Synthesis, Structure, and Reactivity of [RuCl(PP)]PF~6~ (PP = (PPh~3~)~2~, Ph~2~P(CH~2~)~4~PPh~2~; L = Ppy~3~, PPhpy~2~; py = 2-pyridyl). The "Missing" P,N,N'-Coordination Mode for 2-Pyridylphosphines
Richard P. Schutte; Steven J. Rettig; Ajey M. Joshi; Brian R. James; Inorganic Chemistry 36 (1997) 5809–5817; doi:10.1021/ic970835j

data_4323712
_publ_contact_author_address
;
University of British Columbia
Department of Chemistry
2036 Main Mall
Vancouver, BC V6T 1Z1
Canada
;
_publ_contact_author_email       ' xtal@xray5.chem.ubc.ca '
_publ_contact_author_fax         ' 604-822-2847 '
_publ_contact_author_name        ' Brian R. James'
_publ_contact_author_phone       ' 604-822-6645 '
_publ_section_title
;
 Synthesis, Structure, and Reactivity of [RuCl(PP)]PF~6~ (PP =
 (PPh~3~)~2~, Ph~2~P(CH~2~)~4~PPh~2~; L = Ppy~3~, PPhpy~2~; py =
 2-pyridyl). The "Missing" P,N,N'-Coordination Mode for
 2-Pyridylphosphines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5809
_journal_page_last               5817
_journal_paper_doi               10.1021/ic970835j
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C52 H43 Cl F6 N2 P4 Ru'
_chemical_formula_weight         1070.33
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             1997-08-11
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
?
;
_cell_angle_alpha                90
_cell_angle_beta                 97.012(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.795(2)
_cell_length_b                   11.375(4)
_cell_length_c                   23.343(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.2
_cell_measurement_theta_max      15.1
_cell_measurement_theta_min      12.6
_cell_volume                     4689.7(18)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
'DIRDIF92 PATTY (Beurskens, 1992)
;
_diffrn_ambient_temperature      294.2
_diffrn_measurement_device_type  'Rigaku AFC6S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.02036
_diffrn_orient_matrix_UB_12      -0.08032
_diffrn_orient_matrix_UB_13      -0.01001
_diffrn_orient_matrix_UB_21      -0.04704
_diffrn_orient_matrix_UB_22      0.03569
_diffrn_orient_matrix_UB_23      -0.02069
_diffrn_orient_matrix_UB_31      0.02404
_diffrn_orient_matrix_UB_32      0.00179
_diffrn_orient_matrix_UB_33      -0.03654
_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  0.03737
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            14722
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0.80
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.591
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.955
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2176.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.44
_refine_ls_extinction_coef       0.000000074(4)
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_ref   1.730
_refine_ls_hydrogen_treatment    'C-H riding'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     596
_refine_ls_number_reflns         7690
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/esd_max         0.0030
_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_ref         0.0350
_reflns_number_gt                7690
_reflns_number_total             14304
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            ic970835j_2.cif
_cod_data_source_block           bj196/RuCl(PPh3)2(PPhpy2)P
_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)]' 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        4689.8(13)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C52 H43 Cl F6 N2 P4 Ru '
_cod_database_code               4323712