Self-assembly of arene ruthenium acylpyrazolone fragments to tetranuclear metallacycles. Molecular structures and solid-state (15)N CPMAS NMR correlations.
Pettinari, Riccardo; Marchetti, Fabio; Pettinari, Claudio; Condello, Francesca; Skelton, Brian W.; White, Allan H.; Chierotti, Michele R.; Gobetto, Roberto; Dalton transactions (Cambridge, England : 2003) 45 (2016) 3974–3982; doi:10.1039/c6dt00168h

data_7038246
_publ_section_title
;
 Self-assembly of arene ruthenium acylpyrazolone fragments to tetranuclear
 metallacycles. Molecular structures and solid-state (15)N CPMAS NMR
 correlations.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3974
_journal_page_last               3982
_journal_paper_doi               10.1039/c6dt00168h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C22 H24 Cl2 N2 O2 Ru'
_chemical_formula_sum            'C22 H24 Cl2 N2 O2 Ru'
_chemical_formula_weight         520.4
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_date             2012-02-07T12:39:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2013-06-17 deposited with the CCDC.
2016-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                112.841(4)
_cell_angle_beta                 95.967(3)
_cell_angle_gamma                103.150(3)
_cell_formula_units_Z            2
_cell_length_a                   7.5449(3)
_cell_length_b                   12.0143(4)
_cell_length_c                   12.9409(5)
_cell_measurement_reflns_used    15468
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.2436
_cell_measurement_theta_min      2.8322
_cell_volume                     1028.27(8)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
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        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_molecular_graphics    'OrtepII (Johnson, C. K. (1976)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0450581
_diffrn_orient_matrix_UB_12      0.0395298
_diffrn_orient_matrix_UB_13      -0.0241835
_diffrn_orient_matrix_UB_21      0.0878092
_diffrn_orient_matrix_UB_22      0.0047941
_diffrn_orient_matrix_UB_23      0.0297705
_diffrn_orient_matrix_UB_31      0.0050044
_diffrn_orient_matrix_UB_32      -0.0538648
_diffrn_orient_matrix_UB_33      -0.0473044
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27880
_diffrn_reflns_theta_full        33
_diffrn_reflns_theta_max         34.32
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    1.044
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
     CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
               model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.068
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         8240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+0.5183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.069
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                7376
_reflns_number_total             8240
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c6dt00168h2.cif
_cod_data_source_block           cpgp3c
_cod_depositor_comments
'Adding full bibliography for 7038245--7038247.cif.'
_cod_original_cell_volume        1028.27(7)
_cod_original_sg_symbol_Hall     '-p 1'
_cod_database_code               7038246