Use of Calix[4]arenes in the Redox Chemistry of Lanthanides: the Reduction of Dinitrogen by a Calix[4]arene-Samarium Complex
Geoffroy Guillemot; Barbara Castellano; Thierry Prangé; Euro Solari; Carlo Floriani; Inorganic Chemistry 46 (2007) 5152–5154; doi:10.1021/ic700787d

data_4308316
_publ_section_title
;
Use of Calix[4]arenes in the Redox Chemistry of Lanthanides: the
Reduction of Dinitrogen by a Calix[4]arene-Samarium Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5152
_journal_page_last               5154
_journal_paper_doi               10.1021/ic700787d
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C116 H164 Cl2 N0 O14 Sm2'
_chemical_formula_weight         2154.07
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                90.000(10)
_cell_angle_beta                 109.004(10)
_cell_angle_gamma                90.000(10)
_cell_formula_units_Z            4
_cell_length_a                   35.1360(2)
_cell_length_b                   16.7980(2)
_cell_length_c                   20.6270(2)
_cell_measurement_temperature    293(2)
_cell_volume                     11510.8(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8844
_diffrn_reflns_theta_full        24.11
_diffrn_reflns_theta_max         24.11
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    1.114
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4520
_refine_diff_density_max         1.526
_refine_diff_density_min         -1.645
_refine_diff_density_rms         0.152
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -10(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         8844
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          1.780
_refine_ls_shift/su_mean         0.091
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0823P)^2^+191.5356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2084
_refine_ls_wR_factor_ref         0.2159
_reflns_number_gt                6893
_reflns_number_total             8844
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700787d-file003.cif
_cod_data_source_block           gg801
_cod_original_cell_volume        11510.80(19)
_cod_database_code               4308316