A chloro-bridged dinuclear phosphinitopalladium complex, di-μ-chloro-bis[(diphenoxyphosphinite-κ<i>P</i>)(diphenoxyphosphinito-κ<i>P</i>)palladium(II)]
Gniewek, Andrzej; Pryjomska-Ray, Iweta; Trzeciak, Anna M.; Ziółkowski, Józef J.; Lis, Tadeusz; Acta Crystallographica Section C 62 (2006) m491–m494; doi:10.1107/S0108270106034500

data_2015608
_publ_section_title
;A chloro-bridged dinuclear phosphinitopalladium complex,
 di-\m-chloro-bis[(diphenoxyphosphinite-\k<i>P</i>)(diphenoxyphosphinito-\k<i>P</i>)palladium(II)]
;
_journal_coeditor_code           GG3039
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m491
_journal_page_last               m494
_journal_paper_doi               10.1107/S0108270106034500
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Pd2 (C12 H10 O3 P)2 Cl2 (C12 H11 O3 P)2]'
_chemical_formula_moiety         'C48 H42 Cl2 O12 P4 Pd2'
_chemical_formula_sum            'C48 H42 Cl2 O12 P4 Pd2'
_chemical_formula_weight         1218.40
_chemical_name_systematic
;
di-\m-chloro-bis[(diphenoxyphosphinite-\kP)(diphenoxyphosphinito-
\kP)palladium(II)]
;
_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     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 106.78(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.268(3)
_cell_length_b                   10.514(2)
_cell_length_c                   19.549(4)
_cell_measurement_reflns_used    28302
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      37.50
_cell_measurement_theta_min      4.50
_cell_volume                     2414.2(10)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Kuma KM-4 CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0831
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            57621
_diffrn_reflns_theta_full        37.50
_diffrn_reflns_theta_max         37.50
_diffrn_reflns_theta_min         4.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.051
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.042
_refine_diff_density_min         -0.753
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         12649
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0362P)^2^+0.8428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                8606
_reflns_number_total             12649
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg3039.cif
_cod_data_source_block           I
_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_enum 1527 2010-12-29 10:47:43Z saulius 

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 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2015608
_cod_database_fobs_code          2015608