Reactions of the Cationic Fragments [RuCp(PPh2NHR)2]+and [RuTp(PPh2NHR)2]+(R = Ph,n-Pr) with Alkynes: Formation of Four-Membered Azaphosphacarbenes
Pavlik, Sonja; Mereiter, Kurt; Puchberger, Michael; Kirchner, Karl; Organometallics 24 (2005) 3561–; doi:10.1021/om050247a

data_4089342
_publ_section_title
;
 Reactions of the Cationic Fragments [RuCp(PPh2NHR)2]+and
 [RuTp(PPh2NHR)2]+(R = Ph,n-Pr) with Alkynes:&#x00A0; Formation of
 Four-Membered Azaphosphacarbenes
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3561
_journal_paper_doi               10.1021/om050247a
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety
'(C53 H48 B N8 P2 Ru 1+), (F6 Sb 1-), 2(C6 H5 F)'
_chemical_formula_sum            'C65 H58 B F8 N8 P2 Ru Sb'
_chemical_formula_weight         1398.76
_chemical_name_common
;
[RuTp(kappa^2^(C,P)=C(CH~2~Ph)N(Ph)PPh~2~)
(kappa^1^(P)-PPh~2~NHPh)]SbF~6~.2C~6~H~5~F
     (14a.2C~6~H~5~F) 
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.726(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.403(2)
_cell_length_b                   17.341(4)
_cell_length_c                   31.492(7)
_cell_measurement_reflns_used    865
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      2.3
_cell_volume                     6184(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT, SADABS, XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2071
_diffrn_reflns_av_sigmaI/netI    0.2274
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28346
_diffrn_reflns_theta_full        23.12
_diffrn_reflns_theta_max         23.12
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2824
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         8639
_refine_ls_number_restraints     573
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.2321
_refine_ls_R_factor_gt           0.0874
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1037P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1930
_refine_ls_wR_factor_ref         0.2634
_reflns_number_gt                3246
_reflns_number_total             8639
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050247asi20050402_100602.cif
_cod_data_source_block           compd14a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/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_sg_symbol_H-M      'P2(1)/c  '
_cod_database_code               4089342