(<i>S</i>)-1-Acetoxymethyl-2-acetyl-1,2,3,4-tetrahydro-6,7-dimethoxy-1-methylisoquinoline
Maurin, J. K.; Czarnocki, Z.; Paluchowska, B.; Acta Crystallographica Section C 52 (1996) 953–955; doi:10.1107/S0108270195014491

data_2004706
_publ_section_title
(<i>S</i>)-1-Acetoxymethyl-2-acetyl-1,2,3,4-tetrahydro-6,7-dimethoxy-1-methylisoquinoline
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              953
_journal_page_last               955
_journal_paper_doi               10.1107/S0108270195014491
_journal_volume                  52
_journal_year                    1996
_chemical_formula_sum            'C17 H23 N O5'
_chemical_formula_weight         321.36
_chemical_melting_point          408.0(10)
_chemical_name_systematic
;
(S)-1-acetoxymethyl-2-acetyl-1-methyl-
1,2,3,4-tetrahydro-6,7-dimethoxyisoquinoline
;
_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                 101.120(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.0060(10)
_cell_length_b                   12.097(2)
_cell_length_c                   8.7940(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      20
_cell_volume                     835.7(2)
_computing_cell_refinement       'Kuma KM-4 software'
_computing_data_collection       'Kuma KM-4 Software (Kuma, 1991)'
_computing_data_reduction        'Kuma KM-4 software'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'KUMA KM-4 \k-axis four-circle'
_diffrn_measurement_method       'profile data from \q-\w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1972
_diffrn_reflns_theta_max         84.95
_diffrn_reflns_theta_min         5.13
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.165
_refine_diff_density_min         -0.150
_refine_ls_abs_structure_details 'Flack (1983) parameter = 0.14(24)'
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_extinction_coef       0.050(4)
_refine_ls_extinction_method     SHELXL93
_refine_ls_goodness_of_fit_all   1.033
_refine_ls_goodness_of_fit_obs   1.079
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         1874
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_restrained_S_obs      1.079
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_obs          0.0355
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0747P)^2^ + 0.0354P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1024
_refine_ls_wR_factor_obs         0.0967
_reflns_number_observed          1583
_reflns_number_total             1874
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            cf1035.cif
_cod_data_source_block           zb06
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '407-409' was changed to '408.0(10)'
- the average value was taken and precision was estimated.

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 
;
_cod_original_sg_symbol_Hall     'P 2y1'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2004706