Cyclopentadienyl Behavior of Pyrrolyl Anions within the meso-Octaethylporphyrinogen-Binding Lanthanides: Carbon-Hydrogen and Metal-Carbon Bond Rearrangements
Elisa Campazzi; Euro Solari; Rosario Scopelliti; Carlo Floriani; Inorganic Chemistry 38 (1999) 6240–6245; doi:10.1021/ic990742x

data_4322555
_publ_contact_author_address
;
Institut de Chimie Min\'erale et Analytique
BCH # 3307
Universit\'e de Lausanne
CH-1015 Lausanne
Switzerland
;
_publ_contact_author_email       carlo.floriani@icma.unil.ch
_publ_contact_author_fax         '+4121 692 3905'
_publ_contact_author_name        'Carlo Floriani'
_publ_contact_author_phone       '+4121 692 3902'
_publ_section_title
;
 Cyclopentadienyl Behavior of Pyrrolyl Anions within the
 meso-Octaethylporphyrinogen-Binding Lanthanides: Carbon-Hydrogen and
 Metal-Carbon Bond Rearrangements
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6240
_journal_page_last               6245
_journal_paper_doi               10.1021/ic990742x
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety         'C72 H96 N8 Sm2, 2Na(C4 H10 O2)3'
_chemical_formula_sum            'C96 H156 N8 Na2 O12 Sm2'
_chemical_formula_weight         1960.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.61(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.556(3)
_cell_length_b                   24.187(4)
_cell_length_c                   18.759(3)
_cell_measurement_reflns_used    '243 spots from first image'
_cell_measurement_temperature    173(2)
_cell_volume                     5617.0(19)
_computing_cell_refinement       'marresearch, marHKL, release 1.9.1'
_computing_data_collection       'marresearch, mar345, release 1.2.11'
_computing_data_reduction        'marresearch, marHKL'
_computing_molecular_graphics    'Bruker, SHELXTL, release 5.1'
_computing_publication_material  'Bruker, SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'mar345 IPDS'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_sigmaI/netI    0.0691
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38316
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    1.096
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2060
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.055
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.232
_refine_ls_extinction_coef       0.0052(5)
_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   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         8971
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0640
_refine_ls_shift/su_max          0.105
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1427P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1940
_refine_ls_wR_factor_ref         0.2127
_reflns_number_gt                6155
_reflns_number_total             8971
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990742x_3.cif
_cod_data_source_block           11
_cod_original_cell_volume        5616.9(19)
_cod_database_code               4322555