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_7117349
_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         'C74 H110 K2 N6 O2 P2, 2(C37 H55 K N3 O P)'
_chemical_formula_sum            'C148 H220 K4 N12 O4 P4'
_chemical_formula_weight         2511.63
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                72.803(2)
_cell_angle_beta                 78.663(2)
_cell_angle_gamma                70.389(2)
_cell_formula_units_Z            1
_cell_length_a                   12.9906(12)
_cell_length_b                   14.5542(13)
_cell_length_c                   21.8297(19)
_cell_measurement_reflns_used    5875
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.80
_cell_measurement_theta_min      2.30
_cell_volume                     3692.3(6)
_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 0.998
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  triumph
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1848
_diffrn_reflns_av_unetI/netI     0.2149
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            65782
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.160
_diffrn_reflns_theta_min         1.533
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         17796
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.2459
_refine_ls_R_factor_gt           0.0896
_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^)+(0.1094P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1884
_refine_ls_wR_factor_ref         0.2458
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                6627
_reflns_number_total             17796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc02920a3-4.cif
_cod_data_source_block           pbts150130_02
_cod_database_code               7117349
_shelx_estimated_absorpt_t_min   0.958
_shelx_estimated_absorpt_t_max   0.983
_shelxl_version_number           2013-4
_shelx_res_checksum              36509