Metal-Radical Chains Based on Polychlorotriphenylmethyl Radicals: Synthesis, Structure, and Magnetic Properties
Nans Roques; Neus Domingo; Daniel Maspoch; Klaus Wurst; Concepció Rovira; Javier Tejada; Daniel Ruiz-Molina; Jaume Veciana; Inorganic Chemistry 49 (2010) 3482–3488; doi:10.1021/ic100037z

data_4315218
_publ_contact_author_address
;
Campus Universitari
Institut de Ciencia de Materials de Barcelona
Cerdanyola
Barcelona
08193
SPAIN
;
_publ_contact_author_email       VECIANAJ@ICMAB.ES
_publ_contact_author_name        'Prof J Veciana'
_publ_section_title
;
 Metal-Radical Chains Based on Polychlorotriphenylmethyl Radicals:
 Synthesis, Structure, and Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3482
_journal_page_last               3488
_journal_paper_doi               10.1021/ic100037z
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C63 H61 Cl26 Co2 N7 O21'
_chemical_formula_weight         2291.75
_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                 94.630(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   31.532(5)
_cell_length_b                   9.263(2)
_cell_length_c                   16.646(2)
_cell_measurement_reflns_used    37872
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      1.0
_cell_volume                     4846.1(14)
_computing_data_collection       COLLECT
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.698
_diffrn_measured_fraction_theta_max 0.698
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-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  0.0624
_diffrn_reflns_av_sigmaI/netI    0.0772
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6395
_diffrn_reflns_theta_full        19.87
_diffrn_reflns_theta_max         19.87
_diffrn_reflns_theta_min         2.29
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.124
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.0159(19)
_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   1.105
_refine_ls_hydrogen_treatment    omitted
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         3086
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.1787
_refine_ls_R_factor_gt           0.1495
_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^)+(0.1402P)^2^+126.6186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3460
_refine_ls_wR_factor_ref         0.3608
_reflns_number_gt                2309
_reflns_number_total             3086
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100037z_si_002.cif
_cod_data_source_block           d283
_cod_database_code               4315218