A Dihydromorphine-6-<i>O</i>-sulfate
Brock, C. P.; Kottayil, S.; Butterfield, D. A.; Crooks, P. A.; Acta Crystallographica Section C 52 (1996) 122–125; doi:10.1107/S0108270195010250

data_2004374
_publ_section_title
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 A Dihydromorphine-6-<i>O</i>-sulfate
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_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              122
_journal_page_last               125
_journal_paper_doi               10.1107/S0108270195010250
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         'C19 H23 N O7 S'
_chemical_formula_sum            'C19 H23 N O7 S'
_chemical_formula_weight         409.46
_chemical_name_systematic
;
3-O-Acetyl-7,8-dihydromorphine-6-O-sulfate
;
_chemical_temperature_decomposition_gt 573.15
_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                   9.3020(8)
_cell_length_b                   14.0800(10)
_cell_length_c                   14.1587(12)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    296.0(10)
_cell_measurement_theta_max      12.8
_cell_measurement_theta_min      10.6
_cell_volume                     1854.4(3)
_computing_cell_refinement       'CAD-4 VAX/PC'
_computing_data_collection       'CAD-4 VAX/PC (Enraf-Nonius, 1988)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.0(10)
_diffrn_measurement_device       'Enraf-Nonius CAD4-VAX'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_sigmaI/netI    0.0939
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1869
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        6
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.21
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description
'Tablet, short parallel to c with major faces {001}, {111} and {012}'
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.251
_refine_ls_abs_structure_details
;
The absolute configuration was chosen to match that expected from the
synthetic pathway
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.007
_refine_ls_goodness_of_fit_obs   1.163
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         1851
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1287
_refine_ls_R_factor_obs          0.0419
_refine_ls_shift/esd_max         0.065
_refine_ls_shift/esd_mean        0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0677P)^2^]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1224
_refine_ls_wR_factor_obs         0.0994
_reflns_number_observed          1078
_reflns_number_total             1869
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            cr1191.cif
_cod_data_source_block           CROOKS2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition_gt' since the value was
specified 'more than' ('>') a certain temperature. The value '> 300_C
(dec.)' was changed to '573.15' - it was converted from degrees
Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
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_cod_database_code               2004374