AFIX 0
C2 1 -0.151966 -0.456899 -0.522111 11.00000 0.03818 0.03635 =
0.04015 0.00116 0.00482 0.00128
AFIX 23
H2C 2 -0.144627 -0.477877 -0.424510 11.00000 -1.20000
H2D 2 -0.194273 -0.469828 -0.636077 11.00000 -1.20000
AFIX 0
C3 1 -0.267643 -0.425035 -0.459427 11.00000 0.03194 0.06771 =
0.04982 0.00203 -0.00148 0.00277
AFIX 23
H3A 2 -0.286715 -0.406065 -0.563423 11.00000 -1.20000
H3B 2 -0.219209 -0.409618 -0.355842 11.00000 -1.20000
AFIX 0
C7 1 -0.659707 -0.345032 -0.343668 11.00000 0.05047 0.06011 =
0.05698 -0.00223 -0.00645 0.00608
AFIX 23
H7A 2 -0.588495 -0.335366 -0.243138 11.00000 -1.20000
H7B 2 -0.764517 -0.351781 -0.287986 11.00000 -1.20000
AFIX 66
C8 1 -0.682343 -0.309586 -0.499676 11.00000 0.06150 0.04427 =
0.09009 -0.00555 0.01350 -0.00550
C9 1 -0.620410 -0.270725 -0.495535 11.00000 0.11462 0.11499 =
0.11504 -0.00032 -0.00003 0.00003
AFIX 43
H9 2 -0.553826 -0.262547 -0.395358 11.00000 -1.20000
AFIX 65
C10 1 -0.655899 -0.243829 -0.637966 11.00000 0.05992 0.04758 =
0.06960 -0.00875 0.02025 -0.00026
C18 1 -0.753320 -0.255794 -0.784541 11.00000 0.11611 0.11647 =
0.11649 -0.00037 -0.00025 0.00006
C19 1 -0.815254 -0.294655 -0.788685 11.00000 0.10079 0.12582 =
0.09066 0.01681 0.00169 0.01521
AFIX 43
H19 2 -0.881838 -0.302833 -0.888862 11.00000 -1.20000
AFIX 65
C20 1 -0.779766 -0.321552 -0.646254 11.00000 0.06781 0.05898 =
0.06242 -0.00127 0.00887 0.02160
AFIX 43
H20 2 -0.822095 -0.348112 -0.649086 11.00000 -1.20000
AFIX 66
C12 1 -0.655614 -0.186451 -0.823041 11.00000 0.06472 0.06585 =
0.06457 0.00026 0.00012 0.00016
C13 1 -0.649337 -0.149291 -0.912073 11.00000 0.08550 0.08577 =
0.08632 -0.00009 0.00019 0.00012
AFIX 43
H13 2 -0.589914 -0.127801 -0.858784 11.00000 -1.20000
AFIX 65
C14 1 -0.730004 -0.143576 -1.079074 11.00000 0.10101 0.10116 =
0.10106 -0.00010 0.00059 -0.00008
AFIX 43
H14 2 -0.725713 -0.118179 -1.139922 11.00000 -1.20000
AFIX 65
C15 1 -0.816949 -0.175020 -1.157044 11.00000 0.10405 0.08711 =
0.08760 0.02503 0.02049 0.01651
AFIX 43
H15 2 -0.872081 -0.171113 -1.271182 11.00000 -1.20000
AFIX 65
C16 1 -0.823228 -0.212180 -1.068015 11.00000 0.10935 0.10964 =
0.10977 -0.00032 0.00006 -0.00028
AFIX 43
H16 2 -0.882651 -0.233671 -1.121305 11.00000 -1.20000
AFIX 65
C17 1 -0.742562 -0.217896 -0.901014 11.00000 0.14777 0.14770 =
0.14783 0.00020 0.00026 0.00023
AFIX 0
C11 1 -0.585518 -0.201720 -0.648051 11.00000 0.09685 0.08596 =
0.08913 0.01676 0.01253 0.00937
AFIX 23
H11A 2 -0.618512 -0.185146 -0.540126 11.00000 -1.20000
H11B 2 -0.467433 -0.202508 -0.654559 11.00000 -1.20000
AFIX 3
H3C 2 -0.333847 -0.497935 -0.963686 11.00000 -1.50000
H3D 2 -0.384847 -0.459126 -0.934326 11.00000 -1.50000
AFIX 0
HKLF 4
REM fa_a_lt_cu_a.res in P2(1)2(1)2
REM R1 = 0.1243 for 1541 Fo > 4sig(Fo) and 0.1351 for all 1811 data
REM 223 parameters refined using 42 restraints
END
WGHT 0.2000 0.0000
REM Highest difference peak 0.608, deepest hole -0.344, 1-sigma level 0.092
Q1 1 -0.7856 -0.2290 -0.9568 11.00000 0.05 0.61
Q2 1 -0.6536 -0.1725 -0.8238 11.00000 0.05 0.60
Q3 1 -0.7579 -0.2711 -0.7497 11.00000 0.05 0.59
Q4 1 -0.6783 -0.1519 -0.9714 11.00000 0.05 0.58
Q5 1 -0.6042 -0.2747 -0.3856 11.00000 0.05 0.52
Q6 1 -0.8294 -0.2083 -1.1359 11.00000 0.05 0.47
Q7 1 -0.6951 -0.3181 -0.4603 11.00000 0.05 0.46
Q8 1 -0.7775 -0.1779 -1.1063 11.00000 0.05 0.41
Q9 1 -0.8176 -0.3616 -0.0419 11.00000 0.05 0.38
Q10 1 -0.7312 -0.1720 -1.2880 11.00000 0.05 0.37
Q11 1 0.2597 -0.3888 -0.8268 11.00000 0.05 0.36
Q12 1 -0.7530 -0.3112 -0.6368 11.00000 0.05 0.36
Q13 1 -0.1852 -0.4492 -0.1608 11.00000 0.05 0.34
Q14 1 -0.8164 -0.2782 -0.9232 11.00000 0.05 0.34
Q15 1 -0.6733 -0.2476 -0.6731 11.00000 0.05 0.32
Q16 1 -0.2918 -0.4816 -0.8998 11.00000 0.05 0.30
Q17 1 -0.7997 -0.4393 -0.2246 11.00000 0.05 0.29
Q18 1 -0.6830 -0.2062 -1.2826 11.00000 0.05 0.28
Q19 1 0.3804 -0.4175 -0.9388 11.00000 0.05 0.27
Q20 1 -0.6828 -0.1198 -1.2642 11.00000 0.05 0.25
Q21 1 -0.6131 -0.2675 -0.2258 11.00000 0.05 0.25
Q22 1 -0.6923 -0.3222 -0.8836 11.00000 0.05 0.24
Q23 1 -0.8054 -0.4207 -0.3704 11.00000 0.05 0.24
Q24 1 0.1376 -0.4366 -1.1011 11.00000 0.05 0.24
Q25 1 0.2923 -0.4401 -0.8652 11.00000 0.05 0.23
Q26 1 -0.6062 -0.2377 -0.4929 11.00000 0.05 0.22
Q27 1 -0.3545 -0.4589 -0.3207 11.00000 0.05 0.22
Q28 1 -0.6543 -0.1119 -1.0582 11.00000 0.05 0.22
Q29 1 -0.8970 -0.3090 -0.9976 11.00000 0.05 0.22
Q30 1 -0.9717 -0.3689 -0.7260 11.00000 0.05 0.22
Q31 1 -0.9362 -0.2989 -0.9838 11.00000 0.05 0.21
Q32 1 -0.9591 -0.2300 -0.9716 11.00000 0.05 0.21
Q33 1 -0.4628 -0.4601 -0.6998 11.00000 0.05 0.21
Q34 1 -0.4010 -0.4171 -0.2367 11.00000 0.05 0.21
Q35 1 -0.8277 -0.2969 -1.0370 11.00000 0.05 0.20
Q36 1 -0.4465 -0.4116 -0.2248 11.00000 0.05 0.20
Q37 1 -0.3168 -0.5086 -0.9598 11.00000 0.05 0.20
Q38 1 0.0176 -0.4114 -0.5446 11.00000 0.05 0.20
Q39 1 -0.4997 -0.2937 -0.1392 11.00000 0.05 0.20
Q40 1 -0.9668 -0.3300 -0.6326 11.00000 0.05 0.20
Q41 1 -0.6694 -0.3079 -0.1477 11.00000 0.05 0.20
Q42 1 -0.3220 -0.3835 -0.6785 11.00000 0.05 0.19
Q43 1 -1.0112 -0.1418 -1.2856 11.00000 0.05 0.19
Q44 1 -0.7727 -0.4785 -0.2656 11.00000 0.05 0.19
Q45 1 0.0350 -0.4662 -1.1195 11.00000 0.05 0.19
Q46 1 -0.2835 -0.5005 -0.7911 11.00000 0.05 0.19
Q47 1 -0.6948 -0.0786 -1.1477 11.00000 0.05 0.19
Q48 1 -0.4659 -0.4127 -0.6931 11.00000 0.05 0.19
Q49 1 -0.4351 -0.2389 -0.6759 11.00000 0.05 0.19
Q50 1 -0.0326 -0.4699 -0.4321 11.00000 0.05 0.18
;
_shelx_res_checksum 99047
#######################################################################
#
# 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_fa_sma_rt_cu
_database_code_depnum_ccdc_archive 'CCDC 2031639'
loop_
_audit_author_name
_audit_author_address
'Rik Rani koner'
;IIT Mandi
India
;
_audit_update_record
;
2020-11-30 deposited with the CCDC. 2020-12-21 downloaded from the CCDC.
;
_audit_creation_date 2020-11-30
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C8 H7 O3, C20 H25 N4 O2'
_chemical_formula_sum 'C28 H32 N4 O5'
_chemical_formula_weight 504.58
_chemical_absolute_configuration unk
_chemical_melting_point ?
_chemical_oxdiff_formula 'C56 H64 N8 O10'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 4
_space_group_name_H-M_alt 'P 21'
_space_group_name_Hall 'P 2yb'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z'
_cell_length_a 10.8104(5)
_cell_length_b 5.7783(3)
_cell_length_c 21.3807(10)
_cell_angle_alpha 90.00
_cell_angle_beta 91.903(5)
_cell_angle_gamma 90.00
_cell_volume 1334.82(11)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 2088
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 66.9520
_cell_measurement_theta_min 4.1370
_exptl_absorpt_coefficient_mu 0.712
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.614
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 1.255
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description monoclinic
_exptl_crystal_F_000 536
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 0 12 0.0479
-7 0 5 0.0315
2 0 -14 0.0426
-2 -2 10 0.1328
0 4 1 0.1907
0 -4 -1 0.1957
1 -2 -12 0.1018
6 0 -7 0.0487
-1 0 14 0.0346
7 0 1 0.0545
-3 0 -12 0.0479
-6 0 -7 0.0396
_exptl_crystal_size_max 0.393
_exptl_crystal_size_mid 0.098
_exptl_crystal_size_min 0.079
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
3.0000 0.0000 11.9998 -0.7555 -0.1779 -0.5945
-7.0000 0.0001 4.9996 -0.5478 0.3615 0.8191
2.0000 -0.0001 -13.9996 1.0368 -0.0829 -0.0177
-2.0000 -2.0000 9.9998 -0.7201 0.5847 -0.1077
0.0000 4.0000 0.9997 -0.1432 -0.9923 0.3712
-0.0000 -4.0000 -0.9997 0.1432 0.9923 -0.3712
1.0000 -2.0001 -11.9995 0.9051 0.4620 -0.1170
6.0000 -0.0001 -6.9996 0.6596 -0.3054 -0.6554
-1.0000 0.0001 13.9996 -1.0085 0.0301 -0.1116
7.0000 -0.0000 1.0003 0.1277 -0.3712 -0.9224
-3.0000 -0.0000 -11.9998 0.7555 0.1779 0.5945
-6.0000 0.0000 -7.0001 0.3207 0.3282 0.8963
_exptl_special_details
;
?
