(η^2^-Tetracyanoethene)bis(triphenylphosphine-κ<i>P</i>)palladium‒dichloromethane (1/0.7)
Zoe Shackleton; Colin A. Kilner; Gavin D. Reid; Malcolm A. Halcrow; Acta Crystallographica Section C 59 (2003) m136–m138; doi:10.1107/S010827010300458X

data_2013248
_publ_section_title
;(\h^2^-Tetracyanoethene)bis(triphenylphosphine-\k<i>P</i>)palladium--dichloromethane
 (1/0.7)
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m136
_journal_page_last               m138
_journal_paper_doi               10.1107/S010827010300458X
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Pd (C6 N4) (C18 H15 P)2], 0.7C H2 Cl2'
_chemical_formula_moiety         'C42 H30 N4 P2 Pd, 0.7C H2 Cl2'
_chemical_formula_sum            'C42.7 H31.4 Cl1.4 N4 P2 Pd'
_chemical_formula_weight         818.49
_chemical_name_systematic
;
Bis(triphenylphosphine)(tetracyanoethene)palladium--dichloromethane (1/0.7)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.1463(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.33630(10)
_cell_length_b                   37.2805(4)
_cell_length_c                   10.81420(10)
_cell_measurement_reflns_used    29108
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.67
_cell_volume                     3886.56(7)
_computing_cell_refinement       'DENZO--SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        DENZO--SMN
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       'area-detector scans'
_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  0.053
_diffrn_reflns_av_sigmaI/netI    0.046
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            29108
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995)'
_exptl_crystal_colour            Yellow-orange
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1662
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.75
_refine_diff_density_min         -0.80
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         8877
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0582P)^2^+3.3475P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.104
_refine_ls_wR_factor_ref         0.110
_reflns_number_gt                7450
_reflns_number_total             8877
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bm1527.cif
_cod_data_source_block           I
_cod_original_cell_volume        3886.57(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C42.70 H31.40 Cl1.40 N4 P2 Pd'
_cod_database_code               2013248
_cod_database_fobs_code          2013248