Coordination chemistry and X-ray studies with novel sterically constrained diphosphonite ligands
van der Vlugt, Jarl Ivar; Sablong, Rafael; Mills, Allison M.; Kooijman, Huub; Spek, Anthony L.; Meetsma, Auke; Vogt, Dieter; Dalton Transactions  (2003) 4690–; doi:10.1039/b311328k

data_7013654
_publ_section_title
;
 Coordination chemistry and X-ray studies with novel sterically
 constrained diphosphonite ligands
;
_journal_issue                   24
_journal_name_full               'Dalton Transactions'
_journal_page_first              4690
_journal_paper_doi               10.1039/b311328k
_journal_year                    2003
_chemical_formula_moiety         'C55 H63 Cl O5 P2 Pd'
_chemical_formula_sum            'C55 H63 Cl O5 P2 Pd'
_chemical_formula_weight         1007.86
_chemical_name_systematic
;
4,5-bis{di(2-tert-butyl)-phosphonito)}-9,9-dimethylxanthene-chloropallad
ium(II)
;
_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     isomor
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.5200(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4543(1)
_cell_length_b                   26.6986(3)
_cell_length_c                   21.5052(2)
_cell_measurement_reflns_used    48439
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     5147.15(9)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Nonius COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution
'from coordinates of isostructural Pd analogue (s2700a)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f + \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45983
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_T_max  0.9898
_exptl_absorpt_correction_T_min  0.9113
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULABS in PLATON (Spek, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2104
_exptl_crystal_preparation
'recrystallized from dichloromethane/acetonitrile'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         10085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0262P)^2^+3.5153P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0774
_reflns_number_gt                7774
_reflns_number_total             10085
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b311328k.txt
_cod_data_source_block           3
_cod_original_cell_volume        5147.16(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7013654