Stereochemical Investigations of a Novel Class of Chiral Phosphapalladacycle Complexes Derived from 1-[(2,5-Dimethyl)phenyl]ethyldiphenylphosphine
Joseph Kok-Peng Ng; Yongxin Li; Geok-Kheng Tan; Lip-Lin Koh; Jagadese J. Vittal; Pak-Hing Leung; Inorganic Chemistry 44 (2005) 9874–9886; doi:10.1021/ic0509579

data_4310192
_publ_section_title
;
Stereochemical Investigations of a Novel Class of Chiral
Phosphapalladacycle Complexes Derived from
1-[(2,5-Dimethyl)phenyl]ethyldiphenylphosphine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9874
_journal_page_last               9886
_journal_paper_doi               10.1021/ic0509579
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C27 H29 O2 P Pd'
_chemical_formula_weight         522.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5880(7)
_cell_length_b                   26.560(2)
_cell_length_c                   9.5467(7)
_cell_measurement_reflns_used    4774
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      24.923
_cell_measurement_theta_min      2.258
_cell_volume                     2431.1(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w 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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            19132
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_max  0.9351
_exptl_absorpt_correction_T_min  0.8485
_exptl_absorpt_correction_type   'Sadabs, (Sheldrick 2001)'
_exptl_crystal_colour            PALE_YELLOW
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'RECTANGULAR BLOCK'
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         6897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0883
_reflns_number_gt                5695
_reflns_number_total             6897
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0509579si20050614_025810.cif
_cod_data_source_block           2070a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2431.2(3)
_cod_database_code               4310192