Synthesis and Characterization of an Unsymmetrical 1,2-Diphosphinoethanide Complex
Förster, Daniela; Nieger, Martin; Gudat, Dietrich; Organometallics 30 (2011) 2628–; doi:10.1021/om200069t

data_4064373
_publ_section_title
;
 Synthesis and Characterization of an Unsymmetrical
 1,2-Diphosphinoethanide Complex
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2628
_journal_paper_doi               10.1021/om200069t
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C37 H39 Cl2 Li N4 P2 Pd, 2(C2 H3 N)'
_chemical_formula_sum            'C41 H45 Cl2 Li N6 P2 Pd'
_chemical_formula_weight         868.01
_chemical_name_systematic
; 
 Lithium[2-(1,3-bis-(2',6'-dimethylphenyl)[1,3,2]diazaphospholenyl-3-
 diphenylphosphino-1-cyanoethanide]dichloropalladium(II) 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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-97
_cell_angle_alpha                107.57(1)
_cell_angle_beta                 102.66(1)
_cell_angle_gamma                109.74(1)
_cell_formula_units_Z            2
_cell_length_a                   10.471(1)
_cell_length_b                   14.436(1)
_cell_length_c                   15.933(2)
_cell_measurement_reflns_used    273
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1
_cell_volume                     2018.0(5)
_computing_cell_refinement       'EVALCCD (Duisenberg et al., 2003)'
_computing_data_collection       'Collect (Nonius, 1998)'
_computing_data_reduction        'EVALCCD (Duisenberg et al., 2003)'
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       'rotation in phi and omega, 2 deg.'
_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  0.0773
_diffrn_reflns_av_sigmaI/netI    0.1077
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22821
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  0.9562
_exptl_absorpt_correction_T_min  0.5229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.616
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         9125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1169
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0970P)^2^+2.5600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1637
_refine_ls_wR_factor_ref         0.1911
_reflns_number_gt                6071
_reflns_number_total             9125
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200069t_si_001.cif
_cod_data_source_block           dg059_hy_compound_11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2018.0(3)
_cod_database_code               4064373