Molecular replacement for small-molecule crystal structure determination from X-ray and electron diffraction data with reduced resolution.
Gorelik, Tatiana E.; Lukat, Peer; Kleeberg, Christian; Blankenfeldt, Wulf; Mueller, Rolf; Acta crystallographica. Section A, Foundations and advances 79 (2023) 504–514; doi:10.1107/S2053273323008458

data_2312320
_publ_section_title
;
 Molecular replacement for small-molecule crystal structure determination
 from X-ray and electron diffraction data with reduced resolution.
;
_journal_issue                   'Pt 6'
_journal_name_full
'Acta crystallographica. Section A, Foundations and advances'
_journal_page_first              504
_journal_page_last               514
_journal_paper_doi               10.1107/S2053273323008458
_journal_volume                  79
_journal_year                    2023
_chemical_formula_moiety         '2(C26 H32 Cl N7 O5)'
_chemical_formula_sum            'C26 H32 Cl N7 O5'
_chemical_formula_weight         558.04
_chemical_name_common            BI-3812
_chemical_name_systematic
1-(5-chloro-4-((8-methoxy-1-methyl-3-(2-(methylamino)-2-oxoethoxy)-2-oxo-1,2-dihydroquinolin-6-yl)amino)pyrimidin-2-yl)-N,N-dimethylpiperidine-4-carboxamide
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-10-06
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_cell_angle_alpha                108.22
_cell_angle_beta                 103.75
_cell_angle_gamma                107.49
_cell_formula_units_Z            1
_cell_length_a                   8.433
_cell_length_b                   13.424
_cell_length_c                   13.680
_cell_measurement_reflns_used    12039
_cell_measurement_temperature    80
_cell_measurement_theta_max      0.683
_cell_measurement_theta_min      0.062
_cell_volume                     1305.596
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.721
_diffrn_measured_fraction_theta_max 0.721
_diffrn_measurement_device_type  'GLACIOS TEM'
_diffrn_measurement_method       'Continuous Electron Diffraction'
_diffrn_radiation_wavelength     0.0251
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_Laue_measured_fraction_full 0.721
_diffrn_reflns_Laue_measured_fraction_max 0.721
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3313
_diffrn_reflns_point_group_measured_fraction_full 0.721
_diffrn_reflns_point_group_measured_fraction_max 0.721
_diffrn_reflns_theta_full        0.683
_diffrn_reflns_theta_max         0.683
_diffrn_reflns_theta_min         0.062
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    0.710
_exptl_crystal_description       platelet
_exptl_crystal_F_000             112
_exptl_crystal_size_max          0.005
_exptl_crystal_size_mid          0.001
_exptl_crystal_size_min          0.0001
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       2676(22)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   3.613
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         1681
_refine_ls_number_restraints     248
_refine_ls_restrained_S_all      3.441
_refine_ls_R_factor_all          0.3847
_refine_ls_R_factor_gt           0.3668
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.6942
_refine_ls_wR_factor_ref         0.7102
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1398
_reflns_number_total             1681
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lu5029sup1.cif
_cod_data_source_block           II
_cod_depositor_comments
'Adding full bibliography for 2312319--2312320.cif.'
_cod_original_cell_volume        1305.7
_cod_database_code               2312320
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1-C2 \\sim C2-C3 \\sim C3-C4 \\sim C4-C5 \\sim C4-C9 \\sim C9-C8 \\sim C8-C7
\\sim C7-C6 \\sim C5-C6 \\sim C15-
 C16 \\sim C16-C17
 with sigma of 0.02
 C1-C3 \\sim C2-C4 \\sim C3-C5 \\sim C5-C1 \\sim C5-C7 \\sim C6-C8 \\sim C7-C9
\\sim C8-C4 \\sim C9-C5 \\sim C4-C6
 \\sim C15-C17 \\sim C15-C18 \\sim C17-C18
 with sigma of 0.02
 C5-N2 \\sim C1-N2 \\sim C15-N4 \\sim C18-N4 \\sim C18-N5 \\sim N5-C17
 with sigma of 0.02
 C8-N3 \\sim C15-N3 \\sim C13-N1 \\sim C14-N1
 with sigma of 0.02
 N6-C18 \\sim N6-C23 \\sim N6-C19 \\sim N7-C24 \\sim N7-C25 \\sim N7-C26
 with sigma of 0.02
 C18-C19 \\sim C19-C23 \\sim C23-C18 \\sim C24-C25 \\sim C25-C26 \\sim C26-C24
 with sigma of 0.02
 C12-C13 \\sim C19-C20 \\sim C20-C21 \\sim C21-C22 \\sim C22-C23 \\sim C21-C24
 with sigma of 0.02
 C15-Cl1 \\sim C17-Cl1
 with sigma of 0.02
 C19-C21 \\sim C20-C22 \\sim C21-C23 \\sim C23-C19
 with sigma of 0.02
 C2-O2 \\sim O2-C12 \\sim C6-O4 \\sim O4-C11
 with sigma of 0.02
 C6-C11 \\sim C2-C12
 with sigma of 0.02
 C13-O1 \\sim C1-O3 \\sim C24-O5
 with sigma of 0.02
 C13-C14 \\sim C15-C8
 with sigma of 0.02
3. Restrained planarity
 C1, C2, C3, C4, C5, C6, C7, C8, C9, O2, C10, O4, N3
 with sigma of 0.1
 N3, Cl1, N6, C15, C16, C17, N5, C18, N4
 with sigma of 0.1
4.a Ternary CH refined with riding coordinates:
 C21(H21)
4.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C19(H19A,H19B), C20(H20A,H20B), C22(H22A,H22B), C23(H23A,H23B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C9(H9), C17(H17), N1(H1), N3(H3A)
4.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              61052
_shelx_hkl_checksum              70264
_olex2_submission_special_instructions 'No special instructions were received'