Syntheses of novel di- and trinucleating ligands having a triethylbenzene core with N,N-bidentate tethers: their complexation toward Pd and Rh organometallic fragments
Higashihara, Gou; Inagaki, Akiko; Akita, Munetaka; Dalton Transactions  (2008) 1888–1898; doi:10.1039/b713503c

data_7003183
_publ_section_title
;
 Syntheses of novel di- and trinucleating ligands having a
 triethylbenzene core with N,N-bidentate tethers: their complexation
 toward Pd and Rh organometallic fragments
;
_journal_issue                   14
_journal_name_full               'Dalton Transactions'
_journal_page_first              1888
_journal_page_last               1898
_journal_paper_doi               10.1039/b713503c
_journal_year                    2008
_chemical_formula_sum            'C65.5 H82.5 B3 F12 N11.5 O5 Rh3'
_chemical_formula_weight         1680.09
_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                104.890(11)
_cell_angle_beta                 90.88(2)
_cell_angle_gamma                108.688(16)
_cell_formula_units_Z            2
_cell_length_a                   14.304(3)
_cell_length_b                   14.663(5)
_cell_length_c                   18.456(6)
_cell_measurement_temperature    213(2)
_cell_volume                     3523.5(19)
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.881
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device_type  'Rigaku RAXIS-IV Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode X-ray generator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0880
_diffrn_reflns_av_sigmaI/netI    0.0883
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25478
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        0.0000
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisimatic
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.610
_refine_diff_density_min         -2.173
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       0.0219(15)
_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   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     895
_refine_ls_number_reflns         14223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1217
_refine_ls_R_factor_gt           0.0892
_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^)+(0.1758P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2375
_refine_ls_wR_factor_ref         0.2726
_reflns_number_gt                9272
_reflns_number_total             14223
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b713503c.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C65.50 H82.50 B3 F12 N11.50 O5 Rh3'
_cod_database_code               7003183