Dinitrogen Labile Coordination versus Four-Electron Reduction, THF Cleavage, and Fragmentation Promoted by a (calix-tetrapyrrole)Sm(II) Complex
Guan, Jingwen; Dubé, Tiffany; Gambarotta, Sandro; Yap, Glenn P. A.; Organometallics 19 (2000) 4820–4827; doi:10.1021/om000698p

data_4077645
_publ_section_title
;
 Dinitrogen Labile Coordination versus Four-Electron Reduction, THF
 Cleavage, and Fragmentation Promoted by a (calix-tetrapyrrole)Sm(II)
 Complex
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              4820
_journal_page_last               4827
_journal_paper_doi               10.1021/om000698p
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C50 H67 Li3 N4 O3 Sm'
_chemical_formula_weight         943.25
_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                 99.509(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.780(3)
_cell_length_b                   18.755(3)
_cell_length_c                   12.1258(17)
_cell_measurement_temperature    203(2)
_cell_volume                     4660.8(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7946
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    1.304
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1960
_refine_diff_density_max         2.377
_refine_diff_density_min         -1.874
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         7946
_refine_ls_number_restraints     806
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1037
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          1.178
_refine_ls_shift/su_mean         0.026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1487
_refine_ls_wR_factor_ref         0.1615
_reflns_number_gt                4920
_reflns_number_total             7946
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000698p.cif
_cod_data_source_block           sg227a
_cod_original_cell_volume        4660.9(11)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4077645