Synthesis and Dehydrative Condensation of Monomeric Hydroxoruthenium Complexes with Hydrotris(3,5-diisopropylpyrazolyl)borate Ligand, TpiPr2Ru(L2)-OH (L2= dppe, bipy)
Munetaka Akita; Yoshiaki Takahashi; Shiro Hikichi; Yoshihiko Moro-oka; Inorganic Chemistry 40 (2001) 169–172; doi:10.1021/ic000520v

data_4319115
_publ_section_title
;
 Synthesis and Dehydrative Condensation of Monomeric Hydroxoruthenium
 Complexes with Hydrotris(3,5-diisopropylpyrazolyl)borate Ligand,
 TpiPr2Ru(L2)-OH (L2= dppe, bipy)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              169
_journal_page_last               172
_journal_paper_doi               10.1021/ic000520v
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C68 H92 B Cl N6 O5 P2 Ru'
_chemical_formula_weight         1282.75
_chemical_name_common            'compound 4b'
_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
_cell_angle_alpha                91.69(4)
_cell_angle_beta                 115.78(3)
_cell_angle_gamma                100.60(4)
_cell_formula_units_Z            2
_cell_length_a                   16.230(5)
_cell_length_b                   16.205(4)
_cell_length_c                   15.454(9)
_cell_measurement_temperature    213(2)
_cell_volume                     3570(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6273
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.351
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_F_000             1356
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.473
_refine_ls_goodness_of_fit_obs   1.523
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         6273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.473
_refine_ls_restrained_S_obs      1.523
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_obs          0.0660
_refine_ls_shift/esd_max         0.179
_refine_ls_shift/esd_mean        0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2022
_refine_ls_wR_factor_obs         0.1935
_reflns_number_observed          5454
_reflns_number_total             6273
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000520v_2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] 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^)+(0.1000P)^2^+0.0000P] 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        3569.6(25)
_cod_database_code               4319115