Crystal structure of 2-dimethylamino-1-ethoxycarbonyl-3-methyl-3,4,5,6-tetrahydropyrimidin-1-ium tetraphenylborate
Tiritiris, Ioannis; Kantlehner, Willi; Acta Crystallographica Section E 71 (2015) o894–o895; doi:10.1107/S2056989015020034

data_2241269
_publ_section_title
;
 Crystal structure of
 2-dimethylamino-1-ethoxycarbonyl-3-methyl-3,4,5,6-tetrahydropyrimidin-1-ium
 tetraphenylborate
;
_journal_coeditor_code           ZL2648
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o894
_journal_page_last               o895
_journal_paper_doi               10.1107/S2056989015020034
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C10 H20 N3 O2 +, C24 H20 B -'
_chemical_formula_moiety         'C10 H20 N3 O2 +, C24 H20 B -'
_chemical_formula_sum            'C34 H40 B N3 O2'
_chemical_formula_weight         533.50
_chemical_name_systematic
'2-Dimethylamino-1-ethoxycarbonyl-3-methyl-3,4,5,6-tetrahydropyrimidin-1-ium tetraphenylborate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90.00
_cell_angle_beta                 119.280(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.5710(5)
_cell_length_b                   19.2164(7)
_cell_length_c                   18.6107(5)
_cell_measurement_reflns_used    26101
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.10
_cell_measurement_theta_min      1.26
_cell_volume                     5793.0(3)
_computing_cell_refinement
;
SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT (Hooft, 2004)
;
_computing_data_reduction
;
SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2005)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD'
_diffrn_measurement_method       '\f scans, and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_sigmaI/netI    0.0749
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26283
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         1.26
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.254
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         14001
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+5.1462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1188
_reflns_number_gt                9686
_reflns_number_total             14001
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zl2648sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2241269
_cod_database_fobs_code          2241269
_shelx_hkl_checksum              16869
_shelx_res_checksum              8252