Assessing the reactivity of sodium zincate [(TMEDA)Na(TMP)Zn(t)Bu2] towards benzoylferrocene: deprotonative metalation vs. alkylation reactions.
Hevia, Eva; Kennedy, Alan R.; McCall, Matthew D.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 98–103; doi:10.1039/c1dt11465d

data_7017802
_publ_section_title
;
 Assessing the reactivity of sodium zincate [(TMEDA)Na(TMP)Zn(t)Bu2]
 towards benzoylferrocene: deprotonative metalation vs. alkylation
 reactions.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              98
_journal_page_last               103
_journal_paper_doi               10.1039/c1dt11465d
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C36 H56 Fe N3 Na O Zn'
_chemical_formula_sum            'C36 H56 Fe N3 Na O Zn'
_chemical_formula_weight         691.05
_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                 111.772(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.5928(8)
_cell_length_b                   11.8192(4)
_cell_length_c                   19.0005(8)
_cell_measurement_reflns_used    4729
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.6303
_cell_measurement_theta_min      2.6383
_cell_volume                     3460.5(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_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  0.0648
_diffrn_reflns_av_sigmaI/netI    0.1570
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20669
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    1.157
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.787
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         8165
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.788
_refine_ls_R_factor_all          0.1137
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0259P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0771
_reflns_number_gt                4235
_reflns_number_total             8165
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            c1dt11465d.txt
_cod_data_source_block           mm2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7017802