Controlling Substitution Chemistry in Ruthenium(II) Systems. Synthesis of Heteroleptic Complexes Incorporating the [Ru([9]aneS3)]2+ Metal Center
Sue Roche; Harry Adams; Sharon E. Spey; James A. Thomas; Inorganic Chemistry 39 (2000) 2385–2390; doi:10.1021/ic991336g

data_4320982
_publ_section_title
;
 Controlling Substitution Chemistry in Ruthenium(II) Systems. Synthesis of
 Heteroleptic Complexes Incorporating the [Ru([9]aneS3)]2+ Metal Center
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2385
_journal_page_last               2390
_journal_paper_doi               10.1021/ic991336g
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C22 H30 F12 N4 O2 P2 Ru S3'
_chemical_formula_weight         869.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 114.836(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.267(5)
_cell_length_b                   11.5457(18)
_cell_length_c                   26.192(5)
_cell_measurement_temperature    150(2)
_cell_volume                     6385(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.548
_diffrn_measured_fraction_theta_max 0.548
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_number            6223
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.888
_exptl_absorpt_correction_T_max  0.9164
_exptl_absorpt_correction_T_min  0.7765
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.809
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3488
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         4350
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.1013
_reflns_number_gt                3398
_reflns_number_total             4350
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic991336g_1.cif
_cod_data_source_block           iaj4
_cod_original_sg_symbol_H-M      'C 1 c 1'
_cod_database_code               4320982