New enantiopure palladium(II) complexes from a stereodynamic 2,2'-biphosphole ligand
Diab, Lisa; Daran, Jean-Claude; Gouygou, Maryse; Manoury, Eric; Urrutigoïty, Martine; Acta Crystallographica Section C 64 (2008) m43–m45; doi:10.1107/S0108270107049347

data_2016414
_publ_section_title
;
 New enantiopure palladium(II) complexes from a stereodynamic
 2,2'-biphosphole ligand
;
_journal_coeditor_code           SQ3103
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m43
_journal_page_last               m45
_journal_paper_doi               10.1107/S0108270107049347
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Pd Cl2 (C28 H30 P2)] , C H2 Cl2'
_chemical_formula_moiety         'C28 H30 Cl2 P2 Pd , C H2 Cl2'
_chemical_formula_sum            'C29 H32 Cl4 P2 Pd'
_chemical_formula_weight         690.69
_chemical_name_common
;
dichlorido[1,1'-(butane-1,3-diyl)-3,3',4,4'-tetramethyl-5,5'-diphenyl-2,2'-
biphosphole]palladium(II) dichloromethane solvate
;
_chemical_name_systematic
;
dichlorido(1,2,5,10,11-pentamethyl-3,9-
diphenylperhydrodicyclopenta[a,c][1,4]diphosphepine-\k^2^P,P')palladium(II)
dichloromethane solvate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.87(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.963(3)
_cell_length_b                   12.139(5)
_cell_length_c                   13.989(6)
_cell_measurement_reflns_used    1192
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      2.9
_cell_volume                     1477.7(10)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.2632
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur'
_diffrn_measurement_method       '\w and \f'
_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  0.0786
_diffrn_reflns_av_sigmaI/netI    0.2894
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5431
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    1.116
_exptl_absorpt_correction_T_max  0.791
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2006) (empirical absorption
correction using
spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       box
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.663
_refine_diff_density_min         -1.297
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs?'
_refine_ls_abs_structure_Flack   -0.02(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         4033
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.1593
_refine_ls_R_factor_gt           0.0799
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0951P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1760
_refine_ls_wR_factor_ref         0.2256
_reflns_number_gt                1900
_reflns_number_total             4033
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sq3103.cif
_cod_data_source_block           4b
_cod_original_cell_volume        1477.6(10)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2016414
_cod_database_fobs_code          2016414