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_4065027
_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            'C96 H76 Cl2 Fe4 P4 Ru'
_chemical_formula_weight         1748.82
_chemical_name_common            s259
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_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      2.3
_audit_creation_date             2010-12-14T16:51:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.5247(8)
_cell_length_b                   19.5247(8)
_cell_length_c                   9.9352(3)
_cell_measurement_reflns_used    6133
_cell_measurement_temperature    100.0(10)
_cell_volume                     3787.4(2)
_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, 1997)'
_diffrn_ambient_temperature      100.0(10)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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      0.0392606
_diffrn_orient_matrix_UB_12      -0.0121125
_diffrn_orient_matrix_UB_13      -0.0600945
_diffrn_orient_matrix_UB_21      -0.0315178
_diffrn_orient_matrix_UB_22      -0.0002406
_diffrn_orient_matrix_UB_23      -0.079336
_diffrn_orient_matrix_UB_31      0.0094037
_diffrn_orient_matrix_UB_32      0.0497637
_diffrn_orient_matrix_UB_33      -0.0150106
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            20200
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.76
_exptl_absorpt_coefficient_mu    1.148
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.8507
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1788
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), 1691 Friedel pairs'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.857
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.857
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+7.9917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.096
_reflns_number_gt                3296
_reflns_number_total             3854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2005194_si_001.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      P_-4_21_c
_cod_database_code               4065027