(<i>M</i>)- and (<i>P</i>)-8-[(1<i>S</i>,2<i>R</i>)-2-hydroxy-1-methyl-2-phenylethyl]-8-methyl-8,9-dihydro-7<i>H</i>-dinaphth[2,1-<i>c</i>:1',2'-<i>e</i>]azepinium bromide solvates
Schneider, Monica; Linden, Anthony; Rippert, Andreas, J.; Acta Crystallographica Section C 56 (2000) 1004–1006; doi:10.1107/S0108270100006739

data_2011282
_publ_section_title
;(<i>M</i>)- and
 (<i>P</i>)-8-[(1<i>S</i>,2<i>R</i>)-2-hydroxy-1-methyl-2-phenylethyl]-8-methyl-8,9-dihydro-7<i>H</i>-dinaphth[2,1-<i>c</i>:1',2'-<i>e</i>]azepinium
 bromide solvates
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1004
_journal_page_last               1006
_journal_paper_doi               10.1107/S0108270100006739
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          'C32 H30 N O + , Br - , 3C3 H6 O'
_chemical_formula_moiety         'C32 H30 N O + , Br - , 3C3 H6 O'
_chemical_formula_sum            'C41 H48 Br N O4'
_chemical_formula_weight         698.70
_chemical_melting_point          477(4)
_chemical_name_systematic
;
(M)-8-[(1S,2R)-2-hydroxy-1-methyl-2-phenylethyl]-8-methyl-
8,9-dihydro-7H-dinaphth[2,1-c:1',2'-e]azepinium bromide acetone (1/3) solvate
;
_space_group_IT_number           76
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4w'
_symmetry_space_group_name_H-M   'P 41'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.2515(16)
_cell_length_b                   16.2515(16)
_cell_length_c                   13.7964(19)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    173.0(10)
_cell_measurement_theta_max      17.0
_cell_measurement_theta_min      12.5
_cell_volume                     3643.8(7)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software (Molecular
Structure Corporation, 1991)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.0(10)
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device_type  'Rigaku AFC-5R'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode generator'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71069
_diffrn_reflns_av_R_equivalents  .055
_diffrn_reflns_av_sigmaI/netI    .181
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8931
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.169
_exptl_absorpt_correction_T_max  .792
_exptl_absorpt_correction_T_min  .700
_exptl_absorpt_correction_type   \y-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          .45
_exptl_crystal_size_mid          .28
_exptl_crystal_size_min          .20
_refine_diff_density_max         .46
_refine_diff_density_min         -.41
_refine_ls_abs_structure_details 'Flack (1983), 3673 Friedel pairs'
_refine_ls_abs_structure_Flack   -.017(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         8032
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          .197
_refine_ls_R_factor_gt           .065
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0719P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .169
_reflns_number_gt                3936
_reflns_number_total             8032
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1391.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '473-481' was changed to '477(4)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '473-481' was changed to '477(4)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_Hall     'P 41'
_cod_database_code               2011282
_cod_database_fobs_code          2011282