;
_diffrn_reflns_av_R_equivalents 0.0263
_diffrn_reflns_av_unetI/netI 0.0416
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_number 4483
_diffrn_reflns_theta_full 66.86
_diffrn_reflns_theta_max 66.86
_diffrn_reflns_theta_min 7.94
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type Eos
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -51.00 52.00 1.00 1.00 -- 25.69 -57.00-180.00 103
2 \w 57.00 116.00 1.00 1.00 -- 25.69 178.00 30.00 59
3 \w 82.00 119.00 1.00 1.00 -- 25.69 178.00-180.00 37
4 \w 32.00 104.00 1.00 2.00 -- 66.85 63.00-180.00 72
5 \w 4.00 109.00 1.00 2.00 -- 66.85 -50.00-120.00 105
6 \w 105.00 150.00 1.00 2.00 -- 66.85 111.00 -30.00 45
7 \w 43.00 112.00 1.00 2.00 -- 66.85-111.00 30.00 69
8 \w 12.00 84.00 1.00 2.00 -- 66.85-111.00 -90.00 72
9 \w 141.00 175.00 1.00 7.00 -- 108.00 54.00 -30.00 34
10 \w 104.00 177.00 1.00 7.00 -- 108.00 104.00-150.00 73
11 \w 142.00 175.00 1.00 7.00 -- 108.00 65.00 30.00 33
12 \w 95.00 128.00 1.00 7.00 -- 108.00 54.00 -30.00 33
13 \w 109.00 169.00 1.00 7.00 -- 108.00 138.00 -30.00 60
14 \w 109.00 176.00 1.00 7.00 -- 108.00 43.00 90.00 67
15 \w 42.00 99.00 1.00 7.00 -- 108.00-104.00 60.00 57
16 \w 55.00 80.00 1.00 7.00 -- 108.00-104.00 150.00 25
17 \w 24.00 52.00 1.00 7.00 -- 108.00-104.00 150.00 28
18 \w 64.00 91.00 1.00 7.00 -- 108.00 43.00 90.00 27
19 \w 101.00 157.00 1.00 7.00 -- 108.00 104.00 150.00 56
20 \w 95.00 135.00 1.00 7.00 -- 108.00 65.00 30.00 40
21 \w 108.00 175.00 1.00 7.00 -- 108.00 104.00 -60.00 67
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0282486000
_diffrn_orient_matrix_UB_12 -0.0182897000
_diffrn_orient_matrix_UB_13 -0.0700233000
_diffrn_orient_matrix_UB_21 -0.0528035000
_diffrn_orient_matrix_UB_22 -0.2476644000
_diffrn_orient_matrix_UB_23 -0.0016239000
_diffrn_orient_matrix_UB_31 -0.1293091000
_diffrn_orient_matrix_UB_32 0.0971036000
_diffrn_orient_matrix_UB_33 -0.0172115000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_reflns_number_gt 2576
_reflns_number_total 2860
_reflns_odcompleteness_completeness 98.37
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_reflns_threshold_expression >2sigma(I)
_computing_cell_refinement 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2008)'
_computing_structure_solution 'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max 0.115
_refine_diff_density_min -0.127
_refine_diff_density_rms 0.029
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.2(2)
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.988
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 335
_refine_ls_number_reflns 2860
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0384
_refine_ls_R_factor_gt 0.0343
_refine_ls_restrained_S_all 0.988
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0796
_refine_ls_wR_factor_ref 0.0815
_refine_special_details
;Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.,SQUEEZE
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
At 1.5 times of:
All O(H) groups
2.a Ternary CH refined with riding coordinates:
C5(H5), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
N4(H4A,H4B), C7(H7A,H7B), C3(H3A,H3B), C2(H2C,H2D), C11(H11A,H11B), C4(H4C,H4D)
2.c Aromatic/amide H refined with riding coordinates:
C9(H9), N3(H3), C20(H20), C19(H19), C28(H28), C16(H16), C27(H27), C13(H13),
C26(H26), C24(H24), C14(H14), C15(H15), C25(H25)
2.d X=CH2 refined with riding coordinates:
N2(H2A,H2B), N1(H1A,H1B)
2.e Idealised tetrahedral OH refined as rotating group:
O5(H5A)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
O3 O -0.10603(14) -0.3643(3) -0.07700(8) 0.0485(4) Uani 1 d . . .
N4 N -0.52587(15) 0.2502(3) 0.22515(8) 0.0330(4) Uani 1 d . . .
H4A H -0.4942 0.1065 0.2283 0.040 Uiso 1 calc . . R
H4B H -0.5795 0.2518 0.1921 0.040 Uiso 1 calc . . R
N2 N -0.2758(2) 0.1247(5) -0.05283(10) 0.0538(5) Uani 1 d . . .
H2A H -0.2639 0.0084 -0.0770 0.065 Uiso 1 calc . . R
H2B H -0.3327 0.2239 -0.0623 0.065 Uiso 1 calc . . R
O4 O -0.29030(15) -0.3097(4) -0.12346(8) 0.0485(4) Uani 1 d . . .
O1 O -0.42636(17) 0.8173(3) 0.23453(9) 0.0501(4) Uani 1 d . . .
O2 O -0.5627(2) 0.6781(3) 0.16406(10) 0.0610(5) Uani 1 d . . .
O5 O -0.23973(17) -0.6147(3) -0.21641(9) 0.0520(4) Uani 1 d . . .
H5A H -0.2999 -0.6482 -0.1959 0.078 Uiso 1 calc . . GR
C9 C -0.4252(2) 0.1711(4) 0.35961(10) 0.0379(4) Uani 1 d . . .
H9 H -0.4149 0.0371 0.3363 0.045 Uiso 1 calc . . R
C21 C -0.18354(18) -0.3940(4) -0.12096(10) 0.0366(4) Uani 1 d . . .
N1 N -0.1199(2) -0.0014(5) 0.01291(11) 0.0532(5) Uani 1 d . . .
H1A H -0.1085 -0.1172 -0.0115 0.064 Uiso 1 calc . . R
H1B H -0.0745 0.0145 0.0464 0.064 Uiso 1 calc . . R
C7 C -0.59625(18) 0.3006(4) 0.28351(10) 0.0388(5) Uani 1 d . . .
H7A H -0.6452 0.4395 0.2766 0.047 Uiso 1 calc . . R
H7B H -0.6530 0.1739 0.2906 0.047 Uiso 1 calc . . R
N3 N -0.22634(19) 0.3338(4) 0.03488(9) 0.0465(5) Uani 1 d . . .
H3 H -0.2827 0.4296 0.0222 0.056 Uiso 1 calc . . R
C5 C -0.42357(18) 0.4143(4) 0.21280(9) 0.0308(4) Uani 1 d . . .
H5 H -0.3654 0.4151 0.2489 0.037 Uiso 1 calc . . R
C1 C -0.2065(2) 0.1510(5) -0.00102(11) 0.0420(5) Uani 1 d . . .
C18 C -0.3703(2) 0.4095(4) 0.44947(10) 0.0414(5) Uani 1 d . . .
C8 C -0.51496(19) 0.3334(4) 0.34138(10) 0.0372(4) Uani 1 d . . .
C6 C -0.4757(2) 0.6585(4) 0.20321(10) 0.0362(4) Uani 1 d . . .
C17 C -0.2794(2) 0.4075(5) 0.50227(11) 0.0489(6) Uani 1 d . . .
C3 C -0.2485(2) 0.4921(4) 0.14004(11) 0.0412(5) Uani 1 d . . .
H3A H -0.2812 0.6359 0.1229 0.049 Uiso 1 calc . . R
H3B H -0.2022 0.5283 0.1785 0.049 Uiso 1 calc . . R
C22 C -0.1416(2) -0.5434(4) -0.17581(11) 0.0394(5) Uani 1 d . . .
H22 H -0.0992 -0.6810 -0.1590 0.047 Uiso 1 calc . . R
C10 C -0.3516(2) 0.2116(4) 0.41288(10) 0.0395(5) Uani 1 d . . .
C20 C -0.5320(2) 0.5308(4) 0.37795(11) 0.0436(5) Uani 1 d . . .
H20 H -0.5914 0.6390 0.3654 0.052 Uiso 1 calc . . R
C23 C -0.05227(19) -0.4082(4) -0.21500(10) 0.0388(5) Uani 1 d . . .
C19 C -0.4618(2) 0.5684(5) 0.43264(12) 0.0486(6) Uani 1 d . . .
H19 H -0.4758 0.6974 0.4574 0.058 Uiso 1 calc . . R
C2 C -0.1612(2) 0.3859(5) 0.09365(12) 0.0471(5) Uani 1 d . . .
H2C H -0.0941 0.4929 0.0862 0.057 Uiso 1 calc . . R
H2D H -0.1257 0.2449 0.1111 0.057 Uiso 1 calc . . R
C28 C -0.0842(2) -0.1905(5) -0.23685(12) 0.0471(5) Uani 1 d . . .
H28 H -0.1569 -0.1217 -0.2241 0.057 Uiso 1 calc . . R
C16 C -0.2606(3) 0.5657(7) 0.55111(12) 0.0664(8) Uani 1 d . . .
H16 H -0.3106 0.6957 0.5549 0.080 Uiso 1 calc . . R
C11 C -0.2442(2) 0.0726(5) 0.43975(13) 0.0519(6) Uani 1 d . . .
H11A H -0.1782 0.0611 0.4103 0.062 Uiso 1 calc . . R
H11B H -0.2701 -0.0818 0.4514 0.062 Uiso 1 calc . . R
C27 C -0.0086(3) -0.0733(6) -0.27764(15) 0.0664(8) Uani 1 d . . .
H27 H -0.0316 0.0722 -0.2926 0.080 Uiso 1 calc . . R
C12 C -0.2043(3) 0.2126(5) 0.49660(12) 0.0513(6) Uani 1 d . . .
C13 C -0.1066(3) 0.1717(7) 0.53945(15) 0.0690(8) Uani 1 d . . .
H13 H -0.0559 0.0426 0.5358 0.083 Uiso 1 calc . . R
C26 C 0.1002(3) -0.1726(8) -0.29596(15) 0.0737(10) Uani 1 d . . .
H26 H 0.1499 -0.0964 -0.3241 0.088 Uiso 1 calc . . R
C24 C 0.0590(2) -0.5032(5) -0.23245(13) 0.0535(6) Uani 1 d . . .
H24 H 0.0833 -0.6477 -0.2173 0.064 Uiso 1 calc . . R
C14 C -0.0872(4) 0.3297(8) 0.58782(16) 0.0790(11) Uani 1 d . . .
H14 H -0.0217 0.3070 0.6165 0.095 Uiso 1 calc . . R
C15 C -0.1631(4) 0.5194(8) 0.59415(14) 0.0785(11) Uani 1 d . . .
H15 H -0.1492 0.6191 0.6278 0.094 Uiso 1 calc . . R
C25 C 0.1345(3) -0.3823(8) -0.27269(16) 0.0710(10) Uani 1 d . . .
H25 H 0.2096 -0.4464 -0.2838 0.085 Uiso 1 calc . . R
C4 C -0.3557(2) 0.3330(4) 0.15506(10) 0.0374(4) Uani 1 d . . .
