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_7055768
_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_moiety         'C38 H39 N5, 2(B F4)'
_chemical_formula_sum            'C38 H39 B2 F8 N5'
_chemical_formula_weight         739.36
_chemical_name_common            HbimcaPh2HBF4
_chemical_name_systematic
'3,6-Di-tert-butyl-1,8-bis(3-phenylimidazolium)carbazole bis(tetrafluoroborate)'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-04-05 deposited with the CCDC.
2016-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.331(2)
_cell_length_b                   10.6223(14)
_cell_length_c                   25.494(3)
_cell_measurement_reflns_used    3797
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.011
_cell_measurement_theta_min      2.078
_cell_volume                     4151.7(9)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II DUO CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1030
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            89380
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.011
_diffrn_reflns_theta_min         2.078
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS. Ver. 2014/5. (Krause, L., Herbst-Irmer, R., Sheldrick, G. M. 
& Stalke, D. (2015). J. Appl. Crystallogr. 48.)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.011
_exptl_transmission_factor_max   1.0000
_exptl_transmission_factor_min   0.8878
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         5633
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0636
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+5.3279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1379
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3797
_reflns_number_total             5633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj01941b2.cif
_cod_data_source_block           phbimca_kwt_sq
_cod_depositor_comments
'Adding full bibliography for 7055764--7055771.cif.'
_cod_database_code               7055768
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.998
_shelx_estimated_absorpt_t_max   0.999
_shelxl_version_number           2013-4
_shelx_res_checksum              89079
_solvent_exptl_crystal_recrystallization_method Isoproanol