1-Carboxymethyl-1'-carboxylatomethyl-3,3'-[<i>p</i>-phenylenebis(oxymethylene)]dipyridinium bromide dihydrate
Lian, Hong-Lei; Pan, Wei-Cheng; Acta Crystallographica Section E 66 (2010) o2656–; doi:10.1107/S1600536810037748

data_2227881
_publ_section_title
;
 1-Carboxymethyl-1'-carboxylatomethyl-3,3'-[<i>p</i>-phenylenebis(oxymethylene)]dipyridinium
 bromide dihydrate
;
_journal_coeditor_code           PB2040
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2656
_journal_paper_doi               10.1107/S1600536810037748
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C22 H21 N2 O6 +, Br -, 2H2 O'
_chemical_formula_moiety         'C22 H21 N2 O6 +, Br -, 2(H2 O)'
_chemical_formula_sum            'C22 H25 Br N2 O8'
_chemical_formula_weight         525.35
_chemical_name_systematic
;
1-Carboxymethyl-1'-carboxylatomethyl-3,3'-[<i>p</i>-
phenylenebis(oxymethylene)]dipyridinium bromide dihydrate
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.845(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.605(4)
_cell_length_b                   7.9612(12)
_cell_length_c                   15.233(4)
_cell_measurement_reflns_used    186
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.01
_cell_volume                     2285.5(9)
_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  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2537
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    1.849
_exptl_absorpt_correction_T_max  0.5557
_exptl_absorpt_correction_T_min  0.4643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.331
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2009
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+1.7877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                1520
_reflns_number_total             2009
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            pb2040.cif
_cod_data_source_block           I
_cod_original_cell_volume        2285.6(8)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               2227881
_cod_database_fobs_code          2227881