Structure of kopsine: methyl 3-hydroxy-22-oxokopsan-1-carboxylate
Watt, W.; Ghosh, R.; Seal, T.; Mukherjee, B.; Acta Crystallographica Section C 49 (1993) 171–173; doi:10.1107/S0108270192010035

data_2002104
_publ_contact_author
;
    Watt, William
    Research Laboratories,
    The Upjohn Company,
    Kalamazoo,
    MI 49007
    USA
;
_publ_section_title
;
 Structure of kopsine: methyl 3-hydroxy-22-oxokopsan-1-carboxylate
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              171
_journal_page_last               173
_journal_paper_doi               10.1107/S0108270192010035
_journal_volume                  49
_journal_year                    1993
_chemical_formula_sum            'C22 H24 N2 O4'
_chemical_formula_weight         380.43
_chemical_name_systematic
;
 Methyl 3-Hydroxy-22-oxokopsan-1-carboxylate
;
_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'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.193(3)
_cell_length_b                   11.9660(10)
_cell_length_c                   14.802(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    158
_cell_measurement_theta_max      68
_cell_measurement_theta_min      60
_cell_volume                     1805.4(7)
_computing_cell_refinement
;
performed using the program of Duchamp (1977)
;
_computing_data_reduction        'CRYM (Duchamp, 1984)'
_computing_structure_refinement  'CRYM (Duchamp, 1984)'
_computing_structure_solution
;
MULTAN (Main, Fiske, Hull, Lessinger, Germain, Declercq & Woolfson, 1980)
;
_diffrn_ambient_temperature      158
_diffrn_measurement_device       'Siemens P2~1~'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            1775
_diffrn_reflns_theta_max         68
_diffrn_reflns_theta_min         1
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 80
_diffrn_standards_number         10
_exptl_absorpt_coefficient_mu    0.699
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.40
_exptl_crystal_description       'chunky block'
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.48
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.32
_refine_ls_abs_structure_details
;
The absolute configuration was established by nmr
(Guggisberg, Gorman, Bycroft \& Schmid, 1969)
;
_refine_ls_goodness_of_fit_all   4.80
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         1772
_refine_ls_R_factor_all          0.047
_refine_ls_R_factor_obs          0.045
_refine_ls_shift/esd_max         0.020
_refine_ls_shift/esd_mean        0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[\s^2^(F^2^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.123
_refine_ls_wR_factor_obs         0.122
_reflns_number_observed          1689
_reflns_number_total             1775
_reflns_observed_criterion       refl_observed_if_I_>_3.0sigma(I)
_cod_data_source_file            cd1025.cif
_cod_data_source_block           cd1025
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(F^2^)]' 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^(F^2^)]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2002104