1,7-Bis(1,3-dimethyluracil-6-yl)-1,4,7,10-tetraazacyclododecane acetonitrile disolvate at 100 K
Uchida, Akira; Komori, Ayako; Watanabe, Soichiro; Acta Crystallographica Section E 63 (2007) o648–o649; doi:10.1107/S1600536807000463

data_2212256
_publ_section_title
;
 1,7-Bis(1,3-dimethyluracil-6-yl)-1,4,7,10-tetraazacyclododecane
 acetonitrile disolvate at 100 K
;
_journal_coeditor_code           IS2139
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o648
_journal_page_last               o649
_journal_paper_doi               10.1107/S1600536807000463
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C20 H32 N8 O4, 2C2 H3 N'
_chemical_formula_moiety         'C20 H32 N8 O4, 2C2 H3 N'
_chemical_formula_sum            'C24 H38 N10 O4'
_chemical_formula_weight         530.64
_chemical_name_systematic
;
1,1',3,3'-tetramethyl-1,1',2,2',3,3',4,4'-octahydro-6,6-(1,4,7,10-
tetraazacyclododecane-1,7-diyl)dipyrimidine-2,2',4,4'-tetraone
acetonitrile disolvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 92.4510(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.2718(18)
_cell_length_b                   7.5477(6)
_cell_length_c                   14.3193(11)
_cell_measurement_reflns_used    3832
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      28.6
_cell_measurement_theta_min      2.8
_cell_volume                     2620.8(3)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker--Nonius, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker--Nonius, 2004)'
_computing_molecular_graphics
;
PLATON (Spek, 2003) and ORTEPIII (Burnett & Johnson, 1996)
;
_computing_publication_material  'SHELXL97 and PLATON'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100.0(10)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0151
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7243
_diffrn_reflns_theta_full        28.71
_diffrn_reflns_theta_max         28.71
_diffrn_reflns_theta_min         1.68
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.9765
_exptl_absorpt_correction_T_min  0.9627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3096
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+1.6563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.0939
_reflns_number_gt                2681
_reflns_number_total             3096
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            is2139.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2212256
_cod_database_fobs_code          2212256