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_7001121
_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         'C240 H186 F18 Fe6 N12 O33 P12 Pd6 S6'
_chemical_formula_sum            'C120 H93 F9 Fe3 N6 O15 P6 Pd3 S3'
_chemical_formula_weight         2798.75
_chemical_name_systematic
;
?
;
_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                 94.51(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.528(4)
_cell_length_b                   28.904(6)
_cell_length_c                   53.724(11)
_cell_measurement_temperature    150(2)
_cell_volume                     31778(11)
_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 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_radiation_source         'synchrotron x-ray'
_diffrn_radiation_wavelength     0.79999
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19454
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    6.273
_exptl_absorpt_correction_T_max  0.8818
_exptl_absorpt_correction_T_min  0.8447
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS: Blessing, R. (1995), Acta Cryst., A51, 33'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             11376
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_platon_squeeze_details
;
SQUEEZE (PLATON, A.Spek) was used to treat diffuse solvent
contributions. Total electron count found = 2333/unit cell.
Calculated for 18 nitromethane (the reaction solvent)
= 2304/unit cell. The intensive properties (density, F(000), etc.)
reflect these contributions
;
_refine_diff_density_max         4.930
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.00033(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2967
_refine_ls_number_reflns         19454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0977
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1956P)^2^+182.6095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2742
_refine_ls_wR_factor_ref         0.2787
_reflns_number_gt                18079
_reflns_number_total             19454
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b900118b.txt
_cod_data_source_block           1a
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7001121