Remote functionalisation via sodium alkylamidozincate intermediates: access to unusual fluorenone and pyridyl ketone reactivity patterns
James J. Crawford; Ben J. Fleming; Alan R. Kennedy; Jan Klett; Charles T. OHara; Samantha A. Orr; Chem.Commun. 47 (2011) 3772–; doi:10.1039/c1cc10193e

data_7106149
_publ_section_title
;
 Remote functionalisation via sodium alkylamidozincate intermediates:
 access to unusual fluorenone and pyridyl ketone reactivity patterns
;
_journal_name_full               Chem.Commun.
_journal_page_first              3772
_journal_paper_doi               10.1039/c1cc10193e
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C36 H60 N3 Na O Zn'
_chemical_formula_weight         639.23
_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                 94.903(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.2426(6)
_cell_length_b                   19.6573(15)
_cell_length_c                   36.846(3)
_cell_measurement_reflns_used    6857
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.16
_cell_measurement_theta_min      3.13
_cell_volume                     7391.5(9)
_computing_cell_refinement       'Oxford Diffraction Reduction Software'
_computing_data_collection       'Oxford Diffraction Collection Software'
_computing_data_reduction        'Oxford Diffraction Reduction Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur E'
_diffrn_measurement_method       '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  0.0842
_diffrn_reflns_av_sigmaI/netI    0.1959
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            49503
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50172
_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            blue
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sliver
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.762
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         14502
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      0.766
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0332P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0910
_reflns_number_gt                6256
_reflns_number_total             14502
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c1cc10193e.txt
_cod_data_source_block           jkcben11
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7106149