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_7057542
_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         'C75 H57 Cl0 O9 P3 Ru3 S6'
_chemical_formula_sum            'C75 H57 Cl0 O9 P3 Ru3 S6'
_chemical_formula_weight         1690.69
_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_Hall  '-P 2ybc'
_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
_audit_update_record
;
2017-11-24 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.353(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.509(1)
_cell_length_b                   32.409(2)
_cell_length_c                   18.939(2)
_cell_measurement_reflns_used    6081
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.42
_cell_measurement_theta_min      2.27
_cell_volume                     9035.1(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0944
_diffrn_reflns_av_sigmaI/netI    0.1056
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            69529
_diffrn_reflns_theta_full        26.61
_diffrn_reflns_theta_max         26.61
_diffrn_reflns_theta_min         1.30
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3408
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.409
_refine_diff_density_min         -1.246
_refine_diff_density_rms         0.191
_refine_ls_extinction_coef       0.00212(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         18629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0743
_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^)+(0.1247P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2057
_refine_ls_wR_factor_ref         0.2216
_reflns_number_gt                11988
_reflns_number_total             18629
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8nj01442f2.cif
_cod_data_source_block           sq
_cod_depositor_comments
'Adding full bibliography for 7057540--7057543.cif.'
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7057542