Syntheses and Structures of New Diruthenatetraborane Complexes Exhibiting Novel Modes of Coordination for a B2H5Fragment: Phosphine-Complexed [(Cp*Ru)2(μ-H)(∥-μ-η4-B2H5)(PR3)] (PR3= PMe3, PMe2Ph) and Phosphido-Bridgednido-[(Cp*Ru)2(μ-PMe2)(⊥-μ-η4-B2H5)]1
Pangan, Lourdes N.; Kawano, Yasuro; Shimoi, Mamoru; Organometallics 19 (2000) 5575–; doi:10.1021/om000568g

data_4077599
_publ_section_title
;
 Syntheses and Structures of New Diruthenatetraborane Complexes Exhibiting
 Novel Modes of Coordination for a B2H5Fragment:&#x00A0;
 Phosphine-Complexed [(Cp*Ru)2(\m-H)(&#x2225;-\m-\h4-B2H5)(PR3)] (PR3=
 PMe3, PMe2Ph) and
 Phosphido-Bridgednido-[(Cp*Ru)2(\m-PMe2)(&#x22A5;-\m-\h4-B2H5)]1
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              5575
_journal_paper_doi               10.1021/om000568g
_journal_volume                  19
_journal_year                    2000
_chemical_compound_source        '[{(Cp*Ru)2(mu-H)(PMe2Ph)(B2H5)]'
_chemical_formula_analytical     C22H41B2PRu2
_chemical_formula_moiety         Cp*2Ru2(PMe2)(B2H5)
_chemical_formula_structural     '[(Cp*Ru)2(mu-PMe2)(B2H5)]'
_chemical_formula_sum            'C22 H41 B2 P Ru2'
_chemical_formula_weight         560.34
_chemical_name_systematic
; 
(mu-hapto4-pentahydrodiboranyl)(mu-dimethylphosphido)
bis(pentamethylcyclopentadienylruthenium)
;
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.265(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.854(2)
_cell_length_b                   15.238(3)
_cell_length_c                   17.855(3)
_cell_measurement_reflns_used    omega
_cell_measurement_temperature    268
_cell_measurement_theta_max      6
_cell_measurement_theta_min      3
_cell_volume                     5030.9(14)
_computing_cell_refinement       'UNICS-III (Sakurai,1976)'
_computing_data_collection       'COLLECT (RIGAKU)'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku AFC-5'
_diffrn_measurement_method       omega-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            5535
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.251
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_description       block
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.055
_refine_diff_density_min         -1.498
_refine_diff_density_rms         0.274
_refine_ls_extinction_coef       0.00147(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.237
_refine_ls_goodness_of_fit_obs   0.233
_refine_ls_hydrogen_treatment
'H1, H2, H11 and HBB were found by the difference Fourier synthesis and refined isotropically. H12 was found and fixed. Methyl hydrogen atoms were idealized.'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         5379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.237
_refine_ls_restrained_S_obs      0.233
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_obs          0.0518
_refine_ls_shift/esd_max         -3.971
_refine_ls_shift/esd_mean        0.863
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.4266P)^2^+1140.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1666
_refine_ls_wR_factor_obs         0.1628
_reflns_number_observed          5268
_reflns_number_total             5379
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om000568g.cif
_cod_data_source_block           '[(Cp*Ru)2(mu-Pme2)(mu-hapto4-B2H5)'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.4266P)^2^+1140.0000P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.4266P)^2^+1140.0000P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5030.8(14)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4077599