High pressure used for producing a new solvate of 1,4-diazabicyclo[2.2.2]octane hydroiodide
Olejniczak, A.; Podsiadło, M.; Katrusiak, A.; New J. Chem. 40 (2016) 2014–; doi:10.1039/C5NJ01654A

data_7055202
_publ_section_title
;
 High pressure used for producing a new solvate of
 1,4-diazabicyclo[2.2.2]octane hydroiodide
;
_journal_issue                   3
_journal_name_full               'New J. Chem.'
_journal_page_first              2014
_journal_paper_doi               10.1039/C5NJ01654A
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'I, H2 O, C H4 O, C6 H13 N2'
_chemical_formula_sum            'C7 H19 I N2 O2'
_chemical_formula_weight         290.14
_chemical_name_systematic
'1,4-diazabicyclo[2.2.2]octane hydroiodide water methanol cocrystal'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-11-16 deposited with the CCDC.
2015-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.94(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.966(3)
_cell_length_b                   7.4850(12)
_cell_length_c                   23.09(2)
_cell_measurement_temperature    296(2)
_cell_volume                     1860.8(17)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.179
_diffrn_measured_fraction_theta_max 0.169
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.179
_diffrn_reflns_Laue_measured_fraction_max 0.169
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2065
_diffrn_reflns_point_group_measured_fraction_full 0.179
_diffrn_reflns_point_group_measured_fraction_max 0.169
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.404
_diffrn_reflns_theta_min         3.315
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.408
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.57
_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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         323
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0597P)^2^+30.5695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                143
_reflns_number_total             323
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj01654a2.cif
_cod_data_source_block           dabcoHI_H2O_CH3OH
_cod_depositor_comments          'Adding full bibliography for 7055202.cif.'
_cod_original_cell_volume        1860.7(18)
_cod_database_code               7055202
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H) groups, All N(H) groups, All O(H) groups,
  All O(H,H) groups
2. Restrained distances
 O9-H9A
 0.96 with sigma of 0.05
 O9-H9B
 0.96 with sigma of 0.05
 H9A-H9B
 1.66 with sigma of 0.05
 O8-C7
 1.43 with sigma of 0.05
 H9B-I1
 2.38 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(I1) \\sim Ueq, Uanis(I2) \\sim Ueq: with sigma of 0.015 and sigma for
terminal atoms of 0.02
4. Others
 Fixed X: H9A(0.62952)
 Fixed Y: H9A(0.642)
 Fixed Z: H9A(0.63993)
5.a Free rotating group:
 N1(H1,N2,C1,H1A,H1B,C2,H2A,H2B,C3,H3A,H3B,C4,H4A,H4B,C5,H5A,H5B,C6,H6A,H6B)
5.b Tetrahedral OH refined with riding coordinates:
 O8(H8)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method 'Diamond-anvil cell'
_olex2_submission_original_sample_id dabcoHI*H2O*CH3OH
_olex2_submission_special_instructions 'No special instructions were received'