1,4,8,11-Tetrakis(carboxymethyl)-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazoniacyclotetradecane tetrachloride octahydrate
Wang, Shi-Fan; Li, Huan-Qiu; Ruan, Ban-Feng; Zhu, Hai-Liang; Ng, Seik Weng; Acta Crystallographica Section E 61 (2005) o2413–o2414; doi:10.1107/S1600536805020817

data_2206381
_publ_section_title
;1,4,8,11-Tetrakis(carboxymethyl)-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazoniacyclotetradecane
 tetrachloride octahydrate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2413
_journal_page_last               o2414
_journal_paper_doi               10.1107/S1600536805020817
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C24 H48 N4 O8 4+, 4Cl -, 8H2 O'
_chemical_formula_moiety         'C24 H48 N4 O8 4+, 4Cl -, 8H2 O'
_chemical_formula_sum            'C24 H64 Cl4 N4 O16'
_chemical_formula_weight         806.59
_chemical_name_systematic
;
1,4,8,11-Tetrakis(carboxymethyl)-5,5,7,12,12,14-hexamethyl-1,4,8,11-
tetraazoniacyclotetradecane tetrachloride octahydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.1610(10)
_cell_angle_beta                 94.4820(10)
_cell_angle_gamma                103.1680(10)
_cell_formula_units_Z            1
_cell_length_a                   8.6283(3)
_cell_length_b                   10.6995(4)
_cell_length_c                   11.0065(4)
_cell_measurement_reflns_used    8332
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.4
_cell_volume                     966.42(6)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device_type  'Bruker APEX 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  0.017
_diffrn_reflns_av_sigmaI/netI    0.020
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11066
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         1.9
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.34
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4351
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.045
_refine_ls_R_factor_gt           0.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0657P)^2^+0.404P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.120
_refine_ls_wR_factor_ref         0.121
_reflns_number_gt                4153
_reflns_number_total             4351
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci6606.cif
_cod_data_source_block           I
_cod_database_code               2206381
_cod_database_fobs_code          2206381