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_7055766
_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            'C33 H42 Br2 N6'
_chemical_formula_weight         682.54
_chemical_name_common            H(bimcaC5)2HBr
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_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                 111.234(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
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_cell_length_b                   14.5713(12)
_cell_length_c                   25.883(3)
_cell_measurement_reflns_used    6326
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.325
_cell_measurement_theta_min      1.767
_cell_volume                     7105.9(12)
_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 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0530
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
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_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            51295
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.325
_diffrn_reflns_theta_min         1.767
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    2.311
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.
_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            Colorless
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       block
_exptl_crystal_F_000             2816
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.117
_exptl_transmission_factor_max   0.91343
_exptl_transmission_factor_min   0.84395
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         8852
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0618P)^2^+7.0005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1224
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6326
_reflns_number_total             8852
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj01941b2.cif
_cod_data_source_block           eva124_sq_d_sq_s
_cod_depositor_comments
'Adding full bibliography for 7055764--7055771.cif.'
_cod_database_code               7055766
_shelx_estimated_absorpt_t_min   0.569
_shelx_estimated_absorpt_t_max   0.774
_shelxl_version_number           2013-3
_shelx_res_checksum              71371
_shelx_fab_checksum              90470
_solvent_exptl_crystal_recrystallization_method acetonitrile