Stepwise synthetic strategy for the preparation of trinuclear complexes of bis(terpyridyl) bridging ligands containing aza-crown macrocyclic spacer groups
Bushell, Karen L.; Couchman, Samantha M.; Jeffery, John C.; Rees, Leigh H.; Ward, Michael D.; Journal of the Chemical Society, Dalton Transactions  (1998) 3397–; doi:10.1039/a805059g

data_7026988
_publ_section_title
;
 Stepwise synthetic strategy for the preparation of trinuclear complexes
 of bis(terpyridyl) bridging ligands containing aza-crown macrocyclic
 spacer groups
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3397
_journal_paper_doi               10.1039/a805059g
_journal_year                    1998
_chemical_formula_sum            'C57 H71 Cl2 F6 N10 O14 P Ru'
_chemical_formula_weight         1437.18
_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_method           SHELXL-97
_cell_angle_alpha                76.16(3)
_cell_angle_beta                 87.85(2)
_cell_angle_gamma                81.87(2)
_cell_formula_units_Z            2
_cell_length_a                   8.357(4)
_cell_length_b                   17.697(5)
_cell_length_c                   22.442(8)
_cell_measurement_temperature    173(2)
_cell_volume                     3190(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0893
_diffrn_reflns_av_sigmaI/netI    0.1011
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16835
_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1484
_refine_diff_density_max         2.156
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     840
_refine_ls_number_reflns         5931
_refine_ls_number_restraints     270
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1476
_refine_ls_R_factor_gt           0.1044
_refine_ls_shift/su_max          1.458
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2005P)^2^+22.0741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2820
_refine_ls_wR_factor_ref         0.3185
_reflns_number_gt                3891
_reflns_number_total             5931
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            805059gsup1.cif
_cod_data_source_block           structure1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7026988