The first total synthesis of roquefortine D
Wei-Chuan Chen; Madeleine M. Joullié; Tetrahedron Letters 39 (1998) 8401–8404; doi:10.1016/S0040-4039(98)01957-1

data_1513173
_publ_section_title
;
 The first total synthesis of roquefortine D
;
_journal_issue                   46
_journal_name_full               'Tetrahedron Letters'
_journal_page_first              8401
_journal_page_last               8404
_journal_paper_doi               10.1016/S0040-4039(98)01957-1
_journal_volume                  39
_journal_year                    1998
_chemical_formula_sum            'C27 H38 N2 O6'
_chemical_formula_weight         486.59
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 113.312(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5732(5)
_cell_length_b                   13.7918(9)
_cell_length_c                   10.4851(7)
_cell_measurement_temperature    200(2)
_cell_volume                     1404.15(15)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'image plate area detector'
_diffrn_measurement_device_type  'Rigaku R-AXIS IIc'
_diffrn_measurement_method       'phi oscillations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9626
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.11(192)
_refine_ls_extinction_coef       0.0394(47)
_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_all   1.134
_refine_ls_goodness_of_fit_obs   1.177
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         4722
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.134
_refine_ls_restrained_S_obs      1.177
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_obs          0.0743
_refine_ls_shift/esd_max         8.311
_refine_ls_shift/esd_mean        0.029
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0803P)^2^+0.6235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1892
_refine_ls_wR_factor_obs         0.1791
_reflns_number_observed          3967
_reflns_number_total             4722
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            734.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0803P)^2^+0.6235P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0803P)^2^+0.6235P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21       '
_cod_database_code               1513173