1,3-Dipolar Cycloadditions of Ruthenium(II) Azido Complexes with Alkynes and Nitriles
Sara Miguel-Fernández; Sara Martínez de Salinas; Josefina Díez; M. Pilar Gamasa; Elena Lastra; Inorganic Chemistry 52 (2013) 4293–4302; doi:10.1021/ic302264t

data_4334441
_publ_contact_author
;
     Josefina D\'iez
      Departamento de Qu\'imica Org\'anica e Inorg\'anica
      Facultad de Qu\'imica
      Universidad de Oviedo
      Avda. Juli\'an Claver\'ia, 8
      33071 Oviedo
      Spain
;
_publ_contact_author_email       jdv@uniovi.es
_publ_contact_author_fax         '0034 98 5103446'
_publ_contact_author_phone       '0034 98 5102960'
_publ_section_title
;
 1,3-Dipolar Cycloadditions of Ruthenium(II) Azido Complexes with Alkynes
 and Nitriles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4293
_journal_page_last               4302
_journal_paper_doi               10.1021/ic302264t
_journal_volume                  52
_journal_year                    2013
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C44 H44 N12 Na O11 P Ru S, 2(C3 H6 O)'
_chemical_formula_sum            'C50 H56 N12 Na O13 P Ru S'
_chemical_formula_weight         1220.16
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
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_audit_creation_method
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
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_cell_angle_alpha                97.852(2)
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_cell_formula_units_Z            2
_cell_length_a                   13.3422(3)
_cell_length_b                   14.4554(3)
_cell_length_c                   14.7576(3)
_cell_measurement_reflns_used    21801
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.6325
_cell_measurement_theta_min      3.0345
_cell_volume                     2776.14(10)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
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_computing_molecular_graphics    'PLATON (Spek, 2007)'
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_computing_structure_solution    'SIR-92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.2640
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device
; 
165 mm Onyx CCD detector in \k-geometry diffractometer
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_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nova (Cu) x-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
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_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29266
_diffrn_reflns_theta_full        74.80
_diffrn_reflns_theta_max         74.80
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    3.606
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82430
_exptl_absorpt_correction_type   multi-scan
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       prism
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.101
_refine_diff_density_min         -1.783
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         10991
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0732P)^2^+2.2361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1209
_reflns_number_gt                10153
_reflns_number_total             10991
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic302264t_si_001_2.cif
_cod_data_source_block           2b
_cod_database_code               4334441