An irresolute linker: separation, and structural and spectroscopic characterization of the two linkage isomers of a Ru(ii)-(2-(2'-pyridyl)pyrimidine-4-carboxylic acid) complex.
Iengo, E.; Demitri, N.; Balducci, G.; Alessio, E.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 12160–12163; doi:10.1039/c4dt01282h

data_7031930
_publ_section_title
;
 An irresolute linker: separation, and structural and spectroscopic
 characterization of the two linkage isomers of a
 Ru(ii)-(2-(2'-pyridyl)pyrimidine-4-carboxylic acid) complex.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12160
_journal_page_last               12163
_journal_paper_doi               10.1039/c4dt01282h
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety
;
 C22 H31.5 N6 O2 P Ru S3, Cl2.5, 2.75(H2 O)
;
_chemical_formula_sum            'C22 H35.5 Cl2.5 N6 O4.75 P Ru S3'
_chemical_formula_weight         776.91
_chemical_name_common
;
[Ru([9]aneS~3~)(cppH)(PTA)][Cl~2~]
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                112.547(5)
_cell_angle_beta                 105.610(4)
_cell_angle_gamma                96.533(4)
_cell_formula_units_Z            2
_cell_length_a                   10.8640(5)
_cell_length_b                   12.5130(3)
_cell_length_c                   15.2790(8)
_cell_measurement_reflns_used    25093
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.943
_cell_measurement_theta_min      1.512
_cell_volume                     1791.74(17)
_computing_cell_refinement       XDS
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        XDS
_computing_molecular_graphics    'Ortep3 for Windows - PyMol'
_computing_publication_material  'enCIFer - publCIF'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    Sir2011
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type
;
'Huber 4-circles Kappa Goniometer, Pilatus 2M detector'
;
_diffrn_measurement_method       'Rotating crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            45570
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         25.943
_diffrn_reflns_theta_min         1.512
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_description       'Hexagonal prism'
_exptl_crystal_F_000             794
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.163
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       0.062(2)
_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   1.239
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         7033
_refine_ls_number_restraints     230
_refine_ls_restrained_S_all      1.219
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+2.2649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1255
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6934
_reflns_number_total             7033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_duplicate_entry             7031616
_cod_data_source_file            c4dt01282h2.cif
_cod_data_source_block           PDM51Prism2Np
_cod_original_cell_volume        1791.73(15)
_cod_original_formula_sum        'C22 H35.50 Cl2.50 N6 O4.75 P Ru S3'
_cod_database_code               7031930
_shelx_estimated_absorpt_t_min   0.803
_shelx_estimated_absorpt_t_max   0.894
_shelxl_version_number           2013-4