H4C H -0.3244 0.1775 0.1623 0.045 Uiso 1 calc . . R
H4D H -0.4135 0.3276 0.1194 0.045 Uiso 1 calc . . R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O3 0.0409(7) 0.0588(11) 0.0450(8) -0.0062(8) -0.0084(7) -0.0009(8)
N4 0.0362(8) 0.0306(8) 0.0317(8) -0.0025(7) -0.0060(6) 0.0024(7)
N2 0.0540(10) 0.0624(14) 0.0443(11) -0.0065(10) -0.0071(9) 0.0059(11)
O4 0.0398(7) 0.0599(11) 0.0456(9) -0.0088(8) -0.0044(6) 0.0062(7)
O1 0.0644(10) 0.0261(7) 0.0590(10) -0.0054(7) -0.0083(8) 0.0034(7)
O2 0.0745(11) 0.0450(10) 0.0614(11) -0.0046(9) -0.0309(9) 0.0207(9)
O5 0.0507(9) 0.0562(11) 0.0488(9) -0.0118(8) -0.0040(7) -0.0135(8)
C9 0.0430(10) 0.0376(11) 0.0328(9) -0.0049(8) 0.0005(8) -0.0008(9)
C21 0.0323(9) 0.0378(11) 0.0397(10) -0.0027(9) -0.0014(8) -0.0035(9)
N1 0.0484(10) 0.0565(13) 0.0541(12) -0.0170(11) -0.0075(9) 0.0070(10)
C7 0.0329(9) 0.0453(12) 0.0380(10) -0.0036(9) 0.0006(8) -0.0011(9)
N3 0.0530(10) 0.0517(12) 0.0347(9) 0.0003(9) -0.0012(8) 0.0108(10)
C5 0.0341(9) 0.0278(9) 0.0302(9) -0.0035(7) -0.0040(7) 0.0025(8)
C1 0.0400(10) 0.0484(12) 0.0378(10) 0.0015(10) 0.0052(8) -0.0023(10)
C18 0.0479(11) 0.0446(12) 0.0320(10) -0.0033(9) 0.0041(9) -0.0077(10)
C8 0.0359(9) 0.0426(11) 0.0331(10) -0.0033(9) 0.0024(8) -0.0026(9)
C6 0.0460(10) 0.0287(10) 0.0338(10) 0.0000(8) 0.0013(8) 0.0049(9)
C17 0.0582(13) 0.0569(15) 0.0314(11) 0.0019(10) 0.0001(10) -0.0126(12)
C3 0.0455(11) 0.0400(11) 0.0382(11) -0.0080(9) 0.0020(9) -0.0007(9)
C22 0.0394(10) 0.0344(11) 0.0439(12) -0.0024(9) -0.0042(9) 0.0029(8)
C10 0.0459(10) 0.0419(12) 0.0306(10) 0.0002(9) 0.0005(8) -0.0022(10)
C20 0.0429(10) 0.0424(12) 0.0458(12) -0.0044(10) 0.0030(9) 0.0033(9)
C23 0.0362(9) 0.0426(12) 0.0368(10) -0.0049(9) -0.0082(8) -0.0017(9)
C19 0.0528(12) 0.0499(14) 0.0435(12) -0.0143(10) 0.0054(10) 0.0013(11)
C2 0.0410(10) 0.0592(15) 0.0411(11) -0.0077(11) 0.0023(9) -0.0002(11)
C28 0.0442(11) 0.0468(13) 0.0497(13) 0.0030(11) -0.0083(10) -0.0045(10)
C16 0.0879(19) 0.075(2) 0.0364(13) -0.0106(13) -0.0015(13) -0.0185(17)
C11 0.0562(13) 0.0500(14) 0.0486(13) 0.0028(11) -0.0114(11) 0.0045(12)
C27 0.0791(19) 0.0642(18) 0.0547(16) 0.0115(14) -0.0147(14) -0.0279(16)
C12 0.0583(13) 0.0587(16) 0.0364(11) 0.0090(11) -0.0072(10) -0.0121(13)
C13 0.0743(17) 0.078(2) 0.0535(16) 0.0182(16) -0.0206(13) -0.0130(16)
C26 0.0711(18) 0.100(3) 0.0505(15) -0.0094(17) 0.0096(14) -0.037(2)
C24 0.0451(12) 0.0580(15) 0.0571(14) -0.0148(13) -0.0024(11) 0.0058(12)
C14 0.090(2) 0.092(3) 0.0523(16) 0.0180(17) -0.0308(16) -0.029(2)
C15 0.105(2) 0.092(3) 0.0371(13) -0.0059(16) -0.0154(15) -0.037(2)
C25 0.0469(13) 0.103(3) 0.0640(17) -0.0250(19) 0.0147(12) -0.0138(17)
C4 0.0458(10) 0.0277(10) 0.0388(10) -0.0094(8) 0.0018(9) 0.0028(9)
_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
O3 C21 1.250(3) . ?
N4 C7 1.511(3) . ?
N4 C5 1.487(3) . ?
N2 C1 1.325(3) . ?
O4 C21 1.252(3) . ?
O1 C6 1.245(3) . ?
O2 C6 1.243(3) . ?
O5 C22 1.410(3) . ?
C9 C8 1.395(3) . ?
C9 C10 1.387(3) . ?
C21 C22 1.537(3) . ?
N1 C1 1.312(4) . ?
C7 C8 1.506(3) . ?
N3 C1 1.327(3) . ?
N3 C2 1.452(3) . ?
C5 C6 1.531(3) . ?
C5 C4 1.531(3) . ?
C18 C17 1.472(3) . ?
C18 C10 1.404(3) . ?
C18 C19 1.388(4) . ?
C8 C20 1.398(3) . ?
C17 C16 1.397(4) . ?
C17 C12 1.396(4) . ?
C3 C2 1.520(3) . ?
C3 C4 1.522(3) . ?
C22 C23 1.516(3) . ?
C10 C11 1.509(3) . ?
C20 C19 1.390(4) . ?
C23 C28 1.381(4) . ?
C23 C24 1.384(4) . ?
C28 C27 1.391(4) . ?
C16 C15 1.402(5) . ?
C11 C12 1.511(4) . ?
C27 C26 1.378(6) . ?
C12 C13 1.395(4) . ?
C13 C14 1.390(6) . ?
C26 C25 1.357(6) . ?
C24 C25 1.394(5) . ?
C14 C15 1.378(7) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C5 N4 C7 114.93(16) . . ?
C10 C9 C8 119.4(2) . . ?
O3 C21 O4 124.9(2) . . ?
O3 C21 C22 116.31(18) . . ?
O4 C21 C22 118.75(18) . . ?
C8 C7 N4 114.00(16) . . ?
C1 N3 C2 125.6(2) . . ?
N4 C5 C6 109.82(15) . . ?
N4 C5 C4 109.07(16) . . ?
C4 C5 C6 111.04(17) . . ?
N2 C1 N3 118.5(2) . . ?
N1 C1 N2 119.5(2) . . ?
N1 C1 N3 122.0(2) . . ?
C10 C18 C17 108.5(2) . . ?
C19 C18 C17 131.0(2) . . ?
C19 C18 C10 120.6(2) . . ?
C9 C8 C7 121.8(2) . . ?
C9 C8 C20 119.7(2) . . ?
C20 C8 C7 118.6(2) . . ?
O1 C6 C5 117.26(18) . . ?
O2 C6 O1 126.6(2) . . ?
O2 C6 C5 116.16(19) . . ?
C16 C17 C18 130.1(3) . . ?
C12 C17 C18 108.4(2) . . ?
C12 C17 C16 121.5(3) . . ?
C2 C3 C4 112.8(2) . . ?
O5 C22 C21 113.50(18) . . ?
O5 C22 C23 106.89(19) . . ?
C23 C22 C21 109.99(18) . . ?
C9 C10 C18 120.4(2) . . ?
C9 C10 C11 129.5(2) . . ?
C18 C10 C11 110.1(2) . . ?
C19 C20 C8 121.3(2) . . ?
C28 C23 C22 120.0(2) . . ?
C28 C23 C24 118.6(2) . . ?
C24 C23 C22 121.3(2) . . ?
C18 C19 C20 118.6(2) . . ?
N3 C2 C3 110.77(19) . . ?
C23 C28 C27 120.7(3) . . ?
C17 C16 C15 116.9(4) . . ?
C10 C11 C12 102.5(2) . . ?
C26 C27 C28 120.0(3) . . ?
C17 C12 C11 110.5(2) . . ?
C13 C12 C17 120.6(3) . . ?
C13 C12 C11 128.9(3) . . ?
C14 C13 C12 118.0(4) . . ?
C25 C26 C27 119.5(3) . . ?
C23 C24 C25 120.0(3) . . ?
C15 C14 C13 121.3(3) . . ?
C14 C15 C16 121.6(3) . . ?
C26 C25 C24 121.1(3) . . ?
C3 C4 C5 111.94(17) . . ?
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
N4 H4A O1 0.90 1.83 2.728(2) 178.7 1_545
O5 H5A O2 0.82 1.93 2.722(3) 160.5 2_435
N1 H1A O3 0.86 2.00 2.852(3) 170.2 .
N1 H1B O3 0.86 2.15 2.872(3) 140.7 2
_smtbx_masks_special_details ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 -0.557 0.000 71.1 20.9 ?
