(15)N NMR spectroscopy unambiguously establishes the coordination mode of the diimine linker 2-(2'-pyridyl)pyrimidine-4-carboxylic acid (cppH) in Ru(ii) complexes.
Battistin, Federica; Balducci, Gabriele; Demitri, Nicola; Iengo, Elisabetta; Milani, Barbara; Alessio, Enzo; Dalton transactions (Cambridge, England : 2003) 44 (2015) 15671–15682; doi:10.1039/c5dt02361k

data_7036121
_publ_section_title
;
 (15)N NMR spectroscopy unambiguously establishes the coordination mode of
 the diimine linker 2-(2'-pyridyl)pyrimidine-4-carboxylic acid (cppH) in
 Ru(ii) complexes.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15671
_journal_page_last               15682
_journal_paper_doi               10.1039/c5dt02361k
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'0.45 (C12 H7 Cl2 N3 O4 Ru), 0.45 (C H4 O), 0.55 (C13 H9 Cl2 N3 O4 Ru)'
_chemical_formula_sum            'C13 H9.9 Cl2 N3 O4.45 Ru'
_chemical_formula_weight         451.31
_chemical_name_systematic        ' trans,cis-[RuCl2(CO)2(cppCH3-Np)] '
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-07-09 deposited with the CCDC.
2015-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.35(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.5640(13)
_cell_length_b                   21.643(4)
_cell_length_c                   11.766(2)
_cell_measurement_reflns_used    4249
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.085
_cell_measurement_theta_min      1.853
_cell_volume                     1626.4(6)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        'XDS - CCP4'
_computing_molecular_graphics    'Ortep3 for Windows'
_computing_publication_material  enCIFer/publCIF
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Sir2014 (Burla, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.989
_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  0.0261
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28444
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         29.085
_diffrn_reflns_theta_min         1.853
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.247
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_description       Prism
_exptl_crystal_F_000             890
_exptl_crystal_recrystallization_method
'spontaneous precipitation from the reaction mixture; solvent: methanol'
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.869
_refine_diff_density_min         -2.261
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.0033(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4507
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0155P)^2^+6.7432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4264
_reflns_number_total             4507
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02361k2.cif
_cod_data_source_block           5Me
_cod_depositor_comments
'Adding full bibliography for 7036121--7036125.cif.'
_cod_original_formula_sum        'C13 H9.90 Cl2 N3 O4.45 Ru'
_cod_database_code               7036121
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.940
_shelx_estimated_absorpt_t_max   0.940
_shelx_res_checksum              69809