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_4334239
_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         'C27 H20 Cl2 N8 O8 Ru'
_chemical_formula_sum            'C27 H20 Cl2 N8 O8 Ru'
_chemical_formula_weight         756.48
_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                85.888(9)
_cell_angle_beta                 77.750(6)
_cell_angle_gamma                77.536(8)
_cell_formula_units_Z            2
_cell_length_a                   9.6495(13)
_cell_length_b                   12.3186(19)
_cell_length_c                   15.199(3)
_cell_measurement_reflns_used    8652
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.5070
_cell_measurement_theta_min      2.9764
_cell_volume                     1723.3(5)
_computing_cell_refinement       'SAINT Ver. 7.68A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 Ver. 2010.11-3 (Bruker-AXS, 2010)'
_computing_data_reduction        'SAINT Ver. 7.68A'
_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 0.958
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.60\% \w and 0.6\% \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    0.0333
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6252
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         72.17
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    5.598
_exptl_absorpt_correction_T_max  0.7158
_exptl_absorpt_correction_T_min  0.4240
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2011)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;

There were three partially occupied solvent 
molecules present in the asymmetric unit. 
 A significant amount of time was invested 
in identifying and refining the disordered 
molecules.  Bond length restraints were 
applied to model the molecules but the 
resulting isotropic displacement coefficients
 suggested the molecules were mobile.  In addition,
 the refinement was computationally unstable.  Option 
SQUEEZE of program PLATON  was used 
to correct the diffraction data for
 diffuse scattering effects and to identify
 the solvate molecule.  PLATON calculated 
the upper limit of volume that can be occupied
 by the solvent to be 280 \%A3, or 16% of the unit
 cell volume.  The program calculated 86 electrons 
in the unit cell for the diffuse species.  Several 
solvents were used in the crystallization procedure,
 thus no meaningful solvent identification can be made. 
Note that all derived results in the following tables 
are based on the known contents.  No data are given for 
the diffusely scattering species.  
;
_refine_diff_density_max         1.101
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         6252
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0740P)^2^+1.4589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1183
_reflns_number_gt                5530
_reflns_number_total             6252
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic302827s_si_001_3.cif
_cod_data_source_block           stahl124
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_sg_symbol_Hall     '-P 1        '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4334239