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_7028166
_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_moiety         'C32 H29 Cl P2 Ru '
_chemical_formula_sum            'C32 H29 Cl P2 Ru'
_chemical_formula_weight         612.05
_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                 110.58(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.866(9)
_cell_length_b                   11.297(6)
_cell_length_c                   17.389(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      6.5
_cell_measurement_theta_min      3.5
_cell_volume                     2734(3)
_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)'
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC6S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.01121
_diffrn_orient_matrix_UB_12      -0.06493
_diffrn_orient_matrix_UB_13      0.03468
_diffrn_orient_matrix_UB_21      -0.04197
_diffrn_orient_matrix_UB_22      -0.04175
_diffrn_orient_matrix_UB_23      -0.05060
_diffrn_orient_matrix_UB_31      0.05723
_diffrn_orient_matrix_UB_32      -0.04333
_diffrn_orient_matrix_UB_33      -0.00321
_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  0.02964
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
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_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5297
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        -1.40
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow/orange
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_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
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_refine_diff_density_max         0.76
_refine_diff_density_min         -0.26
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     325
_refine_ls_number_reflns         3770
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0300
_refine_ls_shift/esd_max         0.1268
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0382
_reflns_number_observed          3770
_reflns_number_total             5092
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            i801351sup1.cif
_cod_data_source_block           MMC4_M.MCCART_/_S.HIGGINS_
_cod_depositor_comments
;
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) +
0.00022|Fo|^2^]' 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) + 0.00022|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2734(2)
_cod_original_sg_symbol_H-M      'P 21/n     '
_cod_original_formula_sum        'C32 H29 Cl P2 Ru '
_cod_database_code               7028166