Unexpected coupling between an h5-indenyl ligand and alkenyl-vinylidene fragments: Synthesis of unprecedented (h6-indene)-ruthenium(II) metallacycles
Gimeno Jose; Victorio Cadierno; Salvador Conejero; Josefina Diez; M. Pilar Gamasa; Santiago Garcia-granda; Chemical communications (Cambridge, England)  (2003) –; doi:10.1039/b212406h

data_7104042
_publ_section_title
;
Unexpected coupling between an h5-indenyl ligand
and alkenyl-vinylidene fragments: Synthesis of unprecedented
(h6-indene)-ruthenium(II) metallacycles
;
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/b212406h
_journal_year                    2003
_chemical_compound_source        synthesis
_chemical_formula_sum            'C70 H65 B F4 O1.5 P2 Ru'
_chemical_formula_weight         1180.04
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.118(2)
_cell_angle_beta                 80.999(2)
_cell_angle_gamma                83.676(2)
_cell_formula_units_Z            4
_cell_length_a                   14.7232(5)
_cell_length_b                   18.8325(7)
_cell_length_c                   21.3164(9)
_cell_measurement_temperature    120(2)
_cell_volume                     5479.4(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowki & Minor 1997)'
_computing_data_collection       'Collet (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-96 (Beurskens, 1996)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       '95 mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f and \w scan'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.091
_diffrn_reflns_av_sigmaI/netI    0.115
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            158352
_diffrn_reflns_theta_full        69.81
_diffrn_reflns_theta_max         69.81
_diffrn_reflns_theta_min         2.22
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.364
_exptl_absorpt_correction_T_max  0.775
_exptl_absorpt_correction_T_min  0.520
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XABS (Parkin, Moezzi & Hope, 1995)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1432
_refine_ls_number_reflns         20043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1587
_reflns_number_gt                12474
_reflns_number_total             20043
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b212406h.txt
_cod_data_source_block           6b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'C70 H65 B F4 O1.50 P2 Ru'
_cod_database_code               7104042