4,11-Bis(acetamido)-7,14-dimethyl-4,11-diaza-1,8-diazoniacyclotetradecane diperchlorate dihydrate
Choi, Ki-Young; Lee, Han-Hyoung; Smyth, Douglas R.; Suh, Il-Hwan; Tiekink, Edward R. T.; Acta Crystallographica Section E 57 (2001) o480–o482; doi:10.1107/S1600536801007073

data_2200367
_publ_section_title
;
 4,11-Bis(acetamido)-7,14-dimethyl-4,11-diaza-1,8-diazoniacyclotetradecane
 diperchlorate dihydrate
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o480
_journal_page_last               o482
_journal_paper_doi               10.1107/S1600536801007073
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          'C16 H36 N6 O2 2+, 2Cl O4 1-, 2H2O'
_chemical_formula_moiety         'C16 H36 N6 O2 2+, 2Cl O4 1-, 2H2O'
_chemical_formula_sum            'C16 H40 Cl2 N6 O12'
_chemical_formula_weight         579.43
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 90.250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.576(3)
_cell_length_b                   10.877(6)
_cell_length_c                   14.314(2)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    173
_cell_measurement_theta_max      14.6
_cell_measurement_theta_min      7.5
_cell_volume                     2580.7(15)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
 1996)
;
_computing_data_reduction
'TEXSAN for Windows (Molecular Structure Corporation, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'PATTY in DIRDIF92 (Beurskens et al., 1992)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full .998
_diffrn_measured_fraction_theta_max .998
_diffrn_measurement_device       'Rigaku AFC-7R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71069
_diffrn_reflns_av_R_equivalents  .049
_diffrn_reflns_av_sigmaI/netI    .102
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4647
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.6
_diffrn_standards_decay_%        1.8
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .32
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          .36
_exptl_crystal_size_mid          .23
_exptl_crystal_size_min          .13
_refine_diff_density_max         .30
_refine_diff_density_min         -.38
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   .98
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .98
_refine_ls_R_factor_all          .130
_refine_ls_R_factor_gt           .043
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.061P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .130
_reflns_number_gt                1545
_reflns_number_total             2965
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ya6022.cif
_cod_data_source_block           I
_cod_original_cell_volume        2581.0(10)
_cod_original_sg_symbol_Hall     '-C 2yc '
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C16 H40 Cl2 N6 O12 '
_cod_database_code               2200367
_cod_database_fobs_code          2200367