Synthesis, Coordination Characteristics, Conformational Behavior, and Bond Reactivity Studies of a Novel Chiral Phosphapalladacycle Complex
Ding, Yi; Chiang, Minyi; Pullarkat, Sumod A.; Li, Yongxin; Leung, Pak-Hing; Organometallics 28 (2009) 4358–; doi:10.1021/om900423f

data_4069812
_publ_section_title
;
 Synthesis, Coordination Characteristics, Conformational Behavior, and
 Bond Reactivity Studies of a Novel Chiral Phosphapalladacycle Complex
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4358
_journal_paper_doi               10.1021/om900423f
_journal_volume                  28
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_sum            'C31.5 H33 Cl N O2 P Pd'
_chemical_formula_weight         630.41
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            8
_cell_length_a                   11.0151(3)
_cell_length_b                   13.9586(4)
_cell_length_c                   37.1293(12)
_cell_measurement_reflns_used    6826
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.26
_cell_measurement_theta_min      2.42
_cell_volume                     5708.8(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            62466
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_T_max  0.9366
_exptl_absorpt_correction_T_min  0.8011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.614
_refine_diff_density_min         -1.542
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         15144
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0713P)^2^+8.6034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1391
_reflns_number_gt                13946
_reflns_number_total             15144
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900423f_si_011.cif
_cod_data_source_block           leung257
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_original_formula_sum        'C31.50 H33 Cl N O2 P Pd'
_cod_database_code               4069812