11,12-Seco-12,13-didehydromultiflorine Perchlorate Hydrate
Dutkiewicz, G.; Kubicki, M.; Borowiak, T.; Wysocka, W.; Acta Crystallographica Section C 51 (1995) 1182–1184; doi:10.1107/S0108270194011650

data_2003515
_publ_section_title
;
 11,12-Seco-12,13-didehydromultiflorine Perchlorate Hydrate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1182
_journal_page_last               1184
_journal_paper_doi               10.1107/S0108270194011650
_journal_volume                  51
_journal_year                    1995
_chemical_formula_moiety         'C15 H23 N2 O1 1+, Cl1 O4 1-, H2 O'
_chemical_formula_sum            'C15 H25 Cl N2 O6'
_chemical_formula_weight         364.82
_chemical_name_systematic
;
11,12-seco-12,13-didehydromultiflorine perchlorate hydrate
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.53(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.014(2)
_cell_length_b                   8.633(2)
_cell_length_c                   12.600(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.1
_cell_measurement_theta_min      11.0
_cell_volume                     871.7(4)
_computing_cell_refinement       'Kuma KM-4 User's Guide (Kuma, 1991)'
_computing_data_collection       'Kuma KM-4 User's Guide (Kuma, 1991)'
_computing_data_reduction        'Kuma KM-4 User's Guide (Kuma, 1991)'
_computing_molecular_graphics
' Stereochemical Workstation Operation Manual (Siemens, 1989)'
_computing_publication_material  'SHELXL93 (Sheldrick, 1994)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Kuma KM-4 four-circle diffractometer'
_diffrn_measurement_method       \w/2\q
_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  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            1481
_diffrn_reflns_theta_max         60.01
_diffrn_reflns_theta_min         3.51
_diffrn_standards_decay_%        2.3
_diffrn_standards_interval_count 200
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.243
_exptl_absorpt_correction_type   ' empirical (DIFABS; Walker & Stuart, 1983)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       needle
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.202
_refine_ls_abs_structure_details 'Flack (1983); \c = 0.01(3)'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.076
_refine_ls_goodness_of_fit_obs   1.118
_refine_ls_hydrogen_treatment
' noref, except for H16, H1W1, H1W2 which were refined isotropically'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         1313
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.710
_refine_ls_restrained_S_obs      1.191
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_obs          0.0360
_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^)+(0.0735P)~2~+0.1331P]
where P = (F~o~^2^+2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1741
_refine_ls_wR_factor_obs         0.1069
_reflns_number_observed          1079
_reflns_number_total             1380
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            ab1207.cif
_cod_data_source_block           semu
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2003515