Self-assembly between 1,4-diazabicyclo[2.2.2]octane and bis(hexafluoroalcohols): solid/liquid phase switching for catalyst recycling
Legros, Julien; Bonnet-Delpon, Danièle; Crousse, Benoit; Slawin, Alexandra M. Z.; Catalysis Science & Technology 2 (2012) 934–; doi:10.1039/c2cy00528j

data_1556312
_publ_section_title
;
 Self-assembly between 1,4-diazabicyclo[2.2.2]octane and
 bis(hexafluoroalcohols): solid/liquid phase switching for catalyst
 recycling
;
_journal_issue                   5
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              934
_journal_paper_doi               10.1039/c2cy00528j
_journal_volume                  2
_journal_year                    2012
_chemical_formula_moiety         'C6 H12 N2,C12 H6 F12 O2'
_chemical_formula_sum            'C18 H18 F12 N2 O2'
_chemical_formula_weight         522.34
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 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                 110.81(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.06(2)
_cell_length_b                   6.782(5)
_cell_length_c                   13.057(15)
_cell_measurement_reflns_used    1264
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.5
_cell_measurement_theta_min      21.7
_cell_volume                     2074(3)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2004)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1548
_diffrn_reflns_av_sigmaI/netI    0.0797
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12652
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.84
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    1.650
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.166
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.6(3)
_refine_ls_extinction_coef       0.014(2)
_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   1.330
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3574
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.329
_refine_ls_R_factor_all          0.1404
_refine_ls_R_factor_gt           0.1324
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_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          0.3253
_refine_ls_wR_factor_ref         0.3567
_reflns_number_gt                2892
_reflns_number_total             3574
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cy00528j.txt
_cod_data_source_block           1b
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2075(3)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               1556312