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_4078721
_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_absolute_configuration ad
_chemical_formula_moiety         'C69 H51 N5 P2 Ru2, 3(C6 H6)'
_chemical_formula_sum            'C87 H69 N5 P2 Ru2'
_chemical_formula_weight         1448.55
_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_creation_date             2012-04-13T15:54:24-00:00
_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                   14.029(2)
_cell_length_b                   20.6924(17)
_cell_length_c                   24.0829(19)
_cell_measurement_reflns_used    8544
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2819
_cell_measurement_theta_min      2.5309
_cell_volume                     6991.1(13)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0028613929
_diffrn_orient_matrix_UB_12      -0.0215746454
_diffrn_orient_matrix_UB_13      0.0228958511
_diffrn_orient_matrix_UB_21      0.0140754874
_diffrn_orient_matrix_UB_22      -0.0260064726
_diffrn_orient_matrix_UB_23      -0.017393575
_diffrn_orient_matrix_UB_31      0.048559455
_diffrn_orient_matrix_UB_32      0.0062412584
_diffrn_orient_matrix_UB_33      0.0063977484
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_unetI/netI     0.1459
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            49696
_diffrn_reflns_theta_full        27.25
_diffrn_reflns_theta_max         27.25
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    0.529
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.9703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
        (compiled Feb 27 2009,15:38:38)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.451
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.027(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.789
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     949
_refine_ls_number_reflns         15275
_refine_ls_number_restraints     851
_refine_ls_restrained_S_all      0.804
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0131P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0535
_refine_ls_wR_factor_ref         0.0574
_reflns_number_gt                10383
_reflns_number_total             15275
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om300366g_si_002.cif
_cod_data_source_block           br1450
_cod_original_cell_volume        6991.0(14)
_cod_database_code               4078721