Transition of trigonal-bipyramidal to square-planar geometries by oxidation of a coordinated tripodal polyphosphine in Pd(ii) and Pt(ii) complexes
Fernández-Anca, Damián; García-Seijo, M. Inés; García-Fernández, M. Esther; RSC Adv. 2 (2012) 1404–; doi:10.1039/C1RA00897H

data_7238468
_publ_section_title
;
 Transition of trigonal-bipyramidal to square-planar geometries by
 oxidation of a coordinated tripodal polyphosphine in Pd(ii) and Pt(ii)
 complexes
;
_journal_issue                   4
_journal_name_full               'RSC Adv.'
_journal_page_first              1404
_journal_paper_doi               10.1039/C1RA00897H
_journal_volume                  2
_journal_year                    2012
_chemical_formula_sum            'C88 H84 Cl14 P8 Pd'
_chemical_formula_weight         1992.01
_chemical_name_common            (Pd(PP3)2)Cl2.4CHCl3
_chemical_name_systematic
;
[Pd(PP3)2]Cl2.4CHCl3
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 93.440(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.942(2)
_cell_length_b                   18.073(3)
_cell_length_c                   17.298(3)
_cell_measurement_reflns_used    949
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.9965
_cell_measurement_theta_min      2.358
_cell_volume                     4662.9(13)
_computing_cell_refinement       'BRUKER Smart'
_computing_data_collection       'BRUKER Smart'
_computing_data_reduction        'BRUKER Shelxtl'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, =999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '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  0.0848
_diffrn_reflns_av_sigmaI/netI    0.1638
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            28588
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_T_max  0.9474
_exptl_absorpt_correction_T_min  0.8919
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.325
_refine_diff_density_min         -2.433
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         9528
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.1769
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+0.0000P] where ==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1506
_refine_ls_wR_factor_ref         0.1999
_reflns_number_gt                3947
_reflns_number_total             9528
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ra00897h.txt
_cod_data_source_block           dami13*
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        4662.8(13)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7238468