Synthesis and Reactivity of Ruthenium Azido Complexes Containing a Hydridotris(pyrazolyl)borate Ligand and Dimerization of Terminal Alkynes in Organic and Aqueous Media
Chen, Chien-Kai; Tong, Hung-Chun; Chen Hsu, Chih-Yung; Lee, Chia-Yi; Fong, Yih Hsuan; Chuang, Yao-Shun; Lo, Yih-Hsing; Lin, Ying-Chih; Wang, Yu; Organometallics 28 (2009) 3358–; doi:10.1021/om800952t

data_4068569
_publ_section_title
;
 Synthesis and Reactivity of Ruthenium Azido Complexes Containing a
 Hydridotris(pyrazolyl)borate Ligand and Dimerization of Terminal Alkynes
 in Organic and Aqueous Media
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3358
_journal_paper_doi               10.1021/om800952t
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C32 H33 B I3 N8 P Ru'
_chemical_formula_weight         1053.21
_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
_cell_angle_alpha                92.503(2)
_cell_angle_beta                 104.852(2)
_cell_angle_gamma                108.897(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9119(2)
_cell_length_b                   13.0330(3)
_cell_length_c                   15.0779(3)
_cell_measurement_reflns_used    25419
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      30.1455
_cell_measurement_theta_min      2.9727
_cell_volume                     1942.04(8)
_computing_cell_refinement
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) 
(compiled Apr 21 2008,18:23:10) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_computing_data_collection
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) 
(compiled Apr 21 2008,18:23:10) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_computing_data_reduction
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) 
(compiled Apr 21 2008,18:23:10) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15905
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    2.862
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) 
(compiled Apr 21 2008,18:23:10) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.034
_refine_diff_density_min         -1.679
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.00026(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_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         8834
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.189
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+3.3355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0852
_reflns_number_gt                7303
_reflns_number_total             8834
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800952t_si_003.cif
_cod_data_source_block           ic13311
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1942.04(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4068569