Complexes of 2,3-bis(diphenylphosphino)propene with PtII, PdII and RuII: synthesis, characterisation and rearrangements to complexes of cis-1,2-bis(diphenylphosphino)propene
Barkley, Jim; Higgins, Simon J.; McCart, Mark K.; Journal of the Chemical Society, Dalton Transactions  (1998) 1787–; doi:10.1039/a801351i

data_7028165
_publ_contact_author
;
  Dr. S.J. Higgins
  Department of Chemistry
  University of Liverpool
  Chemistry Buildings
  Crown Street
  LIVERPOOL
  L69 7ZD
;
_publ_section_title
;
 Complexes of 2,3-bis(diphenylphosphino)propene with PtII, PdII and RuII:
 synthesis, characterisation and rearrangements to complexes of
 cis-1,2-bis(diphenylphosphino)propene
;
_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1787
_journal_paper_doi               10.1039/a801351i
_journal_year                    1998
_chemical_formula_sum            'C54 H48 B2 F8 P4 Pt'
_chemical_formula_weight         1189.56
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             1998-01-30
_audit_creation_method           'by teXsan v1.7'
_audit_update_record             ?
_cell_angle_alpha                90
_cell_angle_beta                 96.44(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.205(5)
_cell_length_b                   16.313(5)
_cell_length_c                   13.524(4)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    153.2
_cell_measurement_theta_max      15.19
_cell_measurement_theta_min      13.46
_cell_volume                     2456.4(15)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1995)'
_computing_publication_material  'teXsan (MSC, 1995)'
_computing_structure_refinement  'teXsan (MSC, 1995)'
_computing_structure_solution
;
SAPI91 (Fan, 1991)
;
_diffrn_ambient_temperature      153.2
_diffrn_measurement_device       'Rigaku AFC6S'
_diffrn_orient_matrix_UB_11      0.06202
_diffrn_orient_matrix_UB_12      -0.01660
_diffrn_orient_matrix_UB_13      -0.04383
_diffrn_orient_matrix_UB_21      0.06171
_diffrn_orient_matrix_UB_22      0.03279
_diffrn_orient_matrix_UB_23      0.04208
_diffrn_orient_matrix_UB_31      0.02027
_diffrn_orient_matrix_UB_32      -0.04906
_diffrn_orient_matrix_UB_33      0.04295
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.03133
_diffrn_reflns_av_sigmaI/netI    0.050
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4718
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        -0.31
_diffrn_standards_interval_count 0
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_exptl_absorpt_coefficient_mu    3.080
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.781
_exptl_absorpt_correction_type
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1184.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.88
_refine_diff_density_min         -4.63
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   5.899
_refine_ls_goodness_of_fit_obs   5.899
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
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_refine_ls_number_reflns         2830
_refine_ls_number_restraints     0
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_refine_ls_R_factor_obs          0.0735
_refine_ls_shift/esd_max         0.0000
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0539
_refine_ls_wR_factor_obs         0.0539
_reflns_number_observed          2830
_reflns_number_total             4482
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            i801351sup1.cif
_cod_data_source_block           SJH3_S.J.HIGGINS_29-8-96
_cod_depositor_comments
;
 Correcting the GEOM_TORSION loop by removing the _geom_torsion_site_symmetry_1
 data name and adding the _geom_torsion data name.

 Antanas Vaitkus,
 2018-08-09

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo)' 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)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2456(1)
_cod_original_sg_symbol_H-M      'P 21/n     '
_cod_original_formula_sum        'C54 H48 B2 F8 P4 Pt '
_cod_database_code               7028165