Crystal structure of 9,20-dimethyl-1,8,12,19-tetraazatetracyclo[17.3.1.0^2,7^.0^13,18^]tricosane dihydrate from synchrotron X-ray data
Moon, Dohyun; Choi, Jong-Ha; Acta Crystallographica Section E 73 (2017) 387–389; doi:10.1107/S2056989017002444

data_2242152
_publ_section_title
;
 Crystal structure of
 9,20-dimethyl-1,8,12,19-tetraazatetracyclo[17.3.1.0^2,7^.0^13,18^]tricosane
 dihydrate from synchrotron X-ray data
;
_journal_coeditor_code           WM5364
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              387
_journal_page_last               389
_journal_paper_doi               10.1107/S2056989017002444
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C21 H40 N4, 2H2 O'
_chemical_formula_moiety         'C21 H40 N4, 2H2 O'
_chemical_formula_sum            'C21 H44 N4 O2'
_chemical_formula_weight         384.60
_chemical_name_systematic
'9,20-Dimethyl-1,8,12,19-tetraazatetracyclo[17.3.1.0^2,7^.0^13,18^]tricosane dihydrate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                87.20(3)
_cell_angle_beta                 77.83(3)
_cell_angle_gamma                72.31(3)
_cell_formula_units_Z            2
_cell_length_a                   8.3870(17)
_cell_length_b                   10.275(2)
_cell_length_c                   14.115(3)
_cell_measurement_reflns_used    63772
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      33.548
_cell_measurement_theta_min      0.361
_cell_volume                     1132.7(5)
_computing_cell_refinement
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
<i>PAL BL2D-SMDC</i> (Shin <i>et al.</i>,  2016)
;
_computing_data_reduction
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
<i>DIAMOND 4</i> (Putz & Brandenburg, 2014)
;
_computing_publication_material
;
<i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2014</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT2014</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.610
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11640
_diffrn_reflns_theta_full        22.210
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         1.308
_exptl_absorpt_coefficient_mu    0.057
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm SCALEPACK</i>; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_description       block
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.273
_refine_ls_extinction_coef       0.042(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015<i>b</i>)
;
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         5950
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0685P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1233
_reflns_number_gt                3853
_reflns_number_total             5950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5364sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1132.8(5)
_cod_database_code               2242152
_cod_database_fobs_code          2242152
_shelx_estimated_absorpt_t_min   0.996
_shelx_estimated_absorpt_t_max   0.997
_shelx_hkl_checksum              9085
_shelx_res_checksum              18478