Pyrrole-Based New Diphosphines: Pd and Ni Complexes Bearing the PNP Pincer Ligand
Shanish Kumar; Ganesan Mani; Sukanta Mondal; Pratim Kumar Chattaraj; Inorganic Chemistry 51 (2012) 12527–12539; doi:10.1021/ic301967r

data_4331100
_publ_contact_author_address
;Department of Chemistry
Indian Institute of Technology-Kharagpur
Kharagpur, India 721 302
;
_publ_contact_author_email       gmani@chem.iitkgp.ernet.in
_publ_contact_author_fax         91-3222-282252
_publ_contact_author_name        'Mani, Ganesan.'
_publ_contact_author_phone       91-3222-282320
_publ_section_title
;
 Pyrrole-Based New Diphosphines: Pd and Ni Complexes Bearing the PNP
 Pincer Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12527
_journal_page_last               12539
_journal_paper_doi               10.1021/ic301967r
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C47 H40 N2 P2'
_chemical_formula_weight         694.75
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_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.113(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.352(3)
_cell_length_b                   10.4594(11)
_cell_length_c                   26.729(3)
_cell_measurement_reflns_used    30151
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      20.82
_cell_measurement_theta_min      1.47
_cell_volume                     7719.7(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker CCD APEX 2'
_diffrn_measurement_method       hemisphere
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1313
_diffrn_reflns_av_sigmaI/netI    0.0734
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30151
_diffrn_reflns_theta_full        20.82
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  0.9883
_exptl_absorpt_correction_T_min  0.9379
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_description       Needle
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.004
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         4027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1284
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0728P)^2^+22.7625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1456
_refine_ls_wR_factor_ref         0.1809
_reflns_number_gt                2286
_reflns_number_total             4027
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic301967r_si_002_1.cif
_cod_data_source_block           compound5
_cod_original_cell_volume        7719.9(13)
_cod_database_code               4331100