A Ruthenated [3]Dendralene from Phenylethyne and an η3-Butadienyl‒Ruthenium Complex
Bruce, Michael I.; Skelton, Brian W.; Zaitseva, Natasha N.; Organometallics 31 (2012) 5034–; doi:10.1021/om300366g

data_4078720
_publ_section_title
;
 A Ruthenated [3]Dendralene from Phenylethyne and an
 \h3-Butadienyl--Ruthenium Complex
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              5034
_journal_paper_doi               10.1021/om300366g
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C69 H51 N5 P2 Ru2, C7 H8, C H Cl3'
_chemical_formula_sum            'C77 H60 Cl3 N5 P2 Ru2'
_chemical_formula_weight         1425.73
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_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_date             2012-04-16T11:28:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 111.963(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.233(2)
_cell_length_b                   21.0315(9)
_cell_length_c                   20.908(3)
_cell_measurement_reflns_used    12559
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.8691
_cell_measurement_theta_min      2.5054
_cell_volume                     6620.0(15)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
        (compiled Feb 27 2009,15:38:38)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
        (compiled Feb 27 2009,15:38:38)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
        (compiled Feb 27 2009,15:38:38)
;
_computing_molecular_graphics    'OrtepII (Johnson, C. K. (1976)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.92
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0339586181
_diffrn_orient_matrix_UB_12      -0.0187518046
_diffrn_orient_matrix_UB_13      -0.0241870176
_diffrn_orient_matrix_UB_21      0.0107189254
_diffrn_orient_matrix_UB_22      0.0130105727
_diffrn_orient_matrix_UB_23      -0.0274024722
_diffrn_orient_matrix_UB_31      0.0309937058
_diffrn_orient_matrix_UB_32      -0.0250125038
_diffrn_orient_matrix_UB_33      0.0039052313
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0793
_diffrn_reflns_av_unetI/netI     0.1464
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            61075
_diffrn_reflns_theta_full        28.5
_diffrn_reflns_theta_max         29.91
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    0.674
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.96131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
        (compiled Jun 10 2008,16:49:55)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2904
_exptl_crystal_size_max          0.514
_exptl_crystal_size_mid          0.1951
_exptl_crystal_size_min          0.039
_refine_diff_density_max         1.854
_refine_diff_density_min         -1.867
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     920
_refine_ls_number_reflns         17636
_refine_ls_number_restraints     319
_refine_ls_restrained_S_all      0.92
_refine_ls_R_factor_all          0.1328
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0550P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1289
_reflns_number_gt                9448
_reflns_number_total             17636
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om300366g_si_001.cif
_cod_data_source_block           br1449
_cod_original_cell_volume        6619.8(15)
_cod_original_sg_symbol_Hall     -P_2ybc
_cod_database_code               4078720