Synthesis, Structure, and Methyl Methacrylate Polymerization Activity of a Mixed π-Ferrocene π-Toluene Complex of Potassium Tris(hexamethyldisilazide)magnesiate
Honeyman, Gordon W.; Kennedy, Alan R.; Mulvey, Robert E.; Sherrington, David C.; Organometallics 23 (2004) 1197–; doi:10.1021/om034390k

data_4076287
_publ_section_title
;
 Synthesis, Structure, and Methyl Methacrylate Polymerization Activity of
 a Mixed \p-Ferrocene \p-Toluene Complex of Potassium
 Tris(hexamethyldisilazide)magnesiate
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1197
_journal_paper_doi               10.1021/om034390k
_journal_volume                  23
_journal_year                    2004
_chemical_formula_sum            'C52 H90 Fe2 K Mg N3 Si6'
_chemical_formula_weight         1100.92
_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                 99.293(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0176(2)
_cell_length_b                   22.4722(3)
_cell_length_c                   23.2871(4)
_cell_measurement_reflns_used    195597
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      1.01
_cell_volume                     6206.42(17)
_computing_data_collection       'Denzo and Collect'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Shelxs-97
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Nonious Kappa CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1052
_diffrn_reflns_av_sigmaI/netI    0.1627
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            117007
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         1.27
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sortav, R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            'light orange'
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         12844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1651
_refine_ls_R_factor_gt           0.0693
_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^)+(0.0357P)^2^+2.6995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1116
_reflns_number_gt                6963
_reflns_number_total             12844
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om034390ksi20031219_103358.cif
_cod_data_source_block
;grem96_publ_contact_letter_
Dear Sir,

This cif contains the crystallographic data for the proposed paper
"Synthesis, structure, and methyl methacrylate polymerisation activity
of a mixed pi-ferrocene pi-toluene complex of potassium
tris(hexamethyldisilazide)magnesiate" by GW Honeyman, AR Kennedy, RE Mulvey
& DC Sherrington. The ms will shortly be presented to Organometallics
for consideration to publish. Could you please send me a deposit reference
number for this structure? 

Thank You for your help

Alan Kennedy
;
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4076287