_iucr_refine_instructions_details
;
TITL FA_SMA_Rt_Cu in P21 #4
REM Best SHELXD solution FINAL CC 86.12
REM Fragments: 26 11 1
REM reset to P21 #4
CELL 1.54184 10.810447 5.778251 21.380664 90 91.9027 90
ZERR 2 0.000455 0.000267 0.001044 0 0.0045 0
LATT -1
SYMM -X,0.5+Y,-Z
SFAC C H N O
UNIT 56 64 8 10
EQIV $1 +X,-1+Y,+Z
EQIV $2 -1-X,-1.5+Y,-Z
EQIV $3 -X,0.5+Y,-Z
L.S. 30 0 0
PLAN 20
HTAB N4 O1_$1
HTAB O5 O2_$2
HTAB N1 O3
HTAB N1 O3_$3
FREE H1b O3
FREE O3 N1
fmap 2 53
acta
OMIT -2 0 1
OMIT 2 0 0
OMIT 0 0 2
OMIT -4 0 4
OMIT 1 0 1
OMIT 3 0 7
OMIT 5 0 3
OMIT 3 0 6
OMIT 0 0 7
OMIT -4 0 2
OMIT 4 0 0
OMIT 0 1 3
OMIT 1 0 2
OMIT -4 0 1
OMIT 0 2 3
OMIT 2 0 7
OMIT 5 1 0
OMIT 3 2 1
OMIT 5 -1 3
OMIT -3 0 3
OMIT 5 1 3
OMIT -3 0 2
OMIT -3 3 4
OMIT 0 2 10
OMIT -2 2 3
OMIT -1 0 7
OMIT 1 0 11
OMIT 4 0 6
OMIT 5 0 5
OMIT 1 0 8
OMIT 4 2 11
OMIT -4 0 3
OMIT 4 1 0
OMIT 5 0 4
OMIT 1 1 7
OMIT -4 0 6
OMIT 0 1 2
OMIT 2 2 8
OMIT -1 0 11
OMIT -8 -1 3
OMIT 0 0 12
OMIT 1 2 8
OMIT -9 1 1
OMIT -7 5 2
OMIT -4 2 2
OMIT 6 -1 2
OMIT 1 1 5
OMIT -6 2 7
OMIT 4 0 7
OMIT 4 2 7
OMIT 1 1 2
OMIT -5 0 3
OMIT -1 1 7
OMIT 0 0 8
OMIT 3 0 1
OMIT -3 2 3
OMIT 3 0 5
OMIT 3 0 2
OMIT 2 1 12
OMIT -6 4 17
OMIT 4 0 4
OMIT 3 1 3
OMIT -2 0 18
OMIT -7 2 1
OMIT 0 0 11
OMIT 3 0 4
OMIT -1 2 1
OMIT 2 0 10
OMIT -5 0 2
OMIT 2 0 3
OMIT 6 0 6
OMIT 6 -1 1
OMIT -1 1 8
OMIT 0 0 10
OMIT -2 1 5
OMIT -5 0 4
OMIT -1 0 8
OMIT -1 0 10
OMIT 1 0 10
OMIT -2 3 10
OMIT -2 3 3
OMIT 4 2 5
OMIT -7 2 7
OMIT 0 4 17
OMIT 6 0 17
OMIT 2 0 5
OMIT -4 1 4
OMIT -5 3 14
OMIT 5 0 6
OMIT 2 -1 12
OMIT 0 0 3
OMIT -1 0 12
OMIT 9 0 1
OMIT 3 1 2
OMIT 4 0 5
OMIT 1 0 12
OMIT -1 3 4
OMIT -6 3 1
OMIT -5 0 5
OMIT 2 0 4
OMIT 5 3 4
OMIT 0 2 1
OMIT -1 0 2
OMIT 1 3 5
OMIT 4 2 4
OMIT -7 2 2
OMIT 3 0 15
OMIT -12 -2 1
OMIT 2 1 13
OMIT 3 1 9
OMIT 0 6 6
OMIT -1 0 6
OMIT 6 0 13
OMIT 2 3 6
OMIT 3 1 5
OMIT 3 -1 9
OMIT -4 2 3
OMIT -5 4 2
OMIT 3 1 11
OMIT -6 0 2
OMIT -5 -2 11
OMIT 0 4 16
OMIT -1 0 13
OMIT 4 1 10
OMIT 2 2 5
OMIT 3 -1 11
OMIT 0 1 7
OMIT -2 1 8
OMIT -5 3 19
OMIT -6 3 4
OMIT 5 0 17
OMIT 8 5 4
OMIT 3 2 0
OMIT -8 2 3
OMIT 8 -4 1
OMIT -4 0 21
OMIT 2 3 11
OMIT 2 2 18
OMIT -11 3 2
OMIT 8 5 3
OMIT -2 0 2
OMIT -4 3 14
OMIT -2 4 13
OMIT -4 4 11
OMIT -6 1 1
OMIT 2 0 1
OMIT 0 1 4
OMIT 1 1 8
OMIT 5 -5 2
OMIT -8 1 3
OMIT 2 0 2
OMIT 4 2 9
OMIT -3 1 3
OMIT -8 0 16
OMIT 2 1 2
OMIT -9 -3 3
OMIT -1 0 9
OMIT 0 -1 13
OMIT 0 1 14
OMIT 0 3 4
OMIT 1 1 16
OMIT -6 -1 15
OMIT 2 2 1
OMIT -5 0 6
OMIT 0 0 13
OMIT 0 2 0
OMIT 7 -1 15
OMIT 0 0 9
OMIT 0 3 1
OMIT -1 0 1
OMIT -3 -1 12
OMIT 6 2 2
OMIT -1 1 3
OMIT 7 -2 11
OMIT -7 4 5
OMIT 6 1 2
OMIT -1 2 13
OMIT -3 0 6
OMIT 8 0 12
OMIT -5 0 11
OMIT -3 2 1
OMIT 0 2 9
OMIT 5 3 19
OMIT -4 1 5
OMIT -3 5 9
OMIT 5 1 11
OMIT 2 -2 18
OMIT -2 6 4
OMIT 1 0 18
OMIT -8 -4 13
OMIT -3 1 2
OMIT 7 2 2
OMIT -1 2 10
OMIT -1 3 5
OMIT -6 -1 1
OMIT 2 2 17
OMIT 1 1 6
OMIT -5 3 4
OMIT -9 0 1
OMIT -9 -1 1
OMIT -5 3 2
OMIT 6 -2 17
OMIT 3 2 10
OMIT -2 -1 11
OMIT -4 0 15
OMIT 6 0 12
OMIT 8 2 15
OMIT -5 0 7
OMIT -6 6 3
OMIT -8 2 2
OMIT -2 3 19
OMIT -3 -2 13
OMIT -1 2 7
OMIT -11 0 5
OMIT -7 1 4
OMIT -4 1 12
OMIT 9 1 13
OMIT 9 3 1
OMIT -3 -2 11
OMIT -10 4 1
OMIT 0 1 17
OMIT 6 6 3
OMIT -7 3 11
OMIT -3 1 7
OMIT 5 2 13
OMIT -9 -2 6
OMIT -7 1 8
OMIT 1 1 18
OMIT 4 3 0
OMIT -11 3 1
OMIT -6 -1 8
OMIT -5 5 6
OMIT -5 0 15
OMIT -5 3 17
OMIT -3 5 14
OMIT 1 -1 18
OMIT 0 1 19
OMIT 2 0 8
OMIT 2 6 0
OMIT 7 0 7
OMIT 3 1 13
OMIT 8 4 1
OMIT 6 -5 5
OMIT 5 0 14
OMIT -1 1 17
OMIT 7 -2 15
OMIT -8 4 6
OMIT -2 0 17
OMIT 4 0 11
OMIT -9 4 8
OMIT 2 1 1
OMIT -1 1 5
OMIT 1 0 5
OMIT 1 2 7
OMIT -2 -2 11
OMIT 1 0 0
OMIT -2 3 7
OMIT -2 2 6
OMIT 0 1 6
OMIT 1 0 7
OMIT 3 0 10
OMIT 4 2 6
OMIT 5 1 5
OMIT -2 0 11
OMIT -6 0 5
OMIT -5 4 6
OMIT -1 2 6
OMIT 3 2 7
OMIT 0 0 4
OMIT 3 2 12
OMIT -2 0 13
OMIT -8 0 10
OMIT -1 -1 10
OMIT 1 1 10
OMIT -5 2 3
OMIT 1 0 20
OMIT -4 0 17
OMIT -3 -1 11
OMIT 2 3 4
OMIT -3 4 7
OMIT -1 1 6
OMIT -1 4 15
OMIT 4 2 0
OMIT 0 2 12
OMIT 11 0 1
OMIT 0 2 7
OMIT 1 -1 10
OMIT 3 1 4
OMIT -3 4 9
OMIT -4 5 14
OMIT -7 0 2
OMIT 0 1 5
OMIT -6 2 5
OMIT -2 0 4
OMIT 4 1 5
OMIT -7 4 11
OMIT -5 4 8
OMIT 1 0 6
OMIT -3 3 6
OMIT -3 5 4
OMIT -3 3 1
OMIT 5 2 2
OMIT -1 2 8
OMIT 1 3 10
OMIT 5 2 8
OMIT 3 3 9
OMIT 2 4 5
OMIT 1 0 3
OMIT 4 2 8
OMIT -3 3 5
OMIT 0 2 8
OMIT -4 2 18
OMIT 7 -3 4
OMIT 2 3 0
OMIT -1 4 11
OMIT 8 0 0
OMIT 2 4 7
OMIT -10 0 15
OMIT 5 2 9
OMIT 1 3 0
OMIT -5 0 9
OMIT 4 -5 6
OMIT 5 2 5
OMIT -4 5 5
OMIT 5 4 13
OMIT -2 -1 14
OMIT -1 -2 8
OMIT 3 3 11
OMIT 7 3 5
OMIT -6 3 12
OMIT -6 0 10
OMIT -1 2 11
OMIT -6 -1 14
OMIT -7 0 4
OMIT 0 -2 8
OMIT -3 3 3
OMIT 8 -3 3
OMIT 0 2 13
OMIT -1 3 1
OMIT 3 2 3
OMIT 11 -3 2
OMIT 9 -3 5
OMIT -4 1 2
OMIT 2 4 0
OMIT 0 5 9
OMIT 2 1 5
OMIT -4 -2 18
OMIT -3 2 21
OMIT -8 -1 14
OMIT 0 5 6
REM
REM
REM
WGHT 0.039600
FVAR 8.79321
O3 4 -0.106025 -0.364341 -0.076998 11.00000 0.04093 0.05883 =
0.04497 -0.00618 -0.00841 -0.00091
N4 3 -0.525868 0.250184 0.225150 11.00000 0.03621 0.03062 =
0.03171 -0.00253 -0.00601 0.00242
AFIX 23
H4A 2 -0.494175 0.106456 0.228257 11.00000 -1.20000
H4B 2 -0.579543 0.251752 0.192062 11.00000 -1.20000
AFIX 0
N2 3 -0.275816 0.124676 -0.052827 11.00000 0.05401 0.06239 =
0.04431 -0.00654 -0.00706 0.00589
AFIX 93
H2A 2 -0.263884 0.008413 -0.077005 11.00000 -1.20000
H2B 2 -0.332743 0.223856 -0.062262 11.00000 -1.20000
AFIX 0
O4 4 -0.290303 -0.309660 -0.123461 11.00000 0.03978 0.05989 =
0.04558 -0.00885 -0.00444 0.00621
O1 4 -0.426358 0.817292 0.234534 11.00000 0.06440 0.02611 =
0.05902 -0.00538 -0.00828 0.00343
O2 4 -0.562666 0.678098 0.164059 11.00000 0.07450 0.04502 =
0.06142 -0.00460 -0.03086 0.02068
O5 4 -0.239730 -0.614742 -0.216412 11.00000 0.05065 0.05624 =
0.04875 -0.01177 -0.00402 -0.01354
AFIX 147
H5A 2 -0.299893 -0.648244 -0.195867 11.00000 -1.50000
AFIX 0
C9 1 -0.425236 0.171149 0.359607 11.00000 0.04302 0.03764 =
0.03285 -0.00487 0.00050 -0.00081
AFIX 43
H9 2 -0.414877 0.037143 0.336265 11.00000 -1.20000
AFIX 0
C21 1 -0.183537 -0.393996 -0.120961 11.00000 0.03225 0.03780 =
0.03970 -0.00268 -0.00138 -0.00350
N1 3 -0.119864 -0.001410 0.012910 11.00000 0.04837 0.05653 =
0.05408 -0.01704 -0.00750 0.00699
AFIX 93
H1A 2 -0.108467 -0.117237 -0.011492 11.00000 -1.20000
H1B 2 -0.074509 0.014543 0.046444 11.00000 -1.20000
AFIX 0
C7 1 -0.596248 0.300620 0.283505 11.00000 0.03293 0.04531 =
0.03797 -0.00356 0.00060 -0.00112
AFIX 23
H7A 2 -0.645239 0.439490 0.276615 11.00000 -1.20000
H7B 2 -0.652970 0.173936 0.290583 11.00000 -1.20000
AFIX 0
N3 3 -0.226339 0.333806 0.034880 11.00000 0.05297 0.05166 =
0.03473 0.00031 -0.00120 0.01082
AFIX 43
H3 2 -0.282666 0.429630 0.022228 11.00000 -1.20000
AFIX 0
C5 1 -0.423568 0.414260 0.212802 11.00000 0.03412 0.02778 =
0.03017 -0.00353 -0.00403 0.00247
AFIX 13
H5 2 -0.365373 0.415084 0.248936 11.00000 -1.20000
AFIX 0
C1 1 -0.206470 0.151005 -0.001024 11.00000 0.04000 0.04844 =
0.03781 0.00154 0.00524 -0.00234
C18 1 -0.370265 0.409516 0.449472 11.00000 0.04787 0.04462 =
0.03199 -0.00329 0.00413 -0.00772
C8 1 -0.514957 0.333422 0.341384 11.00000 0.03591 0.04258 =
0.03312 -0.00328 0.00244 -0.00263
C6 1 -0.475687 0.658529 0.203208 11.00000 0.04597 0.02866 =
0.03384 -0.00002 0.00133 0.00490
C17 1 -0.279408 0.407498 0.502271 11.00000 0.05822 0.05691 =
0.03142 0.00193 0.00007 -0.01256
C3 1 -0.248459 0.492060 0.140036 11.00000 0.04546 0.03996 =
0.03818 -0.00799 0.00198 -0.00069
AFIX 23
H3A 2 -0.281198 0.635860 0.122926 11.00000 -1.20000
H3B 2 -0.202244 0.528282 0.178455 11.00000 -1.20000
AFIX 0
C22 1 -0.141570 -0.543404 -0.175814 11.00000 0.03942 0.03442 =
0.04395 -0.00238 -0.00415 0.00285
AFIX 13
H22 2 -0.099162 -0.680976 -0.158998 11.00000 -1.20000
AFIX 0
C10 1 -0.351618 0.211569 0.412876 11.00000 0.04594 0.04193 =
0.03058 0.00021 0.00049 -0.00216
C20 1 -0.531950 0.530759 0.377951 11.00000 0.04288 0.04238 =
0.04578 -0.00435 0.00302 0.00331
AFIX 43
H20 2 -0.591417 0.639014 0.365420 11.00000 -1.20000
AFIX 0
C23 1 -0.052272 -0.408206 -0.214995 11.00000 0.03625 0.04261 =
0.03678 -0.00487 -0.00819 -0.00174
C19 1 -0.461783 0.568414 0.432638 11.00000 0.05281 0.04985 =
0.04353 -0.01431 0.00536 0.00133
AFIX 43
H19 2 -0.475832 0.697361 0.457446 11.00000 -1.20000
AFIX 0
C2 1 -0.161194 0.385912 0.093654 11.00000 0.04105 0.05917 =
0.04111 -0.00768 0.00230 -0.00021
AFIX 23
H2C 2 -0.094118 0.492872 0.086193 11.00000 -1.20000
H2D 2 -0.125697 0.244935 0.111129 11.00000 -1.20000
AFIX 0
C28 1 -0.084161 -0.190534 -0.236850 11.00000 0.04425 0.04679 =
0.04973 0.00301 -0.00835 -0.00450
AFIX 43
H28 2 -0.156922 -0.121692 -0.224146 11.00000 -1.20000
AFIX 0
C16 1 -0.260636 0.565664 0.551105 11.00000 0.08790 0.07477 =
0.03643 -0.01055 -0.00147 -0.01849
AFIX 43
H16 2 -0.310550 0.695669 0.554885 11.00000 -1.20000
AFIX 0
C11 1 -0.244222 0.072606 0.439748 11.00000 0.05621 0.05000 =
0.04862 0.00280 -0.01139 0.00445
AFIX 23
H11A 2 -0.178196 0.061065 0.410275 11.00000 -1.20000
H11B 2 -0.270077 -0.081797 0.451409 11.00000 -1.20000
AFIX 0
C27 1 -0.008640 -0.073256 -0.277638 11.00000 0.07910 0.06425 =
