Potassium and Lithium Complexes with Monodeprotonated, Dearomatized PNP and PNCNHC Pincer-Type Ligands
Simler, Thomas; Karmazin, Lydia; Bailly, Corinne; Braunstein, Pierre; Danopoulos, Andreas A.; Organometallics 35 (2016) 903–; doi:10.1021/acs.organomet.6b00048

data_4088386
_publ_section_title
;
 Potassium and Lithium Complexes with Monodeprotonated, Dearomatized PNP
 and PNCNHC Pincer-Type Ligands
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              903
_journal_paper_doi               10.1021/acs.organomet.6b00048
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C37 H55 Li N3 O P'
_chemical_formula_sum            'C37 H55 Li N3 O P'
_chemical_formula_weight         595.75
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 91.553(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6463(16)
_cell_length_b                   14.732(2)
_cell_length_c                   25.439(4)
_cell_measurement_reflns_used    1906
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.68
_cell_measurement_theta_min      2.63
_cell_volume                     3613.8(10)
_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 0.999
_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  0.1132
_diffrn_reflns_av_unetI/netI     0.1347
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            26655
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.008
_diffrn_reflns_theta_min         1.597
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_description       plate
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         8726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.1968
_refine_ls_R_factor_gt           0.0696
_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^)+(0.0581P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3683
_reflns_number_total             8726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00048_si_002.cif
_cod_data_source_block           pbts150311
_cod_original_cell_volume        3613.9(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4088386
_shelx_estimated_absorpt_t_min   0.969
_shelx_estimated_absorpt_t_max   0.995
_shelxl_version_number           2013-4
_shelx_res_checksum              75111
_shelx_hkl_checksum              92206