Modular Synthesis of Alkyne-Substituted Ruthenium Polypyridyl Complexes Suitable for "Click" Coupling
James B. Gerken; Matthew L. Rigsby; Rose E. Ruther; Riviam J. Pérez-Rodríguez; Ilia A. Guzei; Robert J. Hamers; Shannon S. Stahl; Inorganic Chemistry 52 (2013) 2796–2798; doi:10.1021/ic302827s

data_4334237
_publ_contact_author_address
;
Department of Chemistry
University of Wisconsin-Madison
1101 University Ave
Madison, WI  53706
USA
;
_publ_contact_author_email       iguzei@chem.wisc.edu
_publ_contact_author_fax         608-262-0381
_publ_contact_author_name
;
Guzei, Ilia A. 
;
_publ_contact_author_phone       608-263-4694
_publ_section_title
;
 Modular Synthesis of Alkyne-Substituted Ruthenium Polypyridyl Complexes
 Suitable for "Click" Coupling
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2796
_journal_page_last               2798
_journal_paper_doi               10.1021/ic302827s
_journal_volume                  52
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C37.83 H44.75 Br0.08 Cl2 N8.92 O9 Ru Si'
_chemical_formula_sum            'C37.83 H44.75 Br0.08 Cl2 N8.92 O9 Ru Si'
_chemical_formula_weight         975.16
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                86.256(3)
_cell_angle_beta                 83.703(3)
_cell_angle_gamma                84.879(3)
_cell_formula_units_Z            2
_cell_length_a                   8.4875(3)
_cell_length_b                   9.5962(4)
_cell_length_c                   26.8766(11)
_cell_measurement_reflns_used    2589
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.57
_cell_measurement_theta_min      3.31
_cell_volume                     2163.74(15)
_computing_cell_refinement       'SAINT Ver. 7.24A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 Ver. 2.1-4 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT Ver. 7.24A'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.50\% \w and 0.5 \% \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Cu-K\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0588
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7730
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         69.57
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    4.959
_exptl_absorpt_correction_T_max  0.8655
_exptl_absorpt_correction_T_min  0.5042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2007)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       needle
_exptl_crystal_F_000             1002
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         7738
_refine_ls_number_restraints     692
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0730P)^2^+3.8413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1518
_refine_ls_wR_factor_ref         0.1600
_reflns_number_gt                6540
_reflns_number_total             7730
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic302827s_si_001_1.cif
_cod_data_source_block           stahl76
_cod_original_sg_symbol_Hall     '-P 1         '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4334237