0.05471 0.01149 -0.01469 -0.02786
AFIX 43
H27 2 -0.031618 0.072231 -0.292557 11.00000 -1.20000
AFIX 0
C12 1 -0.204265 0.212550 0.496602 11.00000 0.05830 0.05867 =
0.03642 0.00901 -0.00717 -0.01207
C13 1 -0.106576 0.171677 0.539452 11.00000 0.07430 0.07754 =
0.05352 0.01819 -0.02064 -0.01302
AFIX 43
H13 2 -0.055943 0.042603 0.535773 11.00000 -1.20000
AFIX 0
C26 1 0.100237 -0.172572 -0.295956 11.00000 0.07113 0.10009 =
0.05051 -0.00936 0.00955 -0.03714
AFIX 43
H26 2 0.149906 -0.096373 -0.324069 11.00000 -1.20000
AFIX 0
C24 1 0.058968 -0.503244 -0.232447 11.00000 0.04508 0.05798 =
0.05713 -0.01480 -0.00243 0.00578
AFIX 43
H24 2 0.083286 -0.647712 -0.217321 11.00000 -1.20000
AFIX 0
C14 1 -0.087194 0.329701 0.587816 11.00000 0.09014 0.09220 =
0.05234 0.01800 -0.03081 -0.02892
AFIX 43
H14 2 -0.021713 0.306989 0.616472 11.00000 -1.20000
AFIX 0
C15 1 -0.163082 0.519369 0.594150 11.00000 0.10472 0.09241 =
0.03711 -0.00591 -0.01537 -0.03736
AFIX 43
H15 2 -0.149245 0.619093 0.627800 11.00000 -1.20000
AFIX 0
C25 1 0.134472 -0.382283 -0.272695 11.00000 0.04685 0.10313 =
0.06396 -0.02497 0.01473 -0.01377
AFIX 43
H25 2 0.209552 -0.446358 -0.283789 11.00000 -1.20000
AFIX 0
C4 1 -0.355682 0.332954 0.155056 11.00000 0.04585 0.02768 =
0.03881 -0.00941 0.00184 0.00281
AFIX 23
H4C 2 -0.324445 0.177538 0.162284 11.00000 -1.20000
H4D 2 -0.413540 0.327599 0.119425 11.00000 -1.20000
HKLF 4
REM FA_SMA_Rt_Cu in P21 #4
REM R1 = 0.0343 for 2576 Fo > 4sig(Fo) and 0.0384 for all 2860 data
REM 335 parameters refined using 1 restraints
END
WGHT 0.0398 0.0000
REM Highest difference peak 0.115, deepest hole -0.127, 1-sigma level 0.029
Q1 1 -0.1742 0.7277 0.5019 11.00000 0.05 0.12
Q2 1 -0.4605 0.7929 0.2833 11.00000 0.05 0.10
Q3 1 -0.0648 0.6067 0.5762 11.00000 0.05 0.09
Q4 1 -0.3134 -0.1349 0.4830 11.00000 0.05 0.09
Q5 1 -0.3813 -0.3945 -0.1225 11.00000 0.05 0.09
Q6 1 -0.3581 -0.0001 0.4939 11.00000 0.05 0.09
Q7 1 -0.1633 -0.7674 -0.1414 11.00000 0.05 0.09
Q8 1 -0.3724 0.6739 0.1754 11.00000 0.05 0.09
Q9 1 -0.2865 -0.0650 -0.0641 11.00000 0.05 0.09
Q10 1 -0.3737 -0.0629 0.4448 11.00000 0.05 0.09
Q11 1 -0.2216 -0.2880 0.0047 11.00000 0.05 0.09
Q12 1 -0.1689 -0.1998 0.0615 11.00000 0.05 0.09
Q13 1 -0.1312 0.2801 -0.2859 11.00000 0.05 0.09
Q14 1 -0.2004 -0.3208 0.0138 11.00000 0.05 0.09
Q15 1 -0.3446 -0.1836 -0.0766 11.00000 0.05 0.09
Q16 1 -0.2611 -0.3346 0.4174 11.00000 0.05 0.08
Q17 1 -0.2447 0.0024 0.5604 11.00000 0.05 0.08
Q18 1 -0.1813 0.9197 0.1170 11.00000 0.05 0.08
Q19 1 -0.4546 0.7143 0.5376 11.00000 0.05 0.08
Q20 1 -0.1082 0.6506 0.5048 11.00000 0.05 0.08
REM The information below was added by Olex2.
REM
REM R1 = 0.0343 for 2576 Fo > 4sig(Fo) and 0.0384 for all 2860 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.12, deepest hole -0.13
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0384
REM R1_gt = 0.0343
REM wR_ref = 0.0815
REM GOOF = 0.988
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 2860
REM Reflections_gt = 2576
REM Parameters = n/a
REM Hole = -0.13
REM Peak = 0.12
REM Flack = -0.2(2)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.325
_oxdiff_exptl_absorpt_empirical_full_min 0.635
#######################################################################
#
# 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_fda_rma_rt_cu
_database_code_depnum_ccdc_archive 'CCDC 2047297'
loop_
_audit_author_name
_audit_author_address
'Rik Rani koner'
;IIT Mandi
India
;
_audit_update_record
;
2020-11-30 deposited with the CCDC. 2020-12-21 downloaded from the CCDC.
;
_audit_creation_date 2020-11-30
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C8 H7 O3, C20 H25 N4 O2'
_chemical_formula_sum 'C28 H32 N4 O5'
_chemical_formula_weight 504.58
_chemical_absolute_configuration unk
_chemical_melting_point ?
_chemical_oxdiff_formula 'C56 H68 N8 O12'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 4
_space_group_name_H-M_alt 'P 21'
_space_group_name_Hall 'P 2yb'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z'
_cell_length_a 10.8308(8)
_cell_length_b 5.7790(4)
_cell_length_c 21.3692(13)
_cell_angle_alpha 90.00
_cell_angle_beta 91.933(7)
_cell_angle_gamma 90.00
_cell_volume 1336.77(16)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 1317
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 66.6580
_cell_measurement_theta_min 4.0700
_exptl_absorpt_coefficient_mu 0.711
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.839
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 1.254
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description monoclinic
_exptl_crystal_F_000 536
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 1 6 0.0656
1 4 2 0.1137
0 0 -14 0.0396
0 0 14 0.0396
-6 -1 -6 0.0572
-6 1 -6 0.0639
6 0 -9 0.0329
-6 0 8 0.0350
6 0 5 0.0187
-2 -4 -1 0.0902
_exptl_crystal_size_max 0.223
_exptl_crystal_size_mid 0.095
_exptl_crystal_size_min 0.068
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5.9980 1.0016 5.9998 0.2018 0.9558 -0.0976
1.0040 4.0049 2.0101 0.0087 0.1222 -1.0796
0.0030 0.0032 -13.9896 -0.9815 -0.2089 0.1077
-0.0030 -0.0032 13.9896 0.9815 0.2089 -0.1077
-5.9978 -0.9984 -5.9972 -0.5588 0.6632 0.5097
-5.9955 1.0044 -5.9913 -0.6395 0.7768 -0.0053
5.9998 0.0005 -8.9946 -0.4525 -0.9438 -0.1368
-5.9996 -0.0002 7.9953 0.3824 0.9289 0.1445
5.9969 -0.0027 4.9950 0.5290 -0.7349 -0.2445
-2.0038 -4.0048 -1.0106 0.0317 0.0277 1.1063
_exptl_special_details
;
?
;
_diffrn_reflns_av_R_equivalents 0.0373
_diffrn_reflns_av_unetI/netI 0.0559
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 4
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 4185
_diffrn_reflns_theta_full 66.83
_diffrn_reflns_theta_max 66.83
_diffrn_reflns_theta_min 6.22
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type Eos
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -42.00 60.00 1.00 1.00 -- 25.57 -57.00 30.00 102
2 \w -27.00 64.00 1.00 1.00 -- 25.57 -57.00 120.00 91
3 \w -13.00 111.00 1.00 10.00 -- 66.78 -45.00 60.00 124
4 \w 104.00 144.00 1.00 10.00 -- 66.78 121.00 53.00 40
5 \w 5.00 98.00 1.00 10.00 -- 66.78 -61.00 -60.00 93
6 \w 68.00 127.00 1.00 10.00 -- 66.78 61.00-150.00 59
7 \w 93.00 137.00 1.00 35.00 -- 108.00 -21.00 -60.00 44
8 \w 53.00 90.00 1.00 35.00 -- 108.00-104.00 -30.00 37
9 \w 52.00 87.00 1.00 35.00 -- 108.00 -54.00 -90.00 35
10 \w 52.00 177.00 1.00 35.00 -- 108.00 32.00-180.00 125
11 \w 28.00 111.00 1.00 35.00 -- 108.00-104.00 30.00 83
12 \w 38.00 64.00 1.00 35.00 -- 108.00 -21.00 -60.00 26
13 \w 130.00 172.00 1.00 35.00 -- 108.00 54.00 120.00 42
14 \w 27.00 112.00 1.00 35.00 -- 108.00 -32.00-150.00 85
15 \w 68.00 96.00 1.00 35.00 -- 108.00 54.00 120.00 28
16 \w 105.00 147.00 1.00 35.00 -- 108.00 -54.00 -90.00 42
17 \w 119.00 157.00 1.00 35.00 -- 108.00 104.00 30.00 38
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0297642000
_diffrn_orient_matrix_UB_12 -0.0405001000
_diffrn_orient_matrix_UB_13 0.0701586000
_diffrn_orient_matrix_UB_21 -0.1349472000
_diffrn_orient_matrix_UB_22 0.0568509000
_diffrn_orient_matrix_UB_23 0.0149157000
_diffrn_orient_matrix_UB_31 -0.0344205000
_diffrn_orient_matrix_UB_32 -0.2570477000
_diffrn_orient_matrix_UB_33 -0.0077643000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_reflns_number_gt 2442
_reflns_number_total 2815
_reflns_odcompleteness_completeness 98.22
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_reflns_threshold_expression >2sigma(I)
_computing_cell_refinement 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2008)'
_computing_structure_solution 'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max 0.144
_refine_diff_density_min -0.141
_refine_diff_density_rms 0.036
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.0(3)
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.990
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 335
_refine_ls_number_reflns 2815
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0462
_refine_ls_R_factor_gt 0.0389
_refine_ls_restrained_S_all 0.990
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0887
_refine_ls_wR_factor_ref 0.0921
_refine_special_details
;Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.,SQUEEZE
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
At 1.5 times of:
All O(H) groups
2.a Ternary CH refined with riding coordinates:
C5(H5), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
N4(H4A,H4B), C7(H7A,H7B), C4(H4C,H4D), C3(H3A,H3B), C11(H11A,H11B), C2(H2C,H2D)
2.c Aromatic/amide H refined with riding coordinates:
N3(H3), C9(H9), C24(H24), C19(H19), C20(H20), C28(H28), C26(H26), C27(H27),
C13(H13), C15(H15), C25(H25), C16(H16), C14(H14)
2.d X=CH2 refined with riding coordinates:
N1(H1A,H1B), N2(H2A,H2B)
2.e Idealised tetrahedral OH refined as rotating group:
O5(H5A)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
O4 O 0.10581(18) 0.0780(4) 0.07685(9) 0.0486(5) Uani 1 d . . .
