X-ray investigations of potential β-blockers. IV
Domagała, Małgorzata; Rybarczyk, Agnieszka J.; Olszak, Tomasz A.; Brzezińska, Elżbieta; Acta Crystallographica Section C 55 (1999) 1003–1005; doi:10.1107/S0108270199002383

data_2008604
_publ_section_title
;
 X-ray investigations of potential \b-blockers. IV
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1003
_journal_page_last               1005
_journal_paper_doi               10.1107/S0108270199002383
_journal_volume                  55
_journal_year                    1999
_chemical_formula_analytical     'C13 H22 Cl N O4'
_chemical_formula_moiety         'C13 H20 N O3 1+, Cl 1-, H2O'
_chemical_formula_sum            'C13 H22 Cl N O4'
_chemical_formula_weight         291.77
_chemical_name_systematic
;
6,7-dihydroxy-1-(2-methoxypropyl)-1,2,3,4-tetrahydroisoquinolinium
chloride hydrate
;
_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'
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8412(6)
_cell_length_b                   15.6366(7)
_cell_length_c                   9.4044(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      36.24
_cell_measurement_theta_min      27.52
_cell_volume                     1447.18(13)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
 1989a)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1989b)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'PARST97 (Nardelli, 1983b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC-5S'
_diffrn_measurement_method       \w-scan
_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  0.023
_diffrn_reflns_av_sigmaI/netI    0.024
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8586
_diffrn_reflns_theta_full        60.06
_diffrn_reflns_theta_max         60.05
_diffrn_reflns_theta_min         5.31
_diffrn_standards_decay_%        '<2.6, corrected'
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.436
_exptl_absorpt_correction_T_max  0.805
_exptl_absorpt_correction_T_min  0.646
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(Meulenar & Tompa, 1965)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.193
_refine_diff_density_min         -0.171
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.10(2)
_refine_ls_extinction_coef       0.0004(5)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         2155
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.035
_refine_ls_R_factor_gt           0.029
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0569P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.080
_reflns_number_gt                1880
_reflns_number_total             2155
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            os1043.cif
_cod_data_source_block           eb27i
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0569P)^2^] 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^)+(0.0569P)^2^]
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        1447.20(10)
_cod_original_formula_sum        'C13 H22 Cl1 N1 O4'
_cod_database_code               2008604