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_7114180
_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            'C44 H30 Cl28 Cu O15'
_chemical_formula_weight         1854.82
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 92.18(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.644(4)
_cell_length_b                   15.118(3)
_cell_length_c                   18.580(3)
_cell_measurement_reflns_used    46255
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      1.0
_cell_volume                     7198(2)
_computing_data_collection       'Kappa CCD'
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measurement_device       'Kappa CCD'
_diffrn_measurement_method       phi-scan
_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  0.0595
_diffrn_reflns_av_sigmaI/netI    0.0791
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9744
_diffrn_reflns_theta_max         19.00
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.399
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_description       plate
_exptl_crystal_F_000             3676
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.049
_refine_ls_goodness_of_fit_obs   1.150
_refine_ls_hydrogen_treatment    'not refined'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     754
_refine_ls_number_reflns         4212
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.122
_refine_ls_restrained_S_obs      1.151
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_obs          0.0707
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0803P)^2^+62.1514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2068
_refine_ls_wR_factor_obs         0.1678
_reflns_number_observed          3134
_reflns_number_total             4617
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b208759f.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0803P)^2^+62.1514P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0803P)^2^+62.1514P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7198.0(22)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7114180