O1 O 0.5739(2) 0.3967(3) 0.23460(11) 0.0506(5) Uani 1 d . . .
O3 O 0.29048(18) 0.0229(4) 0.12338(9) 0.0496(5) Uani 1 d . . .
O5 O 0.2394(2) 0.3284(4) 0.21638(10) 0.0529(5) Uani 1 d . . .
H5A H 0.2952 0.3820 0.1958 0.079 Uiso 1 calc . . GR
N4 N 0.47370(19) 0.9638(4) 0.22536(9) 0.0338(4) Uani 1 d . . .
H4A H 0.4200 0.9631 0.1923 0.041 Uiso 1 calc . . R
H4B H 0.5056 1.1073 0.2286 0.041 Uiso 1 calc . . R
O2 O 0.4371(2) 0.5352(4) 0.16421(11) 0.0623(6) Uani 1 d . . .
N3 N 0.7731(2) 0.8805(5) 0.03495(11) 0.0470(6) Uani 1 d . . .
H3 H 0.7161 0.7856 0.0226 0.056 Uiso 1 calc . . R
N1 N 0.8803(2) 1.2155(5) 0.01282(13) 0.0545(6) Uani 1 d . . .
H1A H 0.9255 1.2004 0.0464 0.065 Uiso 1 calc . . R
H1B H 0.8915 1.3311 -0.0117 0.065 Uiso 1 calc . . R
N2 N 0.7235(2) 1.0895(6) -0.05296(12) 0.0540(6) Uani 1 d . . .
H2A H 0.7348 1.2071 -0.0768 0.065 Uiso 1 calc . . R
H2B H 0.6669 0.9903 -0.0626 0.065 Uiso 1 calc . . R
C23 C 0.0524(2) 0.1223(5) 0.21451(12) 0.0407(6) Uani 1 d . . .
C6 C 0.5241(2) 0.5550(5) 0.20341(12) 0.0367(5) Uani 1 d . . .
C21 C 0.1840(2) 0.1068(5) 0.12129(12) 0.0381(6) Uani 1 d . . .
C8 C 0.4856(2) 0.8810(5) 0.34122(12) 0.0365(5) Uani 1 d . . .
C18 C 0.6293(3) 0.8047(5) 0.44914(13) 0.0426(6) Uani 1 d . . .
C9 C 0.5743(2) 1.0422(5) 0.35972(12) 0.0384(5) Uani 1 d . . .
H9 H 0.5842 1.1769 0.3366 0.046 Uiso 1 calc . . R
C1 C 0.7938(2) 1.0611(6) -0.00116(13) 0.0411(6) Uani 1 d . . .
C7 C 0.4035(2) 0.9137(5) 0.28349(12) 0.0391(6) Uani 1 d . . .
H7A H 0.3546 0.7748 0.2767 0.047 Uiso 1 calc . . R
H7B H 0.3470 1.0405 0.2906 0.047 Uiso 1 calc . . R
C5 C 0.5758(2) 0.7994(4) 0.21261(11) 0.0318(5) Uani 1 d . . .
H5 H 0.6339 0.7985 0.2488 0.038 Uiso 1 calc . . R
C4 C 0.6443(2) 0.8802(5) 0.15522(12) 0.0385(5) Uani 1 d . . .
H4C H 0.5868 0.8859 0.1194 0.046 Uiso 1 calc . . R
H4D H 0.6754 1.0355 0.1626 0.046 Uiso 1 calc . . R
C3 C 0.7512(3) 0.7222(5) 0.14025(13) 0.0430(6) Uani 1 d . . .
H3A H 0.7186 0.5788 0.1228 0.052 Uiso 1 calc . . R
H3B H 0.7968 0.6851 0.1788 0.052 Uiso 1 calc . . R
C22 C 0.1414(3) 0.2554(5) 0.17553(13) 0.0407(6) Uani 1 d . . .
H22 H 0.0991 0.3925 0.1584 0.049 Uiso 1 calc . . R
C24 C 0.0837(3) -0.0968(6) 0.23647(14) 0.0475(6) Uani 1 d . . .
H24 H 0.1558 -0.1669 0.2235 0.057 Uiso 1 calc . . R
C17 C 0.7213(3) 0.8065(6) 0.50223(13) 0.0491(7) Uani 1 d . . .
C10 C 0.6483(3) 1.0016(5) 0.41292(12) 0.0394(6) Uani 1 d . . .
C19 C 0.5382(3) 0.6469(6) 0.43264(14) 0.0480(7) Uani 1 d . . .
H19 H 0.5242 0.5186 0.4577 0.058 Uiso 1 calc . . R
C11 C 0.7556(3) 1.1409(6) 0.43983(15) 0.0511(7) Uani 1 d . . .
H11A H 0.7296 1.2950 0.4517 0.061 Uiso 1 calc . . R
H11B H 0.8213 1.1532 0.4103 0.061 Uiso 1 calc . . R
C12 C 0.7961(3) 1.0007(6) 0.49659(14) 0.0519(8) Uani 1 d . . .
C20 C 0.4675(3) 0.6831(5) 0.37790(14) 0.0445(6) Uani 1 d . . .
H20 H 0.4078 0.5753 0.3655 0.053 Uiso 1 calc . . R
C2 C 0.8390(3) 0.8285(6) 0.09429(14) 0.0482(7) Uani 1 d . . .
H2C H 0.8742 0.9696 0.1118 0.058 Uiso 1 calc . . R
H2D H 0.9061 0.7216 0.0869 0.058 Uiso 1 calc . . R
C28 C -0.0593(3) 0.2166(7) 0.23254(15) 0.0540(8) Uani 1 d . . .
H28 H -0.0838 0.3610 0.2174 0.065 Uiso 1 calc . . R
C26 C -0.0998(4) -0.1134(10) 0.29562(17) 0.0739(12) Uani 1 d . . .
H26 H -0.1494 -0.1907 0.3235 0.089 Uiso 1 calc . . R
C27 C -0.1343(3) 0.0977(9) 0.27272(18) 0.0694(11) Uani 1 d . . .
H27 H -0.2088 0.1625 0.2842 0.083 Uiso 1 calc . . R
C13 C 0.8930(4) 1.0421(8) 0.53932(17) 0.0689(10) Uani 1 d . . .
H13 H 0.9434 1.1712 0.5355 0.083 Uiso 1 calc . . R
C15 C 0.8364(5) 0.6960(10) 0.59381(17) 0.0828(14) Uani 1 d . . .
H15 H 0.8503 0.5960 0.6274 0.099 Uiso 1 calc . . R
C25 C 0.0089(4) -0.2117(8) 0.27731(18) 0.0676(10) Uani 1 d . . .
H25 H 0.0322 -0.3566 0.2925 0.081 Uiso 1 calc . . R
C16 C 0.7395(4) 0.6492(8) 0.55117(15) 0.0687(10) Uani 1 d . . .
H16 H 0.6895 0.5195 0.5551 0.082 Uiso 1 calc . . R
C14 C 0.9125(5) 0.8862(10) 0.58786(18) 0.0794(13) Uani 1 d . . .
H14 H 0.9775 0.9096 0.6167 0.095 Uiso 1 calc . . R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O4 0.0403(9) 0.0617(13) 0.0429(10) -0.0052(10) -0.0122(7) -0.0002(10)
O1 0.0622(12) 0.0261(9) 0.0625(12) 0.0073(9) -0.0102(10) -0.0025(9)
O3 0.0389(9) 0.0613(13) 0.0478(10) -0.0086(10) -0.0091(7) 0.0054(10)
O5 0.0503(11) 0.0585(13) 0.0491(11) -0.0121(10) -0.0086(9) -0.0139(10)
N4 0.0382(10) 0.0283(10) 0.0342(10) 0.0022(8) -0.0095(8) -0.0030(8)
O2 0.0730(14) 0.0490(13) 0.0625(13) 0.0088(11) -0.0343(11) -0.0215(11)
N3 0.0543(13) 0.0523(14) 0.0340(11) 0.0008(11) -0.0044(10) -0.0110(12)
N1 0.0514(14) 0.0569(15) 0.0542(14) 0.0180(13) -0.0130(11) -0.0074(13)
N2 0.0557(14) 0.0604(17) 0.0452(13) 0.0068(12) -0.0104(11) -0.0072(14)
C23 0.0391(12) 0.0458(15) 0.0362(12) -0.0069(11) -0.0126(10) 0.0000(12)
C6 0.0456(13) 0.0289(12) 0.0350(12) 0.0007(10) -0.0055(10) -0.0073(11)
C21 0.0327(12) 0.0384(14) 0.0426(13) -0.0001(11) -0.0082(10) -0.0053(11)
C8 0.0347(11) 0.0403(13) 0.0344(12) 0.0029(11) -0.0003(9) 0.0024(11)
C18 0.0479(14) 0.0453(14) 0.0344(13) 0.0008(11) 0.0008(11) 0.0112(13)
C9 0.0430(12) 0.0385(14) 0.0336(12) 0.0044(10) -0.0013(9) -0.0003(11)
C1 0.0369(11) 0.0483(15) 0.0381(12) -0.0012(12) 0.0025(10) 0.0013(12)
C7 0.0324(11) 0.0445(14) 0.0402(13) 0.0035(11) -0.0026(10) -0.0030(11)
C5 0.0345(11) 0.0281(11) 0.0320(11) 0.0042(9) -0.0089(9) -0.0029(10)
C4 0.0458(13) 0.0296(12) 0.0397(13) 0.0081(10) -0.0022(10) -0.0014(11)
C3 0.0448(13) 0.0427(14) 0.0414(13) 0.0079(12) -0.0012(11) 0.0046(12)
C22 0.0413(13) 0.0372(14) 0.0429(14) -0.0016(11) -0.0091(11) 0.0017(11)
C24 0.0426(14) 0.0469(15) 0.0520(15) 0.0020(14) -0.0124(12) -0.0058(13)
C17 0.0594(17) 0.0578(18) 0.0298(13) -0.0013(12) -0.0037(11) 0.0189(15)
C10 0.0434(13) 0.0419(14) 0.0327(12) 0.0018(11) -0.0028(10) 0.0018(12)
C19 0.0533(15) 0.0463(16) 0.0445(14) 0.0131(12) 0.0042(12) -0.0013(13)
C11 0.0573(16) 0.0488(16) 0.0460(15) -0.0014(13) -0.0151(12) -0.0046(14)
C12 0.0575(16) 0.0584(19) 0.0389(14) -0.0075(14) -0.0114(12) 0.0139(16)
C20 0.0422(13) 0.0446(15) 0.0465(14) 0.0063(12) -0.0013(11) -0.0039(12)
C2 0.0428(13) 0.0625(19) 0.0390(13) 0.0079(13) -0.0045(11) 0.0009(14)
C28 0.0445(15) 0.0583(18) 0.0586(18) -0.0153(16) -0.0072(13) 0.0091(15)
C26 0.069(2) 0.102(3) 0.0503(18) -0.010(2) 0.0051(16) -0.039(3)
C27 0.0439(15) 0.101(3) 0.063(2) -0.029(2) 0.0094(14) -0.010(2)
C13 0.076(2) 0.073(2) 0.0558(19) -0.0157(18) -0.0260(16) 0.014(2)
C15 0.111(3) 0.098(3) 0.0375(16) 0.008(2) -0.0161(18) 0.041(3)
C25 0.078(2) 0.067(2) 0.0567(19) 0.0124(17) -0.0181(17) -0.027(2)
C16 0.096(3) 0.074(2) 0.0352(15) 0.0126(16) -0.0059(15) 0.023(2)
C14 0.093(3) 0.091(3) 0.0519(19) -0.015(2) -0.0334(19) 0.029(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O4 C21 1.262(3) . ?
