Two complexes derived from the reaction of <i>M</i>~3~(CO)~12~ clusters (<i>M</i> = Ru, Os) with the 9-(triphenylphosphonio)fluorenide ylide: tricarbonyl[9-(triphenylphosphonio)fluorenylidene]ruthenium and nonacarbonyl-μ~3~-fluorenylidene-μ~2~-hydrido-<i>triangulo</i>-triosmium(III)
Arce, Alejandro; De Sanctis, Ysaura; Galarza, Esperanza; Garland, María Teresa; Baggio, Ricardo; Acta Crystallographica Section C 69 (2013) 363–366; doi:10.1107/S0108270113005489

data_2018899
_publ_section_title
;
 Two complexes derived from the reaction of <i>M</i>~3~(CO)~12~ clusters
 (<i>M</i> = Ru, Os) with the 9-(triphenylphosphonio)fluorenide ylide:
 tricarbonyl[9-(triphenylphosphonio)fluorenylidene]ruthenium and
 nonacarbonyl-\m~3~-fluorenylidene-\m~2~-hydrido-<i>triangulo</i>-triosmium(III)
;
_journal_coeditor_code           DT3019
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              363
_journal_page_last               366
_journal_paper_doi               10.1107/S0108270113005489
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Ru (C31 H21 P) (C O)3]'
_chemical_formula_moiety         'C34 H21 O3 P Ru'
_chemical_formula_sum            'C34 H21 O3 P Ru'
_chemical_formula_weight         609.55
_chemical_name_systematic
;
Tricarbonyl[9-(triphenylphosphonio)fluorenylidene]ruthenium
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.50(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.029(7)
_cell_length_b                   15.242(5)
_cell_length_c                   17.922(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      5
_cell_volume                     2734(2)
_computing_cell_refinement       'P3/P4-PC (Siemens, 1991)'
_computing_data_collection       'P3/P4-PC (Siemens, 1991)'
_computing_data_reduction        'P3/P4-PC (Siemens, 1991)'
_computing_molecular_graphics    'SHELXTL-NT (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL-NT (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens R3m'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_av_sigmaI/netI    0.1183
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            4957
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(XEMP in SHELXTL-NT; Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.460
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4799
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0647
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^))^2^+4.5949P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0807
_reflns_number_gt                2864
_reflns_number_total             4799
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dt3019.cif
_cod_data_source_block           I
_cod_original_cell_volume        2735(2)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2018899
_cod_database_fobs_code          2018899