A facile method for the synthesis of heterobimetallic chloro-bridged complexes containing (R3P)2MCl (M = Pt or Pd) fragments
Polborn, Kurt; Severin, Kay; Journal of the Chemical Society, Dalton Transactions  (1999) 759–; doi:10.1039/a808210c

data_7027155
_publ_section_title
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 A facile method for the synthesis of heterobimetallic chloro-bridged
 complexes containing (R3P)2MCl (M&#x2005;=&#x2005;Pt or Pd) fragments
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_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              759
_journal_paper_doi               10.1039/a808210c
_journal_year                    1999
_chemical_formula_moiety         'C27 H59 CL2 P2 Pd Pt         B F4'
_chemical_formula_sum            'C27 H59 B Cl2 F4 P2 Pd Pt'
_chemical_formula_weight         904.88
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00(2)
_cell_angle_beta                 104.745(15)
_cell_angle_gamma                90.00(2)
_cell_formula_units_Z            4
_cell_length_a                   13.675(2)
_cell_length_b                   14.791(3)
_cell_length_c                   19.451(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      9
_cell_volume                     3804.7(13)
_computing_cell_refinement       CAD4(Nonius,_1977)
_computing_data_collection       CAD4(Nonius,_1977)
_computing_data_reduction        process_MOLEN(Fair,_1990)
_computing_molecular_graphics    ZORTEP(Zsolnai,_1994)
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       Nonius_CAD4
_diffrn_measurement_method       \o-2\T-scan
_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  0.0938
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6153
_diffrn_reflns_theta_max         23.99
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        -5.2
_diffrn_standards_interval_time  7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.405
_exptl_absorpt_correction_T_max  0.9975
_exptl_absorpt_correction_T_min  0.6635
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_description       bloc
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          .53
_exptl_crystal_size_mid          .37
_exptl_crystal_size_min          .27
_refine_diff_density_max         1.305
_refine_diff_density_min         -1.527
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.162
_refine_ls_goodness_of_fit_obs   1.178
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         5961
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.161
_refine_ls_restrained_S_obs      1.175
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_obs          0.0520
_refine_ls_shift/esd_max         0.079
_refine_ls_shift/esd_mean        0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0765P)^2^+2.8249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1426
_refine_ls_wR_factor_obs         0.1241
_reflns_number_observed          4478
_reflns_number_total             5961
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            808210csup1.cif
_cod_data_source_block           Severin_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0765P)^2^+2.8249P] 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^)+(0.0765P)^2^+2.8249P] 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        3804.7(12)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7027155