O1 C6 1.244(3) . ?
O3 C21 1.250(3) . ?
O5 H5A 0.8200 . ?
O5 C22 1.416(3) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N4 C7 1.506(3) . ?
N4 C5 1.490(3) . ?
O2 C6 1.245(3) . ?
N3 H3 0.8600 . ?
N3 C1 1.322(4) . ?
N3 C2 1.466(4) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 C1 1.321(4) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?
N2 C1 1.332(4) . ?
C23 C22 1.506(4) . ?
C23 C24 1.389(4) . ?
C23 C28 1.393(4) . ?
C6 C5 1.529(3) . ?
C21 C22 1.527(4) . ?
C8 C9 1.387(4) . ?
C8 C7 1.508(3) . ?
C8 C20 1.404(4) . ?
C18 C17 1.484(4) . ?
C18 C10 1.396(4) . ?
C18 C19 1.381(5) . ?
C9 H9 0.9300 . ?
C9 C10 1.389(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C5 H5 0.9800 . ?
C5 C4 1.527(4) . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C4 C3 1.517(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.520(4) . ?
C22 H22 0.9800 . ?
C24 H24 0.9300 . ?
C24 C25 1.380(5) . ?
C17 C12 1.392(5) . ?
C17 C16 1.395(5) . ?
C10 C11 1.511(4) . ?
C19 H19 0.9300 . ?
C19 C20 1.392(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.512(4) . ?
C12 C13 1.388(5) . ?
C20 H20 0.9300 . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C28 H28 0.9300 . ?
C28 C27 1.384(6) . ?
C26 H26 0.9300 . ?
C26 C27 1.362(7) . ?
C26 C25 1.376(7) . ?
C27 H27 0.9300 . ?
C13 H13 0.9300 . ?
C13 C14 1.385(7) . ?
C15 H15 0.9300 . ?
C15 C16 1.393(7) . ?
C15 C14 1.383(8) . ?
C25 H25 0.9300 . ?
C16 H16 0.9300 . ?
C14 H14 0.9300 . ?
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 O5 H5A 109.5 . . ?
H4A N4 H4B 107.5 . . ?
C7 N4 H4A 108.5 . . ?
C7 N4 H4B 108.5 . . ?
C5 N4 H4A 108.5 . . ?
C5 N4 H4B 108.5 . . ?
C5 N4 C7 115.24(19) . . ?
C1 N3 H3 117.3 . . ?
C1 N3 C2 125.4(3) . . ?
C2 N3 H3 117.3 . . ?
H1A N1 H1B 120.0 . . ?
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C1 N2 H2A 120.0 . . ?
C1 N2 H2B 120.0 . . ?
C24 C23 C22 119.9(3) . . ?
C24 C23 C28 117.9(3) . . ?
C28 C23 C22 122.1(3) . . ?
O1 C6 O2 126.7(3) . . ?
O1 C6 C5 117.4(2) . . ?
O2 C6 C5 115.9(2) . . ?
O4 C21 C22 115.6(2) . . ?
O3 C21 O4 124.8(3) . . ?
O3 C21 C22 119.6(2) . . ?
C9 C8 C7 122.2(3) . . ?
C9 C8 C20 119.8(2) . . ?
C20 C8 C7 118.0(3) . . ?
C10 C18 C17 108.1(3) . . ?
C19 C18 C17 131.0(3) . . ?
C19 C18 C10 121.0(3) . . ?
C8 C9 H9 120.2 . . ?
C8 C9 C10 119.7(3) . . ?
C10 C9 H9 120.2 . . ?
N3 C1 N2 118.6(3) . . ?
N1 C1 N3 122.3(3) . . ?
N1 C1 N2 119.1(3) . . ?
N4 C7 C8 113.5(2) . . ?
N4 C7 H7A 108.9 . . ?
N4 C7 H7B 108.9 . . ?
C8 C7 H7A 108.9 . . ?
C8 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
N4 C5 C6 109.98(19) . . ?
N4 C5 H5 108.6 . . ?
N4 C5 C4 109.59(19) . . ?
C6 C5 H5 108.6 . . ?
C4 C5 C6 111.4(2) . . ?
C4 C5 H5 108.6 . . ?
C5 C4 H4C 109.1 . . ?
C5 C4 H4D 109.1 . . ?
H4C C4 H4D 107.9 . . ?
C3 C4 C5 112.3(2) . . ?
C3 C4 H4C 109.1 . . ?
C3 C4 H4D 109.1 . . ?
C4 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
C4 C3 C2 113.1(2) . . ?
H3A C3 H3B 107.8 . . ?
C2 C3 H3A 109.0 . . ?
C2 C3 H3B 109.0 . . ?
O5 C22 C23 107.0(2) . . ?
O5 C22 C21 113.3(2) . . ?
O5 C22 H22 108.7 . . ?
C23 C22 C21 110.4(2) . . ?
C23 C22 H22 108.7 . . ?
C21 C22 H22 108.7 . . ?
C23 C24 H24 119.7 . . ?
C25 C24 C23 120.7(3) . . ?
C25 C24 H24 119.7 . . ?
C12 C17 C18 108.5(3) . . ?
C12 C17 C16 121.5(3) . . ?
C16 C17 C18 130.0(4) . . ?
C18 C10 C11 110.4(2) . . ?
C9 C10 C18 120.0(3) . . ?
C9 C10 C11 129.5(3) . . ?
C18 C19 H19 120.5 . . ?
C18 C19 C20 118.9(3) . . ?
C20 C19 H19 120.5 . . ?
C10 C11 H11A 111.2 . . ?
C10 C11 H11B 111.2 . . ?
C10 C11 C12 102.6(3) . . ?
H11A C11 H11B 109.2 . . ?
C12 C11 H11A 111.2 . . ?
C12 C11 H11B 111.2 . . ?
C17 C12 C11 110.3(3) . . ?
C13 C12 C17 120.8(3) . . ?
C13 C12 C11 128.9(4) . . ?
C8 C20 H20 119.7 . . ?
C19 C20 C8 120.6(3) . . ?
C19 C20 H20 119.7 . . ?
N3 C2 C3 110.1(2) . . ?
N3 C2 H2C 109.6 . . ?
N3 C2 H2D 109.6 . . ?
C3 C2 H2C 109.6 . . ?
C3 C2 H2D 109.6 . . ?
H2C C2 H2D 108.1 . . ?
C23 C28 H28 119.6 . . ?
C27 C28 C23 120.7(4) . . ?
C27 C28 H28 119.6 . . ?
C27 C26 H26 120.2 . . ?
C27 C26 C25 119.7(4) . . ?
C25 C26 H26 120.2 . . ?
C28 C27 H27 119.7 . . ?
C26 C27 C28 120.5(4) . . ?
C26 C27 H27 119.7 . . ?
C12 C13 H13 120.9 . . ?
C14 C13 C12 118.3(4) . . ?
C14 C13 H13 120.9 . . ?
C16 C15 H15 118.9 . . ?
C14 C15 H15 118.9 . . ?
C14 C15 C16 122.2(4) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 C24 120.5(4) . . ?
C26 C25 H25 119.8 . . ?
C17 C16 H16 121.7 . . ?
C15 C16 C17 116.6(5) . . ?
C15 C16 H16 121.7 . . ?
C13 C14 H14 119.7 . . ?
C15 C14 C13 120.6(4) . . ?
C15 C14 H14 119.7 . . ?
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
O5 H5A O2 0.82 1.92 2.723(3) 168.0 .
N4 H4B O1 0.90 1.83 2.732(3) 178.6 1_565
N1 H1A O4 0.86 2.16 2.871(3) 140.3 1_665
N1 H1B O4 0.86 1.99 2.847(3) 170.6 2_665
_smtbx_masks_special_details ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.278 0.000 0.657 7.2 0.0 ?
2 0.500 -0.535 0.000 70.5 15.9 ?
3 0.722 0.500 0.343 7.2 0.0 ?
