Optimised synthesis of monoanionic bis(NHC)-pincer ligand precursors and their Li-complexes
Jürgens, Eva; Buys, Kai N.; Schmidt, Anna-Theresa; Furfari, Samantha K.; Cole, Marcus L.; Moser, Michael; Rominger, Frank; Kunz, Doris; New J. Chem. 40 (2016) 9160–; doi:10.1039/C6NJ01941B

data_7055767
_publ_section_title
;
 Optimised synthesis of monoanionic bis(NHC)-pincer ligand precursors and
 their Li-complexes
;
_journal_issue                   11
_journal_name_full               'New J. Chem.'
_journal_page_first              9160
_journal_paper_doi               10.1039/C6NJ01941B
_journal_volume                  40
_journal_year                    2016
_chemical_formula_sum            'C41 H45 Br2 Cl2 N5'
_chemical_formula_weight         838.54
_chemical_name_common            H(bimcaBn)2HBr
_chemical_name_systematic
'3,6-Di-tert-butyl-1,8-bis(3-benzylimidazolium)carbazole dibromide'
_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
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-04-05 deposited with the CCDC.
2016-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.7590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5894(7)
_cell_length_b                   25.3500(11)
_cell_length_c                   10.6923(5)
_cell_measurement_reflns_used    8148
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.301
_cell_measurement_theta_min      1.401
_cell_volume                     3940.8(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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            148502
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.301
_diffrn_reflns_theta_min         1.401
_diffrn_source                   microsourece
_exptl_absorpt_coefficient_mu    2.228
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.092
_refine_diff_density_max         1.067
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         9794
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+6.3179P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1047
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8148
_reflns_number_total             9794
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj01941b2.cif
_cod_data_source_block           eva121
_cod_depositor_comments
'Adding full bibliography for 7055764--7055771.cif.'
_cod_database_code               7055767
_shelx_estimated_absorpt_t_min   0.649
_shelx_estimated_absorpt_t_max   0.821
_shelxl_version_number           2013-4
_shelx_res_checksum              18233
_solvent_exptl_crystal_recrystallization_method dichloromethane