Potassium-alkyl magnesiates: synthesis, structures and Mg-H exchange applications of aromatic and heterocyclic substrates
Sharon E. Baillie; Tobias D. Bluemke; William Clegg; Alan R. Kennedy; Jan Klett; Luca Russo; Marco de Tullio; Eva Hevia; Chem.Commun. 50 (2014) 12859–; doi:10.1039/C4cc05305B

data_7115807
_publ_section_title
;
 Potassium-alkyl magnesiates: synthesis, structures and Mg-H exchange
 applications of aromatic and heterocyclic substrates
;
_journal_name_full               Chem.Commun.
_journal_page_first              12859
_journal_paper_doi               10.1039/C4cc05305B
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C36 H78 K2 Mg2 Si6'
_chemical_formula_weight         806.34
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_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                 95.260(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.0299(13)
_cell_length_b                   10.6135(10)
_cell_length_c                   19.8180(17)
_cell_measurement_reflns_used    1711
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.9322
_cell_measurement_theta_min      2.7849
_cell_volume                     2519.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Diffraction Gemini S'
_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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0715
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12822
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    0.377
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95873
_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            colourless
_exptl_crystal_density_diffrn    1.063
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.853
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         5506
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.853
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0637
_reflns_number_gt                3596
_reflns_number_total             5506
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c4cc05305b2.cif
_cod_data_source_block           jksha12
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7115807