Homoannular Double Friedel‒Crafts Acylation of Phosphametallocenes
Ogasawara, Masamichi; Ogura, Morihiko; Sakamoto, Takeshi; Watanabe, Susumu; Arae, Sachie; Nakajima, Kiyohiko; Takahashi, Tamotsu; Organometallics 30 (2011) 5045–; doi:10.1021/om200678q

data_4065277
_publ_section_title
;
 Homoannular Double Friedel--Crafts Acylation of Phosphametallocenes
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              5045
_journal_paper_doi               10.1021/om200678q
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C24 H36 O2 P2 Ru'
_chemical_formula_sum            'C24 H36 O2 P2 Ru'
_chemical_formula_weight         519.56
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 98.782(14)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.826(5)
_cell_length_b                   9.947(3)
_cell_length_c                   21.451(7)
_cell_measurement_reflns_used    19420
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.13
_cell_volume                     2493.8(15)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23626
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.774
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1080.00
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.060
_refine_diff_density_max         4.080
_refine_diff_density_min         -1.000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5703
_refine_ls_R_factor_gt           0.0665
_refine_ls_shift/su_max          0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0070Fo^2^ + 1.0000\s(Fo^2^) + 0.5500]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2491
_reflns_number_gt                4541
_reflns_number_total             5703
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om200678q_si_002.cif
_cod_data_source_block           complex-4
_cod_depositor_comments
'Adding full bibliography for 4065277--4065278.cif.'
_cod_original_cell_volume        2493.7(14)
_cod_database_code               4065277