Strain-induced substitutional lability in a Ru(II) complex of a hypodentate polypyridine ligand.
Akermark, Björn; Bjernemose, Jens; Börje, Anna; Chmielewski, Piotr J.; Paulsen, Hauke; Simonsen, Ole; Stein, Paul C.; Toftlund, Hans; Wolny, Juliusz A.; Dalton transactions (Cambridge, England : 2003)  (2004) 1215–1220; doi:10.1039/b316093a

data_7013890
_publ_section_title
;
 Strain-induced substitutional lability in a Ru(II) complex of a
 hypodentate polypyridine ligand.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1215
_journal_page_last               1220
_journal_paper_doi               10.1039/b316093a
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C33 H35 F6 N7 O8 Ru S2'
_chemical_formula_sum            'C33 H35 F6 N7 O8 Ru S2'
_chemical_formula_weight         936.87
_chemical_name_common            'Ru Gorilla'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2004-02-04T17:04:25-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 110.3320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9820(10)
_cell_length_b                   9.961(3)
_cell_length_c                   22.6050(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      41.47
_cell_measurement_theta_min      37.81
_cell_measurement_wavelength     1.54178
_cell_volume                     3796.7(12)
_computing_cell_refinement       'Enraf-Nonius CAD-4F Software'
_computing_data_collection       'Enraf-Nonius CAD-4F Software'
_computing_data_reduction
;
Norrestam & Nielsen (1982) and Xtal3.2 ADDREF SORTRF (Hall, Flack &
Stewart, 1992)
;
_computing_molecular_graphics    ' Xtal3.2 ORTEP'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device
;
Enraf-Nonius CAD-4F diffractometer
;
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       \w/2\Q
_diffrn_orient_matrix_type
;
x-axis points to radiation source
the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.056777
_diffrn_orient_matrix_UB_12      0.000691
_diffrn_orient_matrix_UB_13      0.028375
_diffrn_orient_matrix_UB_21      -0.016961
_diffrn_orient_matrix_UB_22      -0.001399
_diffrn_orient_matrix_UB_23      0.037678
_diffrn_orient_matrix_UB_31      0.000622
_diffrn_orient_matrix_UB_32      -0.100267
_diffrn_orient_matrix_UB_33      -0.000326
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            6672
_diffrn_reflns_theta_full        65
_diffrn_reflns_theta_max         65
_diffrn_reflns_theta_min         2.72
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enraf Nonius FR590'
_diffrn_standards_decay_%        9
_diffrn_standards_interval_count 30
_diffrn_standards_interval_time  90
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    5.169
_exptl_absorpt_correction_T_max  0.553
_exptl_absorpt_correction_T_min  0.326
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
a grid of  8 x 14 x  8 =   896 sampling points was used
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_meas      1.64
_exptl_crystal_density_method
;
Flotation in mixture of CCl~4~ and CH~2~BrCl.
;
_exptl_crystal_description       prism
_exptl_crystal_F_000             1904
_exptl_crystal_preparation
;
A solution in acetone was layered with ligroin and left for several months.
;
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.25
_refine_diff_density_min         -1.58
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         6450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0976P)^2^+7.5145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1506
_refine_ls_wR_factor_ref         0.1552
_reflns_number_gt                5894
_reflns_number_total             6450
_reflns_threshold_expression     'I > 2.5*sigma(I)'
_cod_data_source_file            b316093a.txt
_cod_data_source_block           gorila
_cod_original_sg_symbol_Hall     -P_2yn
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7013890
_diffrn_standards_decay_corr_max 1.119
_diffrn_standards_decay_corr_min 0.957