Towards validating new enzymatic routes for synthetic conversion: 7,10-bis-<i>O</i>-(2,2,2-trichloroethoxycarbonyl)-10-deacetyl baccatin III–ethyl acetate–water (1/1/1)
Wang, Li; Li, Ya-jun; Li, Zheng-wei; Acta Crystallographica Section C 71 (2015) –; doi:10.1107/S2053229614027399

data_2019865
_publ_section_title
;
 Towards validating new enzymatic routes for synthetic conversion:
 7,10-bis-<i>O</i>-(2,2,2-trichloroethoxycarbonyl)-10-deacetyl baccatin
 III--ethyl acetate--water (1/1/1)
;
_journal_coeditor_code           QS3041
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229614027399
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C34 H38 Cl6 O14, C4 H8 O2, H2 O'
_chemical_formula_moiety         'C34 H38 Cl6 O14, C4 H8 O2, H2 O'
_chemical_formula_sum            'C39 H48 Cl6 O17'
_chemical_formula_weight         1001.47
_chemical_name_systematic
;
7,10-Bis-<i>O</i>-(2,2,2-trichloroethoxycarbonyl)-10-deacetyl baccatin
III--ethyl acetate--water (1/1/1)
;
_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                   14.7029(12)
_cell_length_b                   16.6256(14)
_cell_length_c                   18.8428(15)
_cell_measurement_reflns_used    2132
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.795
_cell_measurement_theta_min      2.485
_cell_volume                     4606.0(7)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
Mercury (Macrae <i>et al.</i>, 2006)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_sigmaI/netI    0.0856
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23553
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  0.8428
_exptl_absorpt_correction_T_min  0.8256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>REQAB</i>; Jacobson, 1998)
;
_exptl_crystal_colour            colorless
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_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.40
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_refine_diff_density_min         -0.222
_refine_ls_abs_structure_details
;
Flack (1983), 3609 Friedel pairs
;
_refine_ls_abs_structure_Flack   -0.04(6)
_refine_ls_extinction_coef       0.0028(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL97 (Sheldrick, 2008)
;
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         8208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0436P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1152
_reflns_number_gt                5474
_reflns_number_total             8208
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            qs3041sup1.cf
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_cod_database_code               2019865
_cod_database_fobs_code          2019865