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_7057541
_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_sum            'C41 H33 O3 P Ru S4'
_chemical_formula_weight         833.95
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-02-06 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                93.359(3)
_cell_angle_beta                 90.408(2)
_cell_angle_gamma                104.584(3)
_cell_formula_units_Z            2
_cell_length_a                   10.2565(7)
_cell_length_b                   10.3981(8)
_cell_length_c                   16.9286(13)
_cell_measurement_reflns_used    4991
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.29
_cell_volume                     1743.8(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by SAINT Bruker-AXS'
_diffrn_orient_matrix_UB_11      -0.684302E-1
_diffrn_orient_matrix_UB_12      -0.809254E-1
_diffrn_orient_matrix_UB_13      -0.218574E-1
_diffrn_orient_matrix_UB_21      0.121043E-1
_diffrn_orient_matrix_UB_22      0.342338E-1
_diffrn_orient_matrix_UB_23      -0.54149E-1
_diffrn_orient_matrix_UB_31      0.729766E-1
_diffrn_orient_matrix_UB_32      -0.468258E-1
_diffrn_orient_matrix_UB_33      -0.96648E-2
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0742
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13368
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.403
_diffrn_reflns_theta_min         2.357
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick,G.M.(2002). SADABS, Bruker AXS Inc.'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         7037
_refine_ls_number_restraints     113
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+1.0259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1344
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5822
_reflns_number_total             7037
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj01442f2.cif
_cod_data_source_block           Compound_5
_cod_depositor_comments
'Adding full bibliography for 7057540--7057543.cif.'
_cod_database_code               7057541
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              81123