Identification, Characterization, Synthesis, and Strategy for Minimization of Potential Impurities Observed in the Synthesis of Solithromycin
Zhong, Zhihong; Du, Chong; Luo, Zhonghua; Song, Shuaihua; Liao, Gaohong; Yao, Jia; Goldmann, Siegfried; Wang, Zhongqing; Organic Process Research & Development 21 (2017) 1371–; doi:10.1021/acs.oprd.7b00201

data_1547550
_publ_section_title
;
 Identification, Characterization, Synthesis, and Strategy for
 Minimization of Potential Impurities Observed in the Synthesis of
 Solithromycin
;
_journal_issue                   9
_journal_name_full               'Organic Process Research &amp; Development'
_journal_page_first              1371
_journal_paper_doi               10.1021/acs.oprd.7b00201
_journal_volume                  21
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_sum            'C43 H65 F N6 O10'
_chemical_formula_weight         845.01
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.60670(10)
_cell_length_b                   19.0255(2)
_cell_length_c                   28.0976(2)
_cell_measurement_reflns_used    18457
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      65.3590
_cell_measurement_theta_min      3.1180
_cell_volume                     4600.89(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.5058
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            44718
_diffrn_reflns_theta_full        65.66
_diffrn_reflns_theta_max         65.66
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_T_max  0.8974
_exptl_absorpt_correction_T_min  0.8090
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.160
_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   0.03(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         7871
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+0.6576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0862
_reflns_number_gt                7179
_reflns_number_total             7871
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            op7b00201_si_002.cif
_cod_data_source_block           solithromycin
_cod_database_code               1547550