_iucr_refine_instructions_details
;
TITL fda_rma_rt_cu_a.res in P2(1)
REM Old TITL FDA_RMA_RT_Cu in P21/m #11
REM SHELXT solution in P2(1)
REM R1 0.142, Rweak 0.039, Alpha 0.002, Orientation as input
REM Flack x = -0.007 ( 0.401 ) from Parsons' quotients
REM Formula found by SHELXT: C28 N2 O7
CELL 1.54184 10.830797 5.779036 21.369207 90 91.933 90
ZERR 2 0.000779 0.000422 0.001338 0 0.0065 0
LATT -1
SYMM -X,0.5+Y,-Z
SFAC C H N O
UNIT 56 64 8 10
EQIV $1 +X,1+Y,+Z
EQIV $2 1+X,1+Y,+Z
EQIV $3 1-X,1.5+Y,-Z
L.S. 30
PLAN 20
HTAB O5 O2
HTAB N4 O1_$1
HTAB N1 O4_$2
HTAB N1 O4_$3
BOND $H
LIST 6
fmap 2
acta
OMIT -2 -3 22
OMIT -3 0 3
OMIT 0 0 7
OMIT 0 0 2
OMIT -2 0 1
OMIT 0 -2 10
OMIT 3 0 6
OMIT -1 -3 8
OMIT 0 0 8
OMIT 6 0 6
OMIT -1 -1 7
OMIT -1 0 8
OMIT 2 0 7
OMIT 5 -1 5
OMIT 0 0 12
OMIT -6 0 5
OMIT -4 0 2
OMIT -12 0 9
OMIT -4 0 4
OMIT -4 0 6
OMIT 2 0 0
OMIT -3 -3 4
OMIT -1 0 10
OMIT 7 -3 7
OMIT 0 -2 9
OMIT 2 -1 12
OMIT 5 0 7
OMIT 5 0 3
OMIT 1 -1 5
OMIT 1 0 8
OMIT 5 -1 0
OMIT -1 -1 8
OMIT 6 -1 2
OMIT 5 -2 18
OMIT 4 0 7
OMIT -3 -4 7
OMIT 5 0 6
OMIT 4 -2 4
OMIT 4 -2 7
OMIT 2 -2 8
OMIT -1 -1 10
OMIT -9 -2 16
OMIT 2 -1 1
OMIT 5 -2 21
OMIT 0 -2 3
OMIT 4 0 4
OMIT -5 -1 12
OMIT -5 -1 20
OMIT -9 -1 17
OMIT 0 -1 7
OMIT -6 -5 3
OMIT 2 0 10
OMIT 0 -1 14
OMIT -3 -2 3
OMIT -1 0 11
OMIT 1 0 10
OMIT 3 -2 0
OMIT 3 -1 11
OMIT 0 0 11
OMIT 2 -2 1
OMIT 2 -1 2
OMIT -1 0 12
OMIT -3 -3 11
OMIT 1 -1 2
OMIT -5 0 5
OMIT -6 -2 4
OMIT 5 -1 1
OMIT 2 0 5
OMIT -10 0 16
OMIT 4 -4 17
OMIT 0 -4 17
OMIT -1 -1 6
OMIT 0 0 13
OMIT 2 1 5
OMIT -4 -4 19
OMIT 4 -2 0
OMIT -1 -2 1
OMIT 3 -2 7
OMIT -2 0 12
OMIT -10 4 5
OMIT -4 2 17
OMIT -9 0 16
OMIT -11 -1 6
OMIT -1 0 1
OMIT -8 0 16
OMIT 1 0 20
OMIT 0 -1 6
OMIT 8 -3 6
OMIT -4 -2 3
OMIT -5 -3 21
OMIT -7 -3 14
OMIT -3 -3 1
OMIT -1 -2 10
OMIT 0 -1 17
OMIT -3 -2 1
OMIT -1 0 2
OMIT 4 0 10
OMIT 4 -2 5
OMIT 8 -1 0
OMIT 3 -1 2
OMIT -7 -2 7
OMIT 1 1 6
OMIT -6 1 4
OMIT 5 0 4
REM
REM
REM
WGHT 0.039300
FVAR 8.53826
O4 4 0.105813 0.078023 0.076852 11.00000 0.04030 0.06170 =
0.04294 -0.00519 -0.01220 -0.00025
O1 4 0.573933 0.396710 0.234604 11.00000 0.06225 0.02615 =
0.06248 0.00731 -0.01018 -0.00253
O3 4 0.290481 0.022927 0.123375 11.00000 0.03893 0.06128 =
0.04776 -0.00865 -0.00906 0.00542
O5 4 0.239374 0.328412 0.216381 11.00000 0.05028 0.05854 =
0.04911 -0.01209 -0.00865 -0.01392
AFIX 147
H5A 2 0.295199 0.382015 0.195826 11.00000 -1.50000
AFIX 0
N4 3 0.473704 0.963810 0.225362 11.00000 0.03816 0.02831 =
0.03416 0.00217 -0.00948 -0.00301
AFIX 23
H4A 2 0.420048 0.963051 0.192273 11.00000 -1.20000
H4B 2 0.505562 1.107315 0.228597 11.00000 -1.20000
AFIX 0
O2 4 0.437055 0.535168 0.164206 11.00000 0.07299 0.04904 =
0.06248 0.00876 -0.03427 -0.02148
N3 3 0.773051 0.880485 0.034950 11.00000 0.05435 0.05231 =
0.03401 0.00076 -0.00439 -0.01098
AFIX 43
H3 2 0.716107 0.785620 0.022599 11.00000 -1.20000
AFIX 0
N1 3 0.880325 1.215466 0.012817 11.00000 0.05143 0.05687 =
0.05422 0.01803 -0.01295 -0.00741
AFIX 93
H1A 2 0.925527 1.200359 0.046433 11.00000 -1.20000
H1B 2 0.891465 1.331083 -0.011694 11.00000 -1.20000
AFIX 0
N2 3 0.723531 1.089550 -0.052956 11.00000 0.05570 0.06039 =
0.04522 0.00676 -0.01039 -0.00719
AFIX 93
H2A 2 0.734830 1.207148 -0.076752 11.00000 -1.20000
H2B 2 0.666862 0.990303 -0.062599 11.00000 -1.20000
AFIX 0
C23 1 0.052367 0.122253 0.214506 11.00000 0.03914 0.04584 =
0.03625 -0.00693 -0.01264 0.00003
C6 1 0.524121 0.555032 0.203407 11.00000 0.04561 0.02892 =
0.03502 0.00072 -0.00546 -0.00729
C21 1 0.184050 0.106815 0.121288 11.00000 0.03273 0.03837 =
0.04263 -0.00008 -0.00818 -0.00527
C8 1 0.485584 0.880964 0.341218 11.00000 0.03469 0.04027 =
0.03439 0.00292 -0.00033 0.00244
C18 1 0.629312 0.804652 0.449143 11.00000 0.04793 0.04530 =
0.03444 0.00084 0.00078 0.01122
C9 1 0.574310 1.042207 0.359718 11.00000 0.04302 0.03847 =
0.03361 0.00441 -0.00130 -0.00027
AFIX 43
H9 2 0.584223 1.176897 0.336606 11.00000 -1.20000
AFIX 0
C1 1 0.793806 1.061126 -0.001164 11.00000 0.03687 0.04831 =
0.03812 -0.00123 0.00249 0.00133
C7 1 0.403548 0.913688 0.283489 11.00000 0.03237 0.04449 =
0.04019 0.00345 -0.00262 -0.00304
AFIX 23
H7A 2 0.354617 0.774830 0.276657 11.00000 -1.20000
H7B 2 0.347047 1.040461 0.290644 11.00000 -1.20000
AFIX 0
C5 1 0.575811 0.799377 0.212607 11.00000 0.03445 0.02813 =
0.03200 0.00417 -0.00888 -0.00293
AFIX 13
H5 2 0.633859 0.798533 0.248792 11.00000 -1.20000
AFIX 0
C4 1 0.644257 0.880155 0.155223 11.00000 0.04579 0.02958 =
0.03974 0.00805 -0.00223 -0.00135
AFIX 23
H4C 2 0.586830 0.885854 0.119429 11.00000 -1.20000
H4D 2 0.675371 1.035512 0.162600 11.00000 -1.20000
AFIX 0
C3 1 0.751153 0.722205 0.140253 11.00000 0.04477 0.04269 =
0.04143 0.00789 -0.00116 0.00460
AFIX 23
H3A 2 0.718600 0.578767 0.122849 11.00000 -1.20000
H3B 2 0.796835 0.685147 0.178777 11.00000 -1.20000
AFIX 0
C22 1 0.141375 0.255391 0.175530 11.00000 0.04134 0.03720 =
0.04290 -0.00157 -0.00915 0.00168
AFIX 13
H22 2 0.099132 0.392527 0.158381 11.00000 -1.20000
AFIX 0
C24 1 0.083693 -0.096846 0.236474 11.00000 0.04262 0.04687 =
0.05201 0.00201 -0.01240 -0.00582
AFIX 43
H24 2 0.155800 -0.166947 0.223547 11.00000 -1.20000
AFIX 0
C17 1 0.721305 0.806513 0.502235 11.00000 0.05936 0.05778 =
0.02979 -0.00129 -0.00371 0.01891
C10 1 0.648298 1.001623 0.412920 11.00000 0.04341 0.04190 =
0.03269 0.00175 -0.00275 0.00179
C19 1 0.538162 0.646904 0.432642 11.00000 0.05327 0.04628 =
0.04450 0.01310 0.00421 -0.00133
AFIX 43
H19 2 0.524211 0.518565 0.457691 11.00000 -1.20000
AFIX 0
C11 1 0.755585 1.140913 0.439834 11.00000 0.05733 0.04882 =
0.04605 -0.00141 -0.01507 -0.00459
AFIX 23
H11A 2 0.729627 1.295030 0.451656 11.00000 -1.20000
H11B 2 0.821269 1.153157 0.410258 11.00000 -1.20000
AFIX 0
C12 1 0.796135 1.000663 0.496593 11.00000 0.05749 0.05842 =
0.03887 -0.00750 -0.01140 0.01386
C20 1 0.467503 0.683115 0.377903 11.00000 0.04219 0.04465 =
0.04654 0.00629 -0.00127 -0.00391
AFIX 43
H20 2 0.407792 0.575296 0.365526 11.00000 -1.20000
AFIX 0
C2 1 0.839040 0.828487 0.094289 11.00000 0.04276 0.06248 =
0.03902 0.00793 -0.00450 0.00087
AFIX 23
H2C 2 0.874212 0.969563 0.111845 11.00000 -1.20000
H2D 2 0.906072 0.721632 0.086925 11.00000 -1.20000
AFIX 0
C28 1 -0.059329 0.216574 0.232545 11.00000 0.04451 0.05834 =
0.05857 -0.01533 -0.00721 0.00909
AFIX 43
H28 2 -0.083771 0.360960 0.217429 11.00000 -1.20000
AFIX 0
C26 1 -0.099767 -0.113405 0.295620 11.00000 0.06936 0.10232 =
0.05032 -0.01008 0.00506 -0.03907
AFIX 43
H26 2 -0.149400 -0.190690 0.323496 11.00000 -1.20000
AFIX 0
C27 1 -0.134311 0.097710 0.272719 11.00000 0.04389 0.10122 =
0.06349 -0.02880 0.00938 -0.00976
AFIX 43
H27 2 -0.208847 0.162461 0.284167 11.00000 -1.20000
AFIX 0
C13 1 0.892955 1.042092 0.539321 11.00000 0.07620 0.07295 =
0.05576 -0.01571 -0.02602 0.01444
AFIX 43
H13 2 0.943386 1.171200 0.535457 11.00000 -1.20000
AFIX 0
C15 1 0.836364 0.696015 0.593807 11.00000 0.11107 0.09840 =
0.03753 0.00800 -0.01612 0.04134
AFIX 43
H15 2 0.850287 0.596025 0.627407 11.00000 -1.20000
AFIX 0
C25 1 0.008899 -0.211690 0.277306 11.00000 0.07809 0.06676 =
0.05670 0.01240 -0.01812 -0.02735
AFIX 43
H25 2 0.032152 -0.356568 0.292543 11.00000 -1.20000
AFIX 0
C16 1 0.739510 0.649161 0.551173 11.00000 0.09628 0.07391 =
0.03525 0.01258 -0.00590 0.02307
AFIX 43
H16 2 0.689500 0.519523 0.555130 11.00000 -1.20000
AFIX 0
C14 1 0.912519 0.886201 0.587856 11.00000 0.09340 0.09056 =
0.05189 -0.01543 -0.03336 0.02870
AFIX 43
H14 2 0.977497 0.909650 0.616724 11.00000 -1.20000
HKLF 4
REM fda_rma_rt_cu_a.res in P2(1)
REM R1 = 0.0389 for 2442 Fo > 4sig(Fo) and 0.0462 for all 2815 data
REM 335 parameters refined using 1 restraints
END
WGHT 0.0395 0.0000
REM Highest difference peak 0.144, deepest hole -0.141, 1-sigma level 0.036
Q1 1 0.0204 0.0822 0.0860 11.00000 0.05 0.14
Q2 1 0.6532 0.6621 -0.0177 11.00000 0.05 0.12
Q3 1 0.6398 0.6297 -0.0365 11.00000 0.05 0.12
Q4 1 0.0997 -0.0397 0.0814 11.00000 0.05 0.11
Q5 1 -0.1719 -0.1726 0.2416 11.00000 0.05 0.11
Q6 1 0.5513 0.7022 -0.0309 11.00000 0.05 0.11
Q7 1 0.5633 0.8427 -0.0121 11.00000 0.05 0.11
Q8 1 0.8055 0.5358 0.6909 11.00000 0.05 0.11
Q9 1 0.3211 0.4252 0.2735 11.00000 0.05 0.11
Q10 1 -0.1927 0.3511 0.2494 11.00000 0.05 0.11
Q11 1 1.0021 1.2034 0.0312 11.00000 0.05 0.11
Q12 1 0.1799 0.4320 0.1402 11.00000 0.05 0.11
Q13 1 0.7787 0.5728 0.2601 11.00000 0.05 0.10
Q14 1 0.5787 0.5483 -0.0114 11.00000 0.05 0.10
Q15 1 0.8158 1.4960 0.4175 11.00000 0.05 0.10
Q16 1 0.7857 1.4294 0.4247 11.00000 0.05 0.10
Q17 1 0.2883 0.6967 0.1702 11.00000 0.05 0.10
Q18 1 -0.2012 0.4756 0.2936 11.00000 0.05 0.10
Q19 1 0.7126 1.1465 -0.1532 11.00000 0.05 0.10
Q20 1 0.0591 -0.2773 0.1540 11.00000 0.05 0.10
REM The information below was added by Olex2.
REM
REM R1 = 0.0389 for 2442 Fo > 4sig(Fo) and 0.0462 for all 2815 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.14, deepest hole -0.14
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0462
REM R1_gt = 0.0389
REM wR_ref = 0.0921
REM GOOF = 0.990
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 2815
REM Reflections_gt = 2442
REM Parameters = n/a
REM Hole = -0.14
REM Peak = 0.14
REM Flack = 0.0(3)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.361
_oxdiff_exptl_absorpt_empirical_full_min 0.807