2,2'-[4,10-Bis(carboxymethyl)-4,10-diaza-1,7-diazoniacyclododecane-1,7-diyl]diacetate dihydrate
Szalay, Paul S.; Zeller, Matthias; Hunter, Allen D.; Acta Crystallographica Section E 67 (2011) o644–; doi:10.1107/S1600536811004843

data_2229436
_publ_section_title
;
 2,2'-[4,10-Bis(carboxymethyl)-4,10-diaza-1,7-diazoniacyclododecane-1,7-diyl]diacetate
 dihydrate
;
_journal_coeditor_code           KP2290
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o644
_journal_paper_doi               10.1107/S1600536811004843
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C16 H28 N4 O8, 2H2 O'
_chemical_formula_moiety         'C16 H28 N4 O8, 2(H2 O)'
_chemical_formula_sum            'C16 H32 N4 O10'
_chemical_formula_weight         440.46
_chemical_name_systematic
;
2,2'-[4,10-Bis(carboxymethyl)-4,10-diaza-1,7-diazoniacyclododecane-1,7-
diyl]diacetate dihydrate
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.183(2)
_cell_length_b                   6.5826(9)
_cell_length_c                   17.983(2)
_cell_measurement_reflns_used    13988
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2841
_cell_measurement_theta_min      0.994182
_cell_volume                     2034.0(4)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and <i>PLATON</i> Spek (2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_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  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19408
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    0.119
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2520
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+0.8651P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1124
_reflns_number_gt                2236
_reflns_number_total             2520
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            kp2290.cif
_cod_data_source_block           I
_cod_original_cell_volume        2034.0(5)
_cod_database_code               2229436
_cod_database_fobs_code          2229436