Reversible Phase Transition of 1,4-Diazoniabicyclo[2.2.2]octane-1-acetate-4-acetic Acid Chloride Trihydrate
Zhang, Yi; Liao, Wei-Qiang; Ye, Heng-Yun; Fu, Da-Wei; Xiong, Ren-Gen; Crystal Growth & Design 13 (2013) 4025–; doi:10.1021/cg400829d

data_4508205
_publ_section_title
;
 Reversible Phase Transition of
 1,4-Diazoniabicyclo[2.2.2]octane-1-acetate-4-acetic Acid Chloride
 Trihydrate
;
_journal_issue                   9
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4025
_journal_paper_doi               10.1021/cg400829d
_journal_volume                  13
_journal_year                    2013
_chemical_formula_moiety         'C10 H16 D N2 O4, Cl,  3 (D2 O)'
_chemical_formula_sum            'C10 H16 Cl D7 N2 O7'
_chemical_formula_weight         325.80
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 103.967(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.907(7)
_cell_length_b                   11.735(6)
_cell_length_c                   17.847(9)
_cell_measurement_reflns_used    12903
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.08
_cell_volume                     2826(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku SCXmini diffractometer'
_diffrn_measurement_method       '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  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30277
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.704
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.379
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         6465
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.380
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0893
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3276
_refine_ls_wR_factor_ref         0.3399
_reflns_number_gt                5696
_reflns_number_total             6465
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg400829d_si_005.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2827(2)
_cod_original_sg_symbol_Hall     '-p 2yn'
_cod_original_sg_symbol_H-M      'p 21/n'
_cod_database_code               4508205