Synthesis, Structure, and Substitution Mechanism of New Ru(II) Complexes Containing 1,4,7-Trithiacyclononane and 1,10-Phenanthroline Ligands
Xavier Sala; Isabel Romero; Montserrat Rodríguez; Antoni Llobet; Gabriel González; Manuel Martínez; Jordi Benet-Buchholz; Inorganic Chemistry 43 (2004) 5403–5409; doi:10.1021/ic0497533

data_4311858
_publ_contact_author
;
    Dr. Benet-Buchholz, Jordi
    Bayer Industry Services    
    Analytics X-Ray Laboratory
    Geb. Q18, Raum 490
    BAYER AG
    D-51368 Leverkusen, Germany
;
_publ_contact_author_email       jordi.benet-buchholz.jb@bayerindustry.de
_publ_contact_author_fax         '049 214 30 50677'
_publ_contact_author_phone       '049 214 30 65852'
_publ_section_title
;
 Synthesis, Structure, and Substitution Mechanism of New Ru(II) Complexes
 Containing 1,4,7-Trithiacyclononane and 1,10-Phenanthroline Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5403
_journal_page_last               5409
_journal_paper_doi               10.1021/ic0497533
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C80 H92 Cl8 N12 O32 Ru4 S12'
_chemical_formula_weight         2806.26
_chemical_name_common
;
 [Ru(1,10-phenantroline)(acetonitrile)(1,4,7-trithiacyclononane)](PF6)2
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.880(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3977(10)
_cell_length_b                   33.495(3)
_cell_length_c                   21.2512(16)
_cell_measurement_temperature    153(2)
_cell_volume                     10194.5(14)
_computing_cell_refinement       'Bruker SAINT program Vers. 5.0'
_computing_data_collection       'Bruker SMART CCD area detector system'
_computing_data_reduction        'Bruker SAINT program Vers. 5.0'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            'Smart 1000 CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'four-circle diffractometer Bruker P4'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans,
 in omega at 0.3 deg scan width, three runs with 98, 67 and 67 frames, phi=0 deg
 in phi at 0.3 deg scan width, two runs with 1207 frames, omega=-32 deg
;
_diffrn_measurement_specimen_support
'magnetic support whith 20 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1249
_diffrn_reflns_av_sigmaI/netI    0.1143
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            148242
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.55
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_current           240
_diffrn_source_power             48
_diffrn_source_size              '10 mm x 0.5 mm fine focus'
_diffrn_source_type              'MACScience Co. M18X-HF'
_exptl_absorpt_coefficient_mu    1.123
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.290966
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5664
_exptl_crystal_preparation
;
 Evaporation of water at room temperature
;
_exptl_crystal_size_max          1.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.431
_refine_diff_density_min         -2.134
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1496
_refine_ls_number_reflns         29676
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1405
_refine_ls_R_factor_gt           0.0762
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1023P)^2^+15.2289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1847
_refine_ls_wR_factor_ref         0.2124
_reflns_number_gt                16869
_reflns_number_total             29676
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0497533si20040225_023759_2.cif
_cod_data_source_block           xs02gigg
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

data name '_diffrn_measurement_specimen_suppport' was replaced with
'_diffrn_measurement_specimen_support' 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_cell_volume        10194.4(13)
_cod_database_code               4311858