An Alternative Scalable Process for the Synthesis of the Key Intermediate of Omarigliptin
Sun, Guodong; Wei, Mingjie; Luo, Zhonghua; Liu, Yongjun; Chen, Zhijun; Wang, Zhongqing; Organic Process Research & Development 20 (2016) 2074–; doi:10.1021/acs.oprd.6b00295

data_1545004
_publ_section_title
;
 An Alternative Scalable Process for the Synthesis of the Key Intermediate
 of Omarigliptin
;
_journal_issue                   12
_journal_name_full               'Organic Process Research &amp; Development'
_journal_page_first              2074
_journal_paper_doi               10.1021/acs.oprd.6b00295
_journal_volume                  20
_journal_year                    2016
_chemical_formula_sum            'C16 H18 F2 I N O3'
_chemical_formula_weight         437.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_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                   5.1315(6)
_cell_length_b                   14.0490(14)
_cell_length_c                   23.6852(19)
_cell_measurement_temperature    293(2)
_cell_volume                     1707.5(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_sigmaI/netI    0.0598
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            5753
_diffrn_reflns_theta_full        68.39
_diffrn_reflns_theta_max         68.39
_diffrn_reflns_theta_min         3.66
_exptl_absorpt_coefficient_mu    65.111
_exptl_crystal_density_diffrn    3.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1512
_refine_diff_density_max         1.222
_refine_diff_density_min         -1.072
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.019(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         2822
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0713P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1204
_reflns_number_gt                2399
_reflns_number_total             2822
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            op6b00295_si_002.cif
_cod_data_source_block           exp_9658
_cod_depositor_comments
;

2019-03-17
Changing absurd Z value.                 miguel
;
_cod_original_formula_units_Z            18
_cod_database_code               1545004