Half-Sandwich Ruthenium-Phosphine Complexes with Pentadienyl and Oxo- and Azapentadienyl Ligands
Reyna-Madrigal, Amira; Moreno-Gurrola, Anabel; Perez-Camacho, Odilia; Navarro-Clemente, M. Elena; Juárez-Saavedra, Patricia; Leyva-Ramirez, Marco A.; Arif, Atta M.; Ernst, Richard D.; Paz-Sandoval, M. Angeles; Organometallics 31 (2012) 7125–; doi:10.1021/om300657z

data_4079304
_publ_section_title
;
 Half-Sandwich Ruthenium-Phosphine Complexes with Pentadienyl and Oxo- and
 Azapentadienyl Ligands
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              7125
_journal_paper_doi               10.1021/om300657z
_journal_volume                  31
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C42 H38 O P2 Ru, 0.5(C6 H6), 0.5(C4 H10 O)'
_chemical_formula_sum            'C47 H46 O1.5 P2 Ru'
_chemical_formula_weight         797.8
_chemical_name_common            'Compound 14'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2012-04-13T15:55:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.5690(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.86590(10)
_cell_length_b                   23.4861(4)
_cell_length_c                   15.9331(2)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      1
_cell_measurement_wavelength     0.71073
_cell_volume                     4053.17(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      198(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.785579E-1
_diffrn_orient_matrix_UB_12      -0.101544E-1
_diffrn_orient_matrix_UB_13      -0.336463E-1
_diffrn_orient_matrix_UB_21      -0.318179E-1
_diffrn_orient_matrix_UB_22      -0.178445E-1
_diffrn_orient_matrix_UB_23      0.509914E-1
_diffrn_orient_matrix_UB_31      -0.36607E-1
_diffrn_orient_matrix_UB_32      0.373012E-1
_diffrn_orient_matrix_UB_33      0.152343E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0926
_diffrn_reflns_av_unetI/netI     0.0877
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            64110
_diffrn_reflns_theta_full        25.5
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.51
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_T_max  0.9231
_exptl_absorpt_correction_T_min  0.8064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.572
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         9260
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1322
_refine_ls_R_factor_gt           0.0647
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+4.6931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1478
_reflns_number_gt                5472
_reflns_number_total             9260
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om300657z_si_012.cif
_cod_data_source_block           apana003
_cod_depositor_comments
;

2021-08-27
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C94 H92 O3 P4 Ru2'
_cod_original_formula_weight         1595.7
_cod_original_formula_moiety         'C42 H39 Cl1 O1 Ru1'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4079304