Structurally Defined Zincated and Aluminated Complexes of Ferrocene Made by Alkali-Metal Synergistic Syntheses
Clegg, William; Crosbie, Elaine; Dale-Black, Sophie H.; Hevia, Eva; Honeyman, Gordon W.; Kennedy, Alan R.; Mulvey, Robert E.; Ramsay, Donna L.; Robertson, Stuart D.; Organometallics 34 (2015) 2580–; doi:10.1021/om5012352

data_4085435
_publ_section_title
;
 Structurally Defined Zincated and Aluminated Complexes of Ferrocene Made
 by Alkali-Metal Synergistic Syntheses
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2580
_journal_paper_doi               10.1021/om5012352
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C48 H94 Fe N6 Na2 Zn2'
_chemical_formula_sum            'C48 H94 Fe N6 Na2 Zn2'
_chemical_formula_weight         987.86
_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                 94.393(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4467(13)
_cell_length_b                   30.620(3)
_cell_length_c                   13.450(3)
_cell_measurement_reflns_used    55
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_cell_volume                     5521.6(15)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs, 1990-2000)'
_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      180(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    '0.6 mm double-pinhole'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'normal focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1005
_diffrn_reflns_av_sigmaI/netI    0.0996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            32291
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.27
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.171
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_correction_T_min  0.774
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SHELXTL'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     670
_refine_ls_number_reflns         9617
_refine_ls_number_restraints     427
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.0792
_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^)+(0.0136P)^2^+15.2535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1332
_reflns_number_gt                6387
_reflns_number_total             9617
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om5012352_si_002.cif
_cod_data_source_block           rem323
_cod_depositor_comments
'Adding full bibliography for 4085434--4085438.cif.'
_cod_original_cell_volume        5521.4(15)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4085435