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_4334238
_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_formula_moiety         'C34 H25 Cl2 N7 O8 Ru'
_chemical_formula_sum            'C34 H25 Cl2 N7 O8 Ru'
_chemical_formula_weight         831.58
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 102.191(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.0382(16)
_cell_length_b                   9.5447(5)
_cell_length_c                   24.5300(15)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.44
_cell_measurement_theta_min      1.70
_cell_volume                     6645.4(7)
_computing_cell_refinement       'SAINT Ver. 7.24A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 Ver. 2.1-4 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT Ver. 7.24A'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXTL, OLEX2 (Dolomanov et al., 2009)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.60\% \w and 0.6\% \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6121
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_T_max  0.9335
_exptl_absorpt_correction_T_min  0.8788
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2007)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       needle
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.815
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         6128
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0446P)^2^+20.6235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0943
_reflns_number_gt                5594
_reflns_number_total             6121
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic302827s_si_001_2.cif
_cod_data_source_block           stahl102
_cod_original_cell_volume        6645.4(6)
_cod_original_sg_symbol_Hall     '-C 2yc      '
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4334238