γ-Substituted Vinylidene, Chroman-2-ylidene, and Hexahydrochromen-2-ylidene from Ruthenium Allenylidene/Alkenylcarbyne Complexes
Bustelo, Emilio; Jiménez-Tenorio, Manuel; Puerta, M. Carmen; Valerga, Pedro; Organometallics 26 (2007) 4300–; doi:10.1021/om700431n

data_4082265
_publ_section_title
;
 \g-Substituted Vinylidene, Chroman-2-ylidene, and
 Hexahydrochromen-2-ylidene from Ruthenium Allenylidene/Alkenylcarbyne
 Complexes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4300
_journal_paper_doi               10.1021/om700431n
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C39 H57 F O2 P2 Ru, B F4'
_chemical_formula_sum            'C39 H57 B F5 O2 P2 Ru'
_chemical_formula_weight         826.67
_chemical_name_common
;
[(\h^5^-C~5~Me~5~)Ru{=C(-OC~6~H~3~OH-CH(C~6~H~4~F)CH~2~-)}(dippe)][BF~4~]
;
_chemical_name_systematic
;       
1,2-bis(diisopropylphosphine)ethane-7-hydroxy-4-p-fluorphenyl-chroman-2-
ylidene-\h^5^-pentamethylcyclopentadienyl-ruthenium (II) tetrafluorborate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.24(3)
_cell_angle_beta                 92.81(3)
_cell_angle_gamma                105.96(3)
_cell_formula_units_Z            2
_cell_length_a                   10.680(2)
_cell_length_b                   10.981(2)
_cell_length_c                   17.341(4)
_cell_measurement_reflns_used    7246
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.041
_cell_measurement_theta_min      2.356
_cell_volume                     1947.8(7)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'ORTEP-3 vers. 1.08 (Faruggia, 2005)'
_computing_publication_material  'SHELXTL (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2001)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '1700 omega scan frames, 0.3 deg, 10 sec'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13188
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.18
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Bruker SMART APEX'
_diffrn_standards_decay_%        -0.0113
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             862
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.302
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         6771
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0737
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+14.0034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.1510
_reflns_number_gt                6408
_reflns_number_total             6771
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700431nsup1.cif
_cod_data_source_block           pv0619
_cod_original_cell_volume        1947.9(7)
_cod_database_code               4082265