Synthesis of nido-[1-OMe-2,3-(Cp*Ru)2{μ-P(OMe)2}B3H5]: Methoxy Transfer from Phosphorus to Boron and Cluster Core Rearrangement
Lourdes N. Pangan; Yasuro Kawano; Mamoru Shimoi; Inorganic Chemistry 40 (2001) 1985–1986; doi:10.1021/ic001334s

data_4319572
_publ_section_title
;
 Synthesis of nido-[1-OMe-2,3-(Cp*Ru)2{\m-P(OMe)2}B3H5]: Methoxy Transfer
 from Phosphorus to Boron and Cluster Core Rearrangement
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1985
_journal_page_last               1986
_journal_paper_doi               10.1021/ic001334s
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        '[{Cp*Ru(mu-H)}2B3H7], P(OMe)3 '
_chemical_formula_analytical     C23H44B3O3PRu2
_chemical_formula_moiety         Cp*2Ru2(P(OMe)2)(BOMe)(B2H5)
_chemical_formula_structural     '[(Cp*Ru)2(mu-P(OMe)2)(BOMe)(B2H5)]'
_chemical_formula_sum            'C23 H44 B3 O3 P Ru2'
_chemical_formula_weight         634.18
_chemical_name_systematic
; 
(mu-hapto4-methoxyboranyl)(mu-hapto4-pentahydrodiboranyl)(mu-dimethoxyphosphido)
bis(pentamethylcyclopentadienylruthenium) ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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                 123.255(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.212(3)
_cell_length_b                   15.0577(10)
_cell_length_c                   15.700(2)
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      8.3
_cell_volume                     5577.3(12)
_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      298(2)
_diffrn_measurement_device       'RIGAKU AFC5'
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3664
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        0.02
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.145
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_description       plate
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.00216(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   0.271
_refine_ls_goodness_of_fit_obs   0.268
_refine_ls_hydrogen_treatment
;
H(1)-H(5) were found by the difference Fourier
synthesis and refined isotropically.  Methyl hydrogen atoms were idealized.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         3456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.271
_refine_ls_restrained_S_obs      0.268
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_obs          0.0335
_refine_ls_shift/esd_max         -0.070
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2633P)^2^+527.4892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1048
_refine_ls_wR_factor_obs         0.1028
_reflns_number_observed          3412
_reflns_number_total             3456
_reflns_observed_criterion       >3sigma(I)
_cod_data_source_file            ic001334s.cif
_cod_data_source_block
nido-[1-(OMe)-2,3-(Cp*Ru)2-2,3-(mu-P(OMe)2)(B3H5)]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.2633P)^2^+527.4892P] 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^)+(0.2633P)^2^+527.4892P] 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        5577.1(10)
_cod_database_code               4319572