<i>tert</i>-Butyl (2<i>S</i>)-2-(9<i>H</i>-fluoren-9-ylmethoxycarbonylamino)-3-(3',4'-dimethoxyphenyl)propionate chloroform sesquisolvate
Clegg, William; Elsegood, Mark R. J.; Acta Crystallographica Section E 59 (2003) o1946–o1948; doi:10.1107/S1600536803025819

data_2202409
_publ_section_title
;<i>tert</i>-Butyl
 (2<i>S</i>)-2-(9<i>H</i>-fluoren-9-ylmethoxycarbonylamino)-3-(3',4'-dimethoxyphenyl)propionate
 chloroform sesquisolvate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1946
_journal_page_last               o1948
_journal_paper_doi               10.1107/S1600536803025819
_journal_volume                  59
_journal_year                    2003
_chemical_formula_moiety         'C30 H33 N O6, 1.5 C H Cl3'
_chemical_formula_sum            'C31.5 H34.5 Cl4.5 N O6'
_chemical_formula_weight         682.63
_chemical_name_systematic
;(2S)-2-(9H-Fluoren-9-ylmethoxycarbonylamino)-3-(3',4'-dimethoxyphenyl)propionic
acid
 tert-butyl ester chloroform sesquisolvate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 98.435(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.1419(11)
_cell_length_b                   5.3779(6)
_cell_length_c                   24.926(2)
_cell_measurement_reflns_used    56
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      24.9
_cell_measurement_theta_min      19.2
_cell_volume                     1610.0(3)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1988)'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Stoe-Siemens four-circle diffractometer'
_diffrn_measurement_method
'\w/\q scans with on-line profile fitting (Clegg, 1981)'
_diffrn_radiation_monochromator  '8 micron Ni filter'
_diffrn_radiation_source         'Bede Microsource'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            8184
_diffrn_reflns_theta_full        67.21
_diffrn_reflns_theta_max         67.21
_diffrn_reflns_theta_min         3.59
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    4.091
_exptl_absorpt_correction_T_max  0.721
_exptl_absorpt_correction_T_min  0.571
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SHELXTL; Sheldrick, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             710
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.275
_refine_ls_abs_structure_details 'Flack (1983), 2019 Friedel pairs'
_refine_ls_abs_structure_Flack   0.2(3)
_refine_ls_extinction_coef       0.0100(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         5020
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0531
_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^)+(0.0588P)^2^+1.03P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1531
_reflns_number_gt                4567
_reflns_number_total             5020
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6382.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C31.50 H34.50 Cl4.50 N O6'
_cod_database_code               2202409