Structural Biology-Inspired Discovery of Novel KRAS-PDEδ Inhibitors.
Jiang, Yan; Zhuang, Chunlin; Chen, Long; Lu, Junjie; Dong, Guoqiang; Miao, Zhenyuan; Zhang, Wannian; Li, Jian; Sheng, Chunquan; Journal of medicinal chemistry 60 (2017) 9400–9406; doi:10.1021/acs.jmedchem.7b01243

data_1547519
_publ_section_title
;
 Structural Biology-Inspired Discovery of Novel KRAS-PDE\d Inhibitors.
;
_journal_issue                   22
_journal_name_full               'Journal of medicinal chemistry'
_journal_page_first              9400
_journal_page_last               9406
_journal_paper_doi               10.1021/acs.jmedchem.7b01243
_journal_volume                  60
_journal_year                    2017
_chemical_formula_sum            'C38 H39 F2 N5 O3'
_chemical_formula_weight         651.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 110.903(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.1734(5)
_cell_length_b                   11.7178(4)
_cell_length_c                   15.5279(6)
_cell_measurement_reflns_used    3194
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      69.47
_cell_measurement_theta_min      3.05
_cell_volume                     2069.21(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_unetI/netI     0.0939
_diffrn_reflns_Laue_measured_fraction_full 0.900
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9462
_diffrn_reflns_point_group_measured_fraction_full 0.731
_diffrn_reflns_point_group_measured_fraction_max 0.731
_diffrn_reflns_theta_full        62.485
_diffrn_reflns_theta_max         62.485
_diffrn_reflns_theta_min         3.046
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.394
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.046
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
; 
 Flack x determined using 1154 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         4832
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0881
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1984P)^2^+0.0355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2507
_refine_ls_wR_factor_ref         0.2672
_reflns_Friedel_coverage         0.539
_reflns_Friedel_fraction_full    0.542
_reflns_Friedel_fraction_max     0.542
_reflns_number_gt                3973
_reflns_number_total             4832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jm7b01243_si_003.cif
_cod_data_source_block           cu_61227a
_cod_depositor_comments          'Adding full bibliography for 1547519.cif.'
_cod_database_code               1547519
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.900
_shelx_estimated_absorpt_t_max   0.942
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              48032
_shelx_hkl_checksum              28608