A triclinic polymorph of bis(μ-di-<i>tert</i>-butylphosphanido)bis[(di-<i>tert</i>-butylphosphane)palladium(I)]
Breunig, Jens; Lerner, Hans-Wolfram; Bolte, Michael; Acta Crystallographica Section E 68 (2012) m836–; doi:10.1107/S1600536812023574

data_2235177
_publ_section_title
;
 A triclinic polymorph of
 bis(\m-di-<i>tert</i>-butylphosphanido)bis[(di-<i>tert</i>-butylphosphane)palladium(I)]
;
_journal_coeditor_code           NG5274
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m836
_journal_paper_doi               10.1107/S1600536812023574
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Pd2 (C8 H18 P)2 (C8 H19 P)2]'
_chemical_formula_moiety         'C32 H74 P4 Pd2'
_chemical_formula_sum            'C32 H74 P4 Pd2'
_chemical_formula_weight         795.59
_chemical_name_systematic
;
bis(\m-di-<i>tert</i>-butylphosphanido)bis[(di-<i>tert</i>-
butylphosphane)palladium(I)]
;
_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           SHELXL97
_cell_angle_alpha                89.064(5)
_cell_angle_beta                 67.307(4)
_cell_angle_gamma                75.330(5)
_cell_formula_units_Z            1
_cell_length_a                   9.0721(5)
_cell_length_b                   10.5156(6)
_cell_length_c                   11.5351(6)
_cell_measurement_reflns_used    11232
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      3.5
_cell_volume                     978.06(10)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2001)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Stoe IPDS II two-circle'
_diffrn_measurement_method       \w
_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  0.0658
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13922
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         3.51
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.102
_exptl_absorpt_correction_T_max  0.9573
_exptl_absorpt_correction_T_min  0.7857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS; Spek, 2009; Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             418
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.310
_refine_diff_density_min         -1.338
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         4481
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0669P)^2^+1.1837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1112
_reflns_number_gt                4083
_reflns_number_total             4481
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ng5274.cif
_cod_data_source_block           I
_cod_original_cell_volume        978.06(9)
_cod_database_code               2235177
_cod_database_fobs_code          2235177