Temperature-induced reversible structural phase transition of 1,4-dimethyl-1,4-diazabicyclo[2.2.2]octane bis(perchlorate)
chen, lizhuang; Cao, Xing-Xing; Huang, Deng-Deng; Pan, Qi-Jian; RSC Adv.  (2015) –; doi:10.1039/C5RA07526B

data_7220770
_publ_section_title
;
 Temperature-induced reversible structural phase transition of
 1,4-dimethyl-1,4-diazabicyclo[2.2.2]octane bis(perchlorate)
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA07526B
_journal_year                    2015
_chemical_formula_moiety         'C8 H18 N2, 2(Cl O4)'
_chemical_formula_sum            'C8 H18 Cl2 N2 O8'
_chemical_formula_weight         341.14
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-01-20 deposited with the CCDC.
2015-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.895(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   13.331(3)
_cell_length_b                   15.185(4)
_cell_length_c                   20.477(5)
_cell_measurement_reflns_used    5901
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.1
_cell_measurement_theta_min      1.7
_cell_volume                     4144.7(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0394
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31339
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         0.99
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  0.9050
_exptl_absorpt_correction_T_min  0.8623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.428
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         7783
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0737
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+31.3036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1834
_refine_ls_wR_factor_ref         0.2039
_reflns_number_gt                6803
_reflns_number_total             7783
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra07526b2.cif
_cod_data_source_block           111
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_original_cell_volume        4144.8(17)
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_database_code               7220770