Pressure-Induced Solvate Crystallization of 1,4-Diazabicyclo[2.2.2]octane Perchlorate with Methanol
Anioła, Michalina; Olejniczak, Anna; Katrusiak, Andrzej; Crystal Growth & Design 14 (2014) 2187–; doi:10.1021/cg4016959

data_4510265
_publ_section_title
;
 Pressure-Induced Solvate Crystallization of 1,4-Diazabicyclo[2.2.2]octane
 Perchlorate with Methanol
;
_journal_issue                   5
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2187
_journal_paper_doi               10.1021/cg4016959
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C6 H13 N2, Cl O4, C H4 O, C H4 O'
_chemical_formula_sum            'C8 H21 Cl N2 O6'
_chemical_formula_weight         276.72
_chemical_name_common
;
dabcoHClO4 methanol cocrystal
;
_chemical_name_systematic
; 
1,4-diazabicyclo[2.2.2]octane perchlorate methanol cocrystal
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.463(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7762(9)
_cell_length_b                   9.782(3)
_cell_length_c                   15.1099(19)
_cell_measurement_pressure       2300000
_cell_measurement_reflns_used    4569
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.74
_cell_measurement_theta_min      4.31
_cell_volume                     1149.3(4)
_computing_cell_refinement       'CrysAlis (Oxford Diffraction, 2010)'
_computing_data_collection       'CrysAlis (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction, 2010)'
_computing_molecular_graphics
;X-Seed (Barbour, 2001) 
and POV-Ray (Persistence of Vision, 2004)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.229
_diffrn_measured_fraction_theta_max 0.229
_diffrn_measurement_device_type  'Kuma KM4CCD \k geometry'
_diffrn_measurement_method
;HP omega scans - for more details see:
A. Budzianowski, A. Katrusiak in High-Pressure Crystallography
(Eds.: A. Katrusiak, P. F. McMillan),
Dordrecht: Kluwer Acad. Publ., 2004 pp.157-168
;
_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  0.1378
_diffrn_reflns_av_sigmaI/netI    0.0726
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_k_min       -2
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4569
_diffrn_reflns_theta_full        27.74
_diffrn_reflns_theta_max         27.74
_diffrn_reflns_theta_min         4.31
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Katrusiak, A. (2003). REDSHABS - Program for correcting
reflections intensities for DAC absorption, gasket shadowing
and sample crystal absorption. Adam Mickiewicz University, Pozna\'n.
Katrusiak, A. (2004). Z. Kristallogr. 219, 461-467
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.009(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         621
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.1190
_refine_ls_R_factor_gt           0.0817
_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^)+(0.1393P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2024
_refine_ls_wR_factor_ref         0.2279
_reflns_number_gt                459
_reflns_number_total             621
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg4016959_si_002.cif
_cod_data_source_block           dabcoHClO4.2CH3OH@2.30
_cod_depositor_comments
'Adding full bibliography for 4510264--4510266.cif.'
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4510265