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_7117350
_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         'C29 H41 Cl Cr N3 P'
_chemical_formula_sum            'C29 H41 Cl Cr N3 P'
_chemical_formula_weight         550.07
_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   geom
_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                 116.249(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.370(2)
_cell_length_b                   23.052(6)
_cell_length_c                   17.180(4)
_cell_measurement_reflns_used    3897
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.69
_cell_measurement_theta_min      2.59
_cell_volume                     2973.0(13)
_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 0.991
_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  0.0971
_diffrn_reflns_av_unetI/netI     0.0968
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            29169
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.113
_diffrn_reflns_theta_min         1.590
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         7188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1320
_refine_ls_R_factor_gt           0.0636
_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^)+(0.0636P)^2^+0.5470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1452
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                4181
_reflns_number_total             7188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc02920a3-4.cif
_cod_data_source_block           pbad150303
_cod_original_cell_volume        2972.9(13)
_cod_database_code               7117350
_shelx_estimated_absorpt_t_min   0.831
_shelx_estimated_absorpt_t_max   0.937
_shelxl_version_number           2013-4
_shelx_res_checksum              95839