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_2021807
_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           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 95.302(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8624(2)
_cell_length_b                   15.0884(3)
_cell_length_c                   16.7029(4)
_cell_measurement_reflns_used    8968
_cell_measurement_temperature    299(1)
_cell_measurement_theta_max      68.00
_cell_measurement_theta_min      3.96
_cell_volume                     2223.95(9)
_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      299(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Kappa APEX-II DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'QUAZAR multilayer optics'
_diffrn_radiation_source         'I\mS microfocus'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26633
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.270
_diffrn_reflns_theta_min         3.956
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       fragment
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4047
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0879
_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^)+(0.1449P)^2^+1.5857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2618
_refine_ls_wR_factor_ref         0.2702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3551
_reflns_number_total             4047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lg3222sup7.txt
_cod_data_source_block           Jurek2RT
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2021807
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.800
_shelx_estimated_absorpt_t_max   0.934
_shelx_res_checksum              7398
_shelx_hkl_checksum              20591