A very bulky carboxylic perchlorotriphenylmethyl radical as a novel ligand for transition metal complexes. A new spin frustrated metal system
Maspoch, Daniel; Ruiz-Molina, Daniel; Wurst, Klaus; Rovira, Concepció; Veciana, Jaume; Chemical Communications  (2002) 2958–2959; doi:10.1039/b208759f

data_7114181
_publ_section_title
;
 A very bulky carboxylic perchlorotriphenylmethyl radical as a novel
 ligand for transition metal complexes. A new spin frustrated metal system
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              2958
_journal_page_last               2959
_journal_paper_doi               10.1039/b208759f
_journal_year                    2002
_chemical_formula_sum            'C52 H34 Cl28 Cu2 O14'
_chemical_formula_weight         2002.47
_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                 93.760(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   26.296(2)
_cell_length_b                   16.9040(9)
_cell_length_c                   8.5648(6)
_cell_measurement_reflns_used    32930
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      1.0
_cell_volume                     3798.9(4)
_computing_data_collection       'Kappa CCD'
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Kappa CCD'
_diffrn_measurement_method       'phi- and omega-scans'
_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  0.0678
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            12387
_diffrn_reflns_theta_full        19.75
_diffrn_reflns_theta_max         19.75
_diffrn_reflns_theta_min         1.43
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.601
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    'mixed, refined at O5 with bond restraints'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         3413
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.217
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+23.3969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1206
_reflns_number_gt                2724
_reflns_number_total             3413
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b208759f.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7114181