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_4088390
_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         'C54 H100 K2 N2 O2 P4'
_chemical_formula_sum            'C54 H100 K2 N2 O2 P4'
_chemical_formula_weight         1011.43
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.232(3)
_cell_length_b                   24.476(5)
_cell_length_c                   20.231(5)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.78
_cell_measurement_theta_min      2.47
_cell_volume                     7047(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.992
_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  0.0745
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            53609
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.115
_diffrn_reflns_theta_min         1.655
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.257
_exptl_absorpt_correction_T_max  0.7336
_exptl_absorpt_correction_T_min  0.6035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    0.953
_exptl_crystal_description       prism
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.480
_exptl_crystal_size_min          0.450
_platon_squeeze_details
;
 The residual electron density was assigned to half a molecule of the
 pentane solvent [186/8 = 23 e per asymmetric unit; half a molecule
 of C5H12 would give 21e].
;
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         8548
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1369
_refine_ls_R_factor_gt           0.1045
_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^)+(0.1283P)^2^+14.5738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2888
_refine_ls_wR_factor_ref         0.3055
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5703
_reflns_number_total             8548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00048_si_002.cif
_cod_data_source_block           pbts150602
_cod_database_code               4088390
_shelx_estimated_absorpt_t_min   0.882
_shelx_estimated_absorpt_t_max   0.893
_shelxl_version_number           2013-4
_shelx_res_checksum              8680
_shelx_hkl_checksum              34914