Palladium(II) Complexes of Monoaryliminophosphorane Derivatives of 1,2-Bis(Diphenylphosphino)methane. Crystal Structure of [Pd{κ2-C6H3(NN−C6H4Me-4‘)-2- (C6H4Me-4‘‘)-5-C,N‘}{κ2-PPh2CH2P(NC6H4Me-4)Ph2-P,N}]†
Vicente, José; Arcas, Aurelia; Bautista, Delia; Ramírez de Arellano, M. Carmen; Organometallics 17 (1998) 4544–; doi:10.1021/om980445k

data_4078405
_publ_section_title
;
 Palladium(II) Complexes of Monoaryliminophosphorane Derivatives of
 1,2-Bis(Diphenylphosphino)methane. Crystal Structure of
 [Pd{\k2-C6H3(NN&#x2212;C6H4Me-4&#x2018;)-2-
 (C6H4Me-4&#x2018;&#x2018;)-5-C,N&#x2018;}{\k2-PPh2CH2P(NC6H4Me-4)Ph2-P,N}]&#x2020;
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4544
_journal_paper_doi               10.1021/om980445k
_journal_volume                  17
_journal_year                    1998
_chemical_formula_sum            'C47 H42 F3 N3 O3 P2 Pd S'
_chemical_formula_weight         954.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 117.019(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.439(2)
_cell_length_b                   14.5052(11)
_cell_length_c                   18.754(2)
_cell_measurement_reflns_used    63
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      12.47
_cell_measurement_theta_min      2.80
_cell_volume                     4468.5(8)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Siemens 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  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18750
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        1.55
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.754
_exptl_absorpt_correction_type   'Psi scans'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       prism
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.001
_refine_ls_goodness_of_fit_obs   1.091
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         7858
_refine_ls_number_restraints     928
_refine_ls_restrained_S_all      0.958
_refine_ls_restrained_S_obs      1.025
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_obs          0.0344
_refine_ls_shift/esd_max         -0.036
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0785
_refine_ls_wR_factor_obs         0.0723
_reflns_number_observed          5786
_reflns_number_total             7858
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om980445k.cif
_cod_data_source_block           dbc01
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+0.0000P] 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^)+(0.0404P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4468.6(7)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4078405