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_7038247
_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_absolute_configuration ad
_chemical_formula_moiety
;
C88 H96 Cl4 N8 O8 Ru4, 4(C F3 O3 S),C H Cl3, 2(H2 O)
;
_chemical_formula_sum            'C93 H101 Cl7 F12 N8 O22 Ru4 S4'
_chemical_formula_weight         2691.49
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-04-04T12:54:55-00:00
_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                90
_cell_angle_beta                 116.629(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   32.1763(17)
_cell_length_b                   11.3815(4)
_cell_length_c                   15.8038(8)
_cell_measurement_reflns_used    6822
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1592
_cell_measurement_theta_min      3.5735
_cell_volume                     5173.7(5)
_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
;
        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 10.4738
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device_type  'Oxford Diffraction Gemini diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0188680111
_diffrn_orient_matrix_UB_12      0.0145127026
_diffrn_orient_matrix_UB_13      0.0097954701
_diffrn_orient_matrix_UB_21      -0.0157261647
_diffrn_orient_matrix_UB_22      -0.0258902684
_diffrn_orient_matrix_UB_23      -0.0434850433
_diffrn_orient_matrix_UB_31      0.0024440114
_diffrn_orient_matrix_UB_32      -0.0548093593
_diffrn_orient_matrix_UB_33      0.0231690832
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0984
_diffrn_reflns_av_unetI/netI     0.2057
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27740
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.58
_exptl_absorpt_coefficient_mu    0.93
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.904
_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            light_brown
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2716
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.487
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.139
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.07(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         11356
_refine_ls_number_restraints     412
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1317
_refine_ls_R_factor_gt           0.0738
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0604P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1486
_reflns_number_gt                6488
_reflns_number_total             11356
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c6dt00168h2.cif
_cod_data_source_block           cpgp4
_cod_depositor_comments
'Adding full bibliography for 7038245--7038247.cif.'
_cod_original_cell_volume        5173.7(4)
_cod_original_sg_symbol_Hall     'c 2y'
_cod_database_code               7038247