Heterogeneous microwave-assisted Ullmann type methodology for synthesis of rigid-core ionic liquid crystals
Fouchet, Julien; Heinrich, Benoît; L’Her, Matthieu; Voirin, Emilie; Karmazin, Lydia; Bailly, Corinne; Welter, Richard; Mirjafari, Arsalan; Douce, Laurent; New Journal of Chemistry 42 (2018) 10421–; doi:10.1039/C8NJ01609G

data_7057455
_publ_section_title
;
 Heterogeneous microwave-assisted Ullmann type methodology for synthesis
 of rigid-core ionic liquid crystals
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10421
_journal_paper_doi               10.1039/C8NJ01609G
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C22 H35 N2, Br'
_chemical_formula_sum            'C22 H35 Br N2'
_chemical_formula_weight         407.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-03-16 deposited with the CCDC.
2018-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.485(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1863(15)
_cell_length_b                   14.2196(12)
_cell_length_c                   8.1410(6)
_cell_measurement_reflns_used    4082
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.58
_cell_volume                     2196.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            15505
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.003
_diffrn_reflns_theta_min         2.146
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.878
_exptl_absorpt_correction_T_max  0.9119
_exptl_absorpt_correction_T_min  0.4853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       plate
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         5300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+0.8455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1062
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3661
_reflns_number_total             5300
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj01609g2.cif
_cod_data_source_block           jlgld110222
_cod_depositor_comments
'Adding full bibliography for 7057453--7057456.cif.'
_cod_database_code               7057455
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.485
_shelx_estimated_absorpt_t_max   0.912
_shelx_res_checksum              75343