1,4,8,11-Tetrakis(carboxymethyl)-5,5,7,12,12,14-hexamethyl-4,11-diaza-1,8-diazoniacyclotetradecane dichloride dihydrate
Wang, Shi-Fan; Liu, Hai-Qing; Yao, Xue-Mei; Yang, Kai; Li, Xiao-Hong; Acta Crystallographica Section E 64 (2008) o885–; doi:10.1107/S1600536808010532

data_2218281
_publ_section_title
;1,4,8,11-Tetrakis(carboxymethyl)-5,5,7,12,12,14-hexamethyl-4,11-diaza-1,8-diazoniacyclotetradecane
 dichloride dihydrate
;
_journal_coeditor_code           WN2251
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o885
_journal_paper_doi               10.1107/S1600536808010532
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C24 H46 N4 O8 2+, 2Cl -, 2H2 O'
_chemical_formula_moiety         'C24 H46 N4 O8 2+, 2(Cl -), 2(H2 O)'
_chemical_formula_sum            'C24 H50 Cl2 N4 O10'
_chemical_formula_weight         625.58
_chemical_name_systematic
;
1,4,8,11-Tetrakis(carboxymethyl)-5,5,7,12,12,14-hexamethyl-
4,11-diaza-1,8-diazoniacyclotetradecane dichloride
dihydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 104.220(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.977(5)
_cell_length_b                   13.475(7)
_cell_length_c                   11.572(6)
_cell_measurement_reflns_used    17651
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.9
_cell_measurement_theta_min      2.35
_cell_volume                     1508.1(13)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008) and local programs'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1434
_diffrn_reflns_av_sigmaI/netI    0.0886
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15242
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    0.274
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.374
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0715P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1407
_reflns_number_gt                2036
_reflns_number_total             2946
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wn2251.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2218281
_cod_database_fobs_code          2218281