Crystal structures of two polymorphic forms of DOTAM-mono-acid dihydrate
Jurek, Paul; Kiefer, Garry E.; Fronczek, Frank R.; Acta Crystallographica Section C 74 (2018) 542–547; doi:10.1107/S2053229618004631

data_2021108
_publ_section_title
;
 Crystal structures of two polymorphic forms of DOTAM-mono-acid dihydrate
;
_journal_coeditor_code           LG3222
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              542
_journal_page_last               547
_journal_paper_doi               10.1107/S2053229618004631
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C16 H31 N7 O5, 2H2 O'
_chemical_formula_moiety         'C16 H31 N7 O5, 2(H2 O)'
_chemical_formula_sum            'C16 H35 N7 O7'
_chemical_formula_weight         437.51
_chemical_name_systematic
'4,7,10-Tris(carbamoylmethyl)-1-(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-ium dihydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 95.903(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8070(6)
_cell_length_b                   14.9505(8)
_cell_length_c                   16.6376(10)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      36.55
_cell_measurement_theta_min      3.67
_cell_volume                     2179.0(2)
_computing_cell_refinement
;
SAINT (Bruker, 2004)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2004)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
SHELXS97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      90.0(5)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Kappa APEXII DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'TRIUMPH curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            54344
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         36.551
_diffrn_reflns_theta_min         1.836
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  0.9282
_exptl_absorpt_correction_T_min  0.8915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2009)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       prism
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.222
_refine_ls_abs_structure_details
;
Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.5(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         19751
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+0.1292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0972
_reflns_number_gt                18244
_reflns_number_total             19751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lg3222sup1.cif
_cod_data_source_block           Jurek2_90K
_cod_database_code               2021108
_cod_database_fobs_code          2021108
_shelx_estimated_absorpt_t_min   0.955
_shelx_estimated_absorpt_t_max   0.969
_shelx_hkl_checksum              8710
_shelx_res_checksum              36048