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_4068567
_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            'C36 H20 B N6 O2 P2 Ru'
_chemical_formula_weight         742.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.7890(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.3520(2)
_cell_length_b                   22.5816(2)
_cell_length_c                   19.4934(2)
_cell_measurement_reflns_used    126314
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     8318.75(15)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            46548
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    0.488
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
; 
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995) 
;
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.332
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.265
_refine_ls_extinction_coef       0.0071(3)
_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   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1058
_refine_ls_number_reflns         14612
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.727
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0870P)^2^+4.5005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1337
_reflns_number_gt                12058
_reflns_number_total             14612
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800952t_si_001.cif
_cod_data_source_block           ic12928
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        8318.75(14)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4068567