Preparation of pyranylidene complexes of ruthenium.
Albertin, Gabriele; Antoniutti, Stefano; Bortoluzzi, Marco; Botter, Alessandra; Castro, Jesús; Dalton transactions (Cambridge, England : 2003) 44 (2015) 7411–7418; doi:10.1039/c5dt00418g

data_7034593
_publ_section_title
;
 Preparation of pyranylidene complexes of ruthenium.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7411
_journal_page_last               7418
_journal_paper_doi               10.1039/c5dt00418g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C34 H37 O7 P2 Ru, C24 H20 B'
_chemical_formula_sum            'C58 H57 B O7 P2 Ru'
_chemical_formula_weight         1039.86
_chemical_name_systematic        'Ruthenium pyranylidene'
_space_group_IT_number           2
_symmetry_cell_setting           Triclinic'
_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
_audit_update_record
;
2015-01-28 deposited with the CCDC.
2015-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                81.410(4)
_cell_angle_beta                 87.130(4)
_cell_angle_gamma                87.354(3)
_cell_formula_units_Z            2
_cell_length_a                   10.9219(8)
_cell_length_b                   14.7181(11)
_cell_length_c                   16.2149(12)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      67.31
_cell_measurement_theta_min      2.76
_cell_volume                     2572.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker CCD Smart 6000'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Incoatec Quazar MX multilayer optics'
_diffrn_radiation_source         'Incoatec I\muS microsource'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            62732
_diffrn_reflns_theta_full        67.88
_diffrn_reflns_theta_max         67.88
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    3.474
_exptl_absorpt_correction_T_max  0.6970
_exptl_absorpt_correction_T_min  0.5239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1080
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ethanol/dichloromethane'
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.051
_refine_diff_density_max         1.293
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         9003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0938P)^2^+0.6069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1399
_reflns_number_gt                7766
_reflns_number_total             9003
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00418g3.cif
_cod_data_source_block           pat_LZ43
_cod_depositor_comments          'Adding full bibliography for 7034593.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7034593