Reaction of carbonyl trinuclear clusters with 2,5-bis(2-thienyl)-1-phenyl-phosphole as a ligand: a new pathway to ruthenacyclopentadiene and cyclopentadienone ruthenium complexes
Otero, Yomaira; Peña, Deisy; Lescop, Christophe; Ávila, Edward; Arce, Alejandro; Hissler, Muriel; Réau, Regis; Machado, Rubén; New Journal of Chemistry 42 (2018) 12234–; doi:10.1039/C8NJ01442F

data_7057540
_publ_section_title
;
 Reaction of carbonyl trinuclear clusters with
 2,5-bis(2-thienyl)-1-phenyl-phosphole as a ligand: a new pathway to
 ruthenacyclopentadiene and cyclopentadienone ruthenium complexes
;
_journal_issue                   14
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12234
_journal_paper_doi               10.1039/C8NJ01442F
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C55 H40 Cl2 O10 Os3 P2 S4'
_chemical_formula_sum            'C55 H40 Cl2 O10 Os3 P2 S4'
_chemical_formula_weight         1692.55
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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           SHELXL-97
_audit_update_record
;
2017-10-12 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.276(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2208(5)
_cell_length_b                   20.4111(9)
_cell_length_c                   24.2182(9)
_cell_measurement_reflns_used    5689
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      2.64
_cell_volume                     5419.8(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       none
_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  0.0784
_diffrn_reflns_av_sigmaI/netI    0.0999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            35824
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.32
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    7.387
_exptl_absorpt_correction_T_max  0.5538
_exptl_absorpt_correction_T_min  0.3302
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sheldrick,G.M.(2002).SADABS BrukerAXS Inc.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.074
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3224
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.771
_refine_diff_density_min         -3.284
_refine_diff_density_rms         0.560
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         12425
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0876P)^2^+11.4219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1521
_refine_ls_wR_factor_ref         0.1818
_reflns_number_gt                8725
_reflns_number_total             12425
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8nj01442f2.cif
_cod_data_source_block           import
_cod_depositor_comments
'Adding full bibliography for 7057540--7057543.cif.'
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7057540