Hydrogen-bonded and π-interaction assembly in two 8-alkoxycarbonyl-1,8-diazabicyclo[5.4.0]undec-7-enium chloride salts
Mesto, E.; Quaranta, E.; Acta Crystallographica Section C 69 (2013) 444–447; doi:10.1107/S0108270113005970

data_2018895
_publ_section_title
;
 Hydrogen-bonded and \p-interaction assembly in two
 8-alkoxycarbonyl-1,8-diazabicyclo[5.4.0]undec-7-enium chloride salts
;
_journal_coeditor_code           CU3025
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              444
_journal_page_last               447
_journal_paper_doi               10.1107/S0108270113005970
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C11 H19 N2 O2 + , Cl - , H2 O'
_chemical_formula_moiety         'C11 H19 N2 O2 +, Cl -, H2 O'
_chemical_formula_sum            'C11 H21 Cl N2 O3'
_chemical_formula_weight         264.75
_chemical_name_systematic
;
8-Methcarbonyl-1,8-diazabicyclo[5.4.0]undec-7-enium chloride monohydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90.237(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.6506(4)
_cell_length_b                   15.5432(10)
_cell_length_c                   13.2041(10)
_cell_measurement_reflns_used    3652
_cell_measurement_temperature    298
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     1364.92(16)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>, 2008)'
_computing_publication_material  'CRYSTALS (Betteridge <i>et al.</i>, 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>, 2003)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device       area
_diffrn_measurement_device_type  'Bruker Kappa APEXII area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11826
_diffrn_reflns_theta_full        25.047
_diffrn_reflns_theta_max         30.545
_diffrn_reflns_theta_min         2.024
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.280
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.750
_exptl_crystal_size_mid          0.650
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.25
_refine_diff_density_min         -0.16
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2457
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.0006192
_refine_ls_shift/su_mean         0.0000411
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting (Prince, 1982)
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
 A~i~ are:
 0.871 1.05 0.637 0.264 0.809E-01
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0766
_refine_ls_wR_factor_gt          0.0499
_refine_ls_wR_factor_ref         0.0467
_reflns_number_gt                2701
_reflns_number_total             3855
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cu3025.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C11 H21 Cl1 N2 O3'
_cod_database_code               2018895
_cod_database_fobs_code          2018895