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_2021806
_publ_section_title
;
 Crystal structures of two polymorphic forms of DOTAM-mono-acid dihydrate
;
_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_moiety         'C16 H31 N7 O5, 2(H2 O)'
_chemical_formula_sum            'C16 H35 N7 O7'
_chemical_formula_weight         437.51
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 95.666(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8215(6)
_cell_length_b                   15.0094(10)
_cell_length_c                   16.6719(12)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    180.0(5)
_cell_measurement_theta_max      33.74
_cell_measurement_theta_min      2.32
_cell_volume                     2196.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.0(5)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa APEX-II 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  0.0281
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            76674
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         35.027
_diffrn_reflns_theta_min         1.830
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.323
_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         0.520
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.1(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         16916
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0906P)^2^+0.2404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1413
_reflns_Friedel_coverage         0.940
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                14399
_reflns_number_total             16916
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lg3222sup6.txt
_cod_data_source_block           Jurek2_180K
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2021806
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.956
_shelx_estimated_absorpt_t_max   0.970
_shelx_res_checksum              63634
_shelx_hkl_checksum              62926