A Homologous Series of Regioselectively Tetradeprotonated Group 8 Metallocenes: New Inverse Crown Ring Compounds Synthesized via a Mixed Sodium-Magnesium Tris(diisopropylamide) Synergic Base
Prokopis C. Andrikopoulos; David R. Armstrong; William Clegg; Carly J. Gilfillan; Eva Hevia; Alan R. Kennedy; Robert E. Mulvey; Charles T. O'Hara; John A. Parkinson; Duncan M. Tooke; Journal of the American Chemical Society 126 (2004) 11612–11620; doi:10.1021/ja0472230

data_4112946
_publ_section_title
;
 A Homologous Series of Regioselectively Tetradeprotonated Group 8
 Metallocenes: New Inverse Crown Ring Compounds Synthesized via a Mixed
 Sodium-Magnesium Tris(diisopropylamide) Synergic Base
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11612
_journal_page_last               11620
_journal_paper_doi               10.1021/ja0472230
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C58 H118 Fe Mg4 N8 Na4'
_chemical_formula_sum            'C58 H118 Fe Mg4 N8 Na4'
_chemical_formula_weight         1172.65
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.082(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.1070(7)
_cell_length_b                   15.2446(6)
_cell_length_c                   16.2557(7)
_cell_measurement_reflns_used    19059
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.45
_cell_volume                     3521.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29235
_diffrn_reflns_theta_full        26.0
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.248
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         8205
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.248
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0599P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1127
_reflns_number_gt                6565
_reflns_number_total             8205
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja0472230si20040712_113051_1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4112946