A hydrogen-bridged adduct 3,4,6,7,8,9-hexahydro-2<i>H</i>-pyrimido[1,2-<i>a</i>]pyrimidin-1-ium [1,3-bis(<i>tert</i>-butyldimethylsilyloxy)-1,3-bis(pyridin-2-yl)propan-2-ylidene]nitronate acetonitrile monosolvate
Schulz, Martin; Görls, Helmar; Westerhausen, Matthias; Acta Crystallographica Section E 67 (2011) o2396–; doi:10.1107/S1600536811033927

data_2231642
_publ_section_title
;
 A hydrogen-bridged adduct
 3,4,6,7,8,9-hexahydro-2<i>H</i>-pyrimido[1,2-<i>a</i>]pyrimidin-1-ium
 [1,3-bis(<i>tert</i>-butyldimethylsilyloxy)-1,3-bis(pyridin-2-yl)propan-2-ylidene]nitronate
 acetonitrile monosolvate
;
_journal_coeditor_code           NK2105
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2396
_journal_paper_doi               10.1107/S1600536811033927
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C7 H14 N3 +, C25 H40 N3 O4 Si2 -, C H3 CN '
_chemical_formula_moiety         'C25 H40 N3 O4 Si2, C7 H14 N3, C2 H3 N'
_chemical_formula_sum            'C34 H57 N7 O4 Si2'
_chemical_formula_weight         684.05
_chemical_name_systematic
;
3,4,6,7,8,9-hexahydro-2<i>H</i>-
pyrimido[1,2-<i>a</i>]pyrimidin-1-ium [1,3-bis(<i>tert</i>-
butyldimethylsilyloxy)-1,3-bis(pyridin-2-yl)propan-2-ylidene]nitronate
acetonitrile monosolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.062(4)
_cell_angle_beta                 98.098(4)
_cell_angle_gamma                95.197(5)
_cell_formula_units_Z            2
_cell_length_a                   9.4335(8)
_cell_length_b                   11.1149(9)
_cell_length_c                   19.4529(14)
_cell_measurement_reflns_used    12006
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      1.90
_cell_volume                     1951.2(3)
_computing_cell_refinement       'DENZO  (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO  (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f and \w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_sigmaI/netI    0.1762
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12006
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.274
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         8497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.1814
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1409
_reflns_number_gt                3820
_reflns_number_total             8497
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            nk2105.cif
_cod_data_source_block           I
_cod_database_code               2231642
_cod_database_fobs_code          2231642