Melting point suppression in new lanthanoid(III) ionic liquids by trapping of kinetic polymorphs: an in situ synchrotron powder diffraction study
Anthony S. R. Chesman; Mei Yang; Bert Mallick; Tamsyn M. Ross; Ian A. Gass; Glen B. Deacon; Stuart R. Batten; Anja-Verena Mudring; Chem.Commun. 48 (2012) 124–; doi:10.1039/c1cc14744g

data_7107112
_publ_section_title
;
 Melting point suppression in new lanthanoid(III) ionic liquids by
 trapping of kinetic polymorphs: an in situ synchrotron powder diffraction
 study
;
_journal_name_full               Chem.Commun.
_journal_page_first              124
_journal_paper_doi               10.1039/c1cc14744g
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C18 Ce N18 O6, 3(C16 H36 N)'
_chemical_formula_sum            'C66 H108 Ce N21 O6'
_chemical_formula_weight         1431.85
_chemical_name_common            (N4444)3[Ce(dcnm)6]
_chemical_name_systematic
;
Tri(tetrabutylammonium) hexakis(dicyanonitrosomethanido)cerium(III)
;
_space_group_IT_number           155
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   17.4269(5)
_cell_length_b                   17.4269(5)
_cell_length_c                   22.3789(6)
_cell_measurement_reflns_used    19769
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      29.00
_cell_measurement_theta_min      3.26
_cell_volume                     5885.9(3)
_computing_cell_refinement       'Bruker SMART (Bruker)'
_computing_data_collection       'Bruker SMART (Bruker)'
_computing_data_reduction        'Bruker SAINT (Bruker)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(1)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker X8 Apex II CCD'
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19769
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_T_max  0.8829
_exptl_absorpt_correction_T_min  0.8315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2271
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(6)
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.720
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         3269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.720
_refine_ls_R_factor_all          0.0158
_refine_ls_R_factor_gt           0.0158
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0413
_refine_ls_wR_factor_ref         0.0413
_reflns_number_gt                3263
_reflns_number_total             3269
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc14744g.txt
_cod_data_source_block           AC2P782.CIF
_cod_original_sg_symbol_H-M      R32
_cod_database_code               7107112