Octahedral Alkynylphosphine Ruthenium(II) Complexes: Synthesis, Structure, and Electrochemistry
Berenguer, Jesús; Bernechea, María; Fernández, Julio; Gil, Belén; Lalinde, Elena; Moreno, M. Teresa; Ruiz, Santiago; Sánchez, Sergio; Organometallics 30 (2011) 4665–; doi:10.1021/om2005194

data_4065030
_publ_section_title
;
 Octahedral Alkynylphosphine Ruthenium(II) Complexes: Synthesis,
 Structure, and Electrochemistry
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4665
_journal_paper_doi               10.1021/om2005194
_journal_volume                  30
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_sum            'C72.5 H59 Cl O1.5 P3 Ru'
_chemical_formula_weight         1183.7069
_chemical_name_common            'Compound X'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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             2010-12-20T18:45:34-00:00
_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                   13.5500(3)
_cell_length_b                   18.1803(5)
_cell_length_c                   27.7471(5)
_cell_measurement_reflns_used    28316
_cell_measurement_temperature    173.0(10)
_cell_volume                     6835.3(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.0(10)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.005047
_diffrn_orient_matrix_UB_12      -0.0218995
_diffrn_orient_matrix_UB_13      -0.0329682
_diffrn_orient_matrix_UB_21      -0.0707561
_diffrn_orient_matrix_UB_22      0.0125058
_diffrn_orient_matrix_UB_23      -0.0061494
_diffrn_orient_matrix_UB_31      0.0203628
_diffrn_orient_matrix_UB_32      0.0488827
_diffrn_orient_matrix_UB_33      -0.0131966
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.042
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13744
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.1
_exptl_absorpt_coefficient_mu    0.376
_exptl_absorpt_correction_T_max  0.9201
_exptl_absorpt_correction_T_min  0.7808
_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    1.15
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
platon (Spek 1995)
;
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.039(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         13744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+1.9893P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0959
_reflns_number_gt                12578
_reflns_number_total             13744
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om2005194_si_001.cif
_cod_data_source_block           8
_cod_original_sg_symbol_H-M      'P 212121'
_cod_database_code               4065030