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_7238469
_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_moiety         'C84 H84 Cl14 O4 P8 Pd1 Sn6'
_chemical_formula_sum            'C86 H90 Cl2 O12 P8 Pd'
_chemical_formula_weight         1740.64
_chemical_name_common            (Pd(P(PO)2)2)Cl2.2MeOH.6H2O
_chemical_name_systematic
;
[Pd(P(PO)2)2]Cl2.2MeOH.6H2O
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.495(7)
_cell_angle_beta                 98.909(7)
_cell_angle_gamma                102.948(7)
_cell_formula_units_Z            1
_cell_length_a                   11.808(6)
_cell_length_b                   13.975(7)
_cell_length_c                   15.675(7)
_cell_measurement_reflns_used    938
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.84
_cell_measurement_theta_min      2.77
_cell_volume                     2365(2)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            25012
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    0.441
_exptl_absorpt_correction_T_max  0.9131
_exptl_absorpt_correction_T_min  0.8574
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             902
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.686
_refine_diff_density_min         -1.268
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         9623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0685
_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^)+(0.1384P)^2^+4.2383P] where ==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2029
_refine_ls_wR_factor_ref         0.2402
_reflns_number_gt                7033
_reflns_number_total             9623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ra00897h.txt
_cod_data_source_block           PdOCl13
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' 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        2364.9(19)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7238469