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_7115808
_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            'C34 H90 K2 Mg N6 Si4'
_chemical_formula_weight         797.99
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2327(4)
_cell_length_b                   17.0823(5)
_cell_length_c                   25.0444(9)
_cell_measurement_reflns_used    11114
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.4274
_cell_measurement_theta_min      2.7102
_cell_volume                     5233.3(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0572
_diffrn_reflns_av_sigmaI/netI    0.1182
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            40219
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    0.311
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.013
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.17(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.806
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         13880
_refine_ls_number_restraints     170
_refine_ls_restrained_S_all      0.805
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0188P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0596
_reflns_number_gt                8778
_reflns_number_total             13880
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c4cc05305b2.cif
_cod_data_source_block           jksha21
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               7115808