Commercialization and Late-Stage Development of a Semisynthetic Antifungal API: Anidulafungin/d-Fructose (Eraxis)
Norris, Timothy; VanAlsten, John; Hubbs, Stephen; Ewing, Marcus; Cai, Weiling; Jorgensen, Matthew L.; Bordner, Jon; Jensen, Grace O.; Organic Process Research & Development 12 (2008) 447–; doi:10.1021/op800055h

data_1504997
_publ_section_title
;
 Commercialization and Late-Stage Development of a Semisynthetic
 Antifungal API: Anidulafungin/d-Fructose (Eraxis)
;
_journal_issue                   3
_journal_name_full               'Organic Process Research &amp; Development'
_journal_page_first              447
_journal_paper_doi               10.1021/op800055h
_journal_volume                  12
_journal_year                    2008
_chemical_formula_sum            'C30 H27 N3 O3'
_chemical_formula_weight         477.55
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 99.3790(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   52.7951(12)
_cell_length_b                   7.8456(2)
_cell_length_c                   12.2836(2)
_cell_measurement_reflns_used    4789
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      58.74
_cell_measurement_theta_min      5.70
_cell_volume                     5019.96(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Montel multilayer optics'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9738
_diffrn_reflns_theta_full        58.94
_diffrn_reflns_theta_max         58.94
_diffrn_reflns_theta_min         5.70
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            translucent
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       NEEDLE
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.00040(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         3286
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0688
_refine_ls_shift/su_max          0.259
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1342P)^2^+4.4201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1955
_refine_ls_wR_factor_ref         0.2172
_reflns_number_gt                2434
_reflns_number_total             3286
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            op800055h-file001.cif
_cod_data_source_block           i649
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1504997