Synthesis and characterisation of heterometallic molecular triangles using ambidentate linker: self-selection of a single linkage isomer
Bar, Arun Kumar; Chakrabarty, Rajesh; Chi, Ki-Whan; Batten, Stuart R.; Mukherjee, Partha Sarathi; Dalton Transactions  (2009) 3222–3229; doi:10.1039/b900118b

data_7001122
_publ_section_title
;
 Synthesis and characterisation of heterometallic molecular triangles
 using ambidentate linker: self-selection of a single linkage isomer
;
_journal_issue                   17
_journal_name_full               'Dalton Transactions'
_journal_page_first              3222
_journal_page_last               3229
_journal_paper_doi               10.1039/b900118b
_journal_year                    2009
_chemical_formula_moiety
'C117 H94 Fe3 N6 O6 P6 Pt3, 3(C F3 O3 S), 5(C H3 N O2)'
_chemical_formula_sum            'C125 H108 F9 Fe3 N11 O25 P6 Pt3 S3'
_chemical_formula_weight         3370.02
_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                84.91(3)
_cell_angle_beta                 75.09(3)
_cell_angle_gamma                60.48(3)
_cell_formula_units_Z            2
_cell_length_a                   18.580(4)
_cell_length_b                   18.840(4)
_cell_length_c                   22.725(5)
_cell_measurement_temperature    293(2)
_cell_volume                     6682(3)
_computing_molecular_graphics    'ORTEP-3 for Windows(Farrugia, 1997)'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_diffrn_radiation_source         'synchrotron x-ray'
_diffrn_radiation_wavelength     0.69998
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            38395
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    3.635
_exptl_absorpt_correction_T_max  0.544
_exptl_absorpt_correction_T_min  0.463
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS: Blessing, R. (1995), Acta Cryst., A51, 33'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             3012
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
SQUEEZE (PLATON, A.Spek) was used to treat diffuse solvent
contributions. Total electron count found = 302/unit cell.
Calculated for 5 nitromethane (the reaction solvent)
= 320/unit cell. The intensive properties (density, F(000), etc.)
reflect these contributions
;
_refine_diff_density_max         1.491
_refine_diff_density_min         -2.256
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1486
_refine_ls_number_reflns         25610
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0683P)^2^+11.9923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.0936
_reflns_number_gt                24776
_reflns_number_total             25610
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b900118b.txt
_cod_data_source_block           1b
_cod_original_cell_volume        6682(2)
_cod_database_code               7001122