Absolute Configuration of Mutilin, 5-Acetylmutilin and 5-Bromoacetylmutilin
Pilati, T.; Cravotto, G.; Palmisano, G.; Acta Crystallographica Section C 51 (1995) 2676–2680; doi:10.1107/S0108270195008602

data_2004304
_publ_section_title
;
 Absolute Configuration of Mutilin, 5-Acetylmutilin and
 5-Bromoacetylmutilin
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2676
_journal_page_last               2680
_journal_paper_doi               10.1107/S0108270195008602
_journal_volume                  51
_journal_year                    1995
_chemical_formula_sum            'C22 H33 Br O4'
_chemical_formula_weight         441.39
_chemical_melting_point          174
_chemical_name_common            5-bromoacetilmutilin
_chemical_name_systematic
;S-(3a\a,4\b,5\a,6\a,8\b,9\a,9\a\b,10S*]-5-bromoacetate-6-ethenyloctahydro-5,8-
dihydroxy-4,6,9,10-tetramethyl-3a,9-propano-3aH-cyclopentacycloocten-1(4H)-one
;
_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'
_cell_angle_alpha                90.00
_cell_angle_beta                 109.266(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3200(10)
_cell_length_b                   11.2510(10)
_cell_length_c                   10.6710(10)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.15
_cell_measurement_theta_min      3.62
_cell_volume                     1056.29(18)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Fait,, 1991)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\q/2\q scan'
_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  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0703
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3909
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        5.50
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.970
_exptl_absorpt_correction_T_max  0.458
_exptl_absorpt_correction_T_min  0.397
_exptl_absorpt_correction_type
'Empirical \y scan, SHELXL/PC (Sheldrick, 1990)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.239
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.017(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.074
_refine_ls_hydrogen_treatment
;
H atoms of methyl and ethyl groups were calculated, all the others
were refined isotropically, by imposing restraints on the
X-H bond distance (DFIX of SHELXL93).
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         3677
_refine_ls_number_restraints     14
_refine_ls_restrained_S_obs      1.072
_refine_ls_R_factor_obs          0.0444
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0310P)^2^+0.1348P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0912
_refine_ls_wR_factor_obs         0.0776
_reflns_number_observed          2407
_reflns_number_total             3677
_reflns_observed_criterion       '> 2. sigma(I) '
_cod_data_source_file            na1195.cif
_cod_data_source_block           3
_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_enum 1527 2010-12-29 10:47:43Z saulius 

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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0310P)^2^+0.1348P] 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^)+(0.0310P)^2^+0.1348P] where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1056.3(2)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2004304