Synthesis and Crystal Structure of 1,4,7-Tris(2-mercaptoethyl)-1,4,7-triazacyclononane
MIKURIYA, Masahiro; MIYOSHI, Kazufumi; KURANO, Shuhei; TAGUCHI, Jun; KOTERA, Takanori; YOSHIOKA, Daisuke; X-ray Structure Analysis Online 31 (2015) 59–; doi:10.2116/xraystruct.31.59

data_1551631
_publ_section_title
;
 Synthesis and Crystal Structure of
 1,4,7-Tris(2-mercaptoethyl)-1,4,7-triazacyclononane
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              59
_journal_paper_doi               10.2116/xraystruct.31.59
_journal_volume                  31
_journal_year                    2015
_chemical_formula_sum            'C12 H31 Cl2 N3 O S3'
_chemical_formula_weight         400.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.528(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9553(13)
_cell_length_b                   13.7164(19)
_cell_length_c                   14.724(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1962.7(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXL'
_computing_publication_material  'Bruker SHELXL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11908
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.690
_diffrn_reflns_theta_min         2.052
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.771
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       plate
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         4528
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0538
_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^)+(0.0554P)^2^+1.5245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1436
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3912
_reflns_number_total             4528
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            31_59_1.txt
_cod_data_source_block           H3L0508
_cod_database_code               1551631
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.771
_shelx_estimated_absorpt_t_max   0.950
_shelx_res_checksum              48695
_shelx_hkl_checksum              62061