Chiral palladium complexes from N-diphenylphosphinoamino methyl esters
Zhang, Qingzhi; Slawin, Alexandra M. Z.; Woollins, J. Derek; Journal of the Chemical Society, Dalton Transactions  (2001) 3598–; doi:10.1039/b104571g

data_7010860
_publ_section_title
;
 Chiral palladium complexes from N-diphenylphosphinoamino methyl esters
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3598
_journal_paper_doi               10.1039/b104571g
_journal_year                    2001
_chemical_formula_analytical     'C32.50 H35 Cl3 N2 O4 P2 Pd2 S2'
_chemical_formula_moiety         'C32 H34 Cl2 N2 O4 P2 Pd2 S2.[C H2 Cl2]0.5'
_chemical_formula_structural     'C32.50 H35 Cl3 N2 O4 P2 Pd2 S2'
_chemical_formula_sum            'C32.5 H35 Cl3 N2 O4 P2 Pd2 S2'
_chemical_formula_weight         962.84
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.86210(10)
_cell_length_b                   18.7870(3)
_cell_length_c                   9.1333(2)
_cell_measurement_reflns_used    94
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      168
_cell_measurement_theta_min      12
_cell_volume                     2035.39(6)
_computing_cell_refinement       SMART/SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       SMART
_diffrn_measurement_method       CCD
_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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9025
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    1.297
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.683248
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       prism
_exptl_crystal_F_000             962
_exptl_crystal_size_max          .14
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .4
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.06(5)
_refine_ls_extinction_coef       0.0017(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.129
_refine_ls_goodness_of_fit_obs   1.135
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2883
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.446
_refine_ls_restrained_S_obs      1.134
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_obs          0.0344
_refine_ls_shift/esd_max         4.562
_refine_ls_shift/esd_mean        0.351
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+1.6788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1154
_refine_ls_wR_factor_obs         0.0875
_reflns_number_observed          2695
_reflns_number_total             2928
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b104571g.txt
_cod_data_source_block           7
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+1.6788P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+1.6788P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2
_cod_original_formula_sum        'C32.50 H35 Cl3 N2 O4 P2 Pd2 S2'
_cod_database_code               7010860