N-Heterocyclic carbene-phosphino-picolines as precursors of anionic 'pincer' ligands with dearomatised pyridine backbones; transmetallation from potassium to chromium
Thomas Simler; Andreas A. Danopoulos; Pierre Braunstein; Chem.Commun. 51 (2015) 10699–; doi:10.1039/C5cc02920A

data_7117348
_publ_section_title
;
 N-Heterocyclic carbene-phosphino-picolines as precursors of anionic
 'pincer' ligands with dearomatised pyridine backbones; transmetallation
 from potassium to chromium
;
_journal_name_full               Chem.Commun.
_journal_page_first              10699
_journal_paper_doi               10.1039/C5cc02920A
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C33 H48 N3 P, C H2 Cl2, 2(Br)'
_chemical_formula_sum            'C34 H50 Br2 Cl2 N3 P'
_chemical_formula_weight         762.46
_chemical_name_systematic
;
 ?
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-04-02 deposited with the CCDC.
2015-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 123.958(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1055(4)
_cell_length_b                   25.0614(9)
_cell_length_c                   14.6620(4)
_cell_measurement_reflns_used    7390
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.76
_cell_measurement_theta_min      2.33
_cell_volume                     3689.5(2)
_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-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0413
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36844
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.005
_diffrn_reflns_theta_min         1.625
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    2.412
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       prism
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.113
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         8912
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0581P)^2^+8.2172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1487
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                6146
_reflns_number_total             8912
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc02920a3-4.cif
_cod_data_source_block           pbts150113
_cod_database_code               7117348
_shelx_estimated_absorpt_t_min   0.486
_shelx_estimated_absorpt_t_max   0.644
_shelxl_version_number           2013-4
_shelx_res_checksum              68664