1,12-Bis(2-carboxyphenyl)-5,8-dioxa-2,11-diazadodecane-2,11-diium dichloride methanol solvate
Johnson, Samuel; Musie, Ghezai T.; Tiekink, Edward R. T.; Acta Crystallographica Section E 66 (2010) o64–o65; doi:10.1107/S1600536809051824

data_2224668
_publ_section_title
;
 1,12-Bis(2-carboxyphenyl)-5,8-dioxa-2,11-diazadodecane-2,11-diium
 dichloride methanol solvate
;
_journal_coeditor_code           HG2615
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o64
_journal_page_last               o65
_journal_paper_doi               10.1107/S1600536809051824
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C22 H30 N2 O6 2+ , 2Cl - , C H4 O'
_chemical_formula_moiety         'C22 H30 N2 O6 2+ , 2Cl - , C H4 O'
_chemical_formula_sum            'C23 H34 Cl2 N2 O7'
_chemical_formula_weight         521.42
_chemical_name_systematic
;
1,12-Bis(2-carboxyphenyl)-5,8-dioxa-2,11-diazadodecane-2,11-diium dichloride
methanol solvate
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 102.760(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.567(3)
_cell_length_b                   11.352(2)
_cell_length_c                   20.052(5)
_cell_measurement_reflns_used    10052
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.3
_cell_volume                     2568.0(10)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC 2005)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'publCIF (Westrip, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku AFC12\k/SATURN724'
_diffrn_measurement_method       \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  0.050
_diffrn_reflns_av_sigmaI/netI    0.020
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            66801
_diffrn_reflns_theta_full        27.6
_diffrn_reflns_theta_max         27.6
_diffrn_reflns_theta_min         2.4
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.51
_refine_diff_density_min         -0.34
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5874
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.038
_refine_ls_R_factor_gt           0.036
_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^)+(0.0485P)^2^+1.3403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.092
_refine_ls_wR_factor_ref         0.094
_reflns_number_gt                5598
_reflns_number_total             5874
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2615.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2224668
_cod_database_fobs_code          2224668