Total Synthesis and Structural Determination of XR774, a Tyrosine Kinase Inhibitor.
Tatsuta, Kuniaki; Sekine, Daisuke; Hayama, Shinichi; Kataoka, Yasuhiro; Hayashi, Shinya; Hosokawa, Seijiro; The Journal of organic chemistry 83 (2018) 7010–7018; doi:10.1021/acs.joc.7b02997

data_4033479
_publ_section_title
;
 Total Synthesis and Structural Determination of XR774, a Tyrosine Kinase
 Inhibitor.
;
_journal_issue                   13
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              7010
_journal_page_last               7018
_journal_paper_doi               10.1021/acs.joc.7b02997
_journal_volume                  83
_journal_year                    2018
_chemical_formula_moiety         'C26 H30 I2 O6'
_chemical_formula_sum            'C26 H30 I2 O6'
_chemical_formula_weight         692.30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                93.3776(14)
_cell_angle_beta                 101.1847(14)
_cell_angle_gamma                104.6735(13)
_cell_formula_units_Z            2
_cell_length_a                   8.34194(18)
_cell_length_b                   11.9310(2)
_cell_length_c                   14.0513(3)
_cell_measurement_reflns_used    12586
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      68.23
_cell_measurement_theta_min      3.23
_cell_volume                     1318.56(5)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1008
_diffrn_reflns_av_unetI/netI     0.1009
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14917
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.229
_diffrn_reflns_theta_min         3.227
_exptl_absorpt_coefficient_mu    19.046
_exptl_absorpt_correction_T_max  0.264
_exptl_absorpt_correction_T_min  0.016
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.670
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.060
_refine_diff_density_min         -1.593
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+1.4202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1216
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4026
_reflns_number_total             4724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b02997_si_006.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 4033477--4033481.cif.'
_cod_original_cell_volume        1318.55(5)
_cod_database_code               4033479
_shelx_estimated_absorpt_t_min   0.028
_shelx_estimated_absorpt_t_max   0.349
_shelxl_version_number           2014/6
_shelx_res_checksum              14173
_shelx_hkl_checksum              49121