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_4079301
_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_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C42 H42 Cl1 N1 P2 Ru1'
_chemical_formula_sum            'C50 H56 Cl N O P2 Ru'
_chemical_formula_weight         885.42
_chemical_name_common            'compound 7 '
_chemical_name_systematic
;
        ?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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             2012-04-27T13:49:57-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.420(5)
_cell_length_b                   15.661(3)
_cell_length_c                   10.368(2)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      1
_cell_measurement_wavelength     0.71073
_cell_volume                     4289.9(14)
_computing_cell_refinement       'hkl2000 software (Enraf-Nonius, 2000)'
_computing_data_collection       'hkl2000 software (Enraf-Nonius, 2000)'
_computing_data_reduction        'WinGx (Ferrugia Louis, 2000)'
_computing_molecular_graphics    'WinGx (Ferrugia Louis, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SHELXS-97(Sheldrick 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Enraf-Nonius CCD'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.81806E-1
_diffrn_orient_matrix_UB_12      -0.333834E-1
_diffrn_orient_matrix_UB_13      -0.32432E-2
_diffrn_orient_matrix_UB_21      0.114445E-1
_diffrn_orient_matrix_UB_22      0.19042E-2
_diffrn_orient_matrix_UB_23      0.375658E-1
_diffrn_orient_matrix_UB_31      -0.498021E-1
_diffrn_orient_matrix_UB_32      -0.543987E-1
_diffrn_orient_matrix_UB_33      0.33052E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.058
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            32878
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.3
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  0.9735
_exptl_absorpt_correction_T_min  0.8995
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
        Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
        for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
        p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
        A31,146-148) is used with some modification.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.414
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         8855
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+8.8057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1099
_reflns_number_gt                7281
_reflns_number_total             8855
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om300657z_si_009.cif
_cod_data_source_block           apami20
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'heavy-atom-method' was changed
to 'heavy'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        4289.7(15)
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               4079301