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_2312319
_publ_section_title
;
 Molecular replacement for small-molecule crystal structure determination
 from X-ray and electron diffraction data with reduced resolution.
;
_journal_coeditor_code           LU5029
_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         'C26 H32 Cl N7 O5, 5(H2 O)'
_chemical_formula_sum            'C26 H42 Cl N7 O10'
_chemical_formula_weight         648.11
_chemical_name_common            'BI-3812, pentahydrate'
_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   mixed
_audit_creation_date             2023-01-10
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                83.865(2)
_cell_angle_beta                 75.600(3)
_cell_angle_gamma                80.454(4)
_cell_formula_units_Z            2
_cell_length_a                   8.948(2)
_cell_length_b                   12.190(2)
_cell_length_c                   14.881(2)
_cell_measurement_reflns_used    17627
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      27.821
_cell_measurement_theta_min      1.481
_cell_volume                     1546.7(5)
_computing_cell_refinement       XDS
_computing_data_reduction        XDS
_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)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.661
_diffrn_measurement_device_type  P11
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.61992
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 0.903
_diffrn_reflns_Laue_measured_fraction_max 0.661
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            55502
_diffrn_reflns_point_group_measured_fraction_full 0.903
_diffrn_reflns_point_group_measured_fraction_max 0.661
_diffrn_reflns_theta_full        21.836
_diffrn_reflns_theta_max         27.821
_diffrn_reflns_theta_min         1.481
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       platelet
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         7314
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0753P)^2^+0.4490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1211
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6940
_reflns_number_total             7314
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lu5029sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 2312319--2312320.cif.'
_cod_original_cell_volume        1546.7(6)
_cod_database_code               2312319
_cod_database_fobs_code          2312319
_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
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O7-H7A = O7-H7B
 0.84 with sigma of 0.01
 O8-H8A = O8-H8B
 0.84 with sigma of 0.01
 O9-H9A = O9-H9B
 0.84 with sigma of 0.01
 O9A-H9AB = O9A-H9AA
 0.84 with sigma of 0.01
 O10-H10D = O10-H10E
 0.84 with sigma of 0.01
 O10A-H10F = O10A-H10G
 0.84 with sigma of 0.01
 H7A-H7B
 1.33 with sigma of 0.02
 H8A-H8B
 1.33 with sigma of 0.02
 H9A-H9B
 1.33 with sigma of 0.02
 H9AA-H9AB
 1.33 with sigma of 0.02
 H10D-H10E
 1.33 with sigma of 0.02
 H10F-H10G
 1.33 with sigma of 0.02
 C12-O4 \\sim C12-O4A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O9) = Uanis(O9A)
Uanis(O4) = Uanis(O4A)
4. Others
 Sof(O4A)=1-FVAR(1)
 Sof(O4)=FVAR(1)
 Sof(O9A)=Sof(H9AA)=Sof(H9AB)=1-FVAR(2)
 Sof(O9)=Sof(H9A)=Sof(H9B)=FVAR(2)
 Sof(O10A)=Sof(H10F)=Sof(H10G)=1-FVAR(3)
 Sof(O10)=Sof(H10D)=Sof(H10E)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C20(H20)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C18(H18A,H18B), C19(H19A,H19B), C21(H21A,H21B), C22(H22A,H22B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C7(H7), C17(H17)
5.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              1448
_shelx_hkl_checksum              45771
_olex2_submission_special_instructions 'No special instructions were received'