Bis(amido)magnesium mediated aldol additions: first structural characterisation of an amidomagnesium aldolate intermediate
Allan, John F.; Henderson, Kenneth W.; Kennedy, Alan R.; Chemical Communications  (1999) 1325–; doi:10.1039/a903784e

data_7110589
_publ_contact_author
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Alan Kennedy
Dept. of P & A Chemistry
University of Strathclyde
295 Cathedral St
Glasgow G1 1XL
Scotland
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_publ_section_title
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 Bis(amido)magnesium mediated aldol additions: first structural
 characterisation of an amidomagnesium aldolate intermediate
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_journal_issue                   14
_journal_name_full               'Chemical Communications'
_journal_page_first              1325
_journal_paper_doi               10.1039/a903784e
_journal_year                    1999
_chemical_formula_sum            'C36 H82 Mg2 N2 O4 Si4'
_chemical_formula_weight         768.02
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.90(2)
_cell_angle_beta                 104.00(2)
_cell_angle_gamma                105.996(19)
_cell_formula_units_Z            1
_cell_length_a                   9.610(3)
_cell_length_b                   11.381(2)
_cell_length_c                   12.024(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      22.41
_cell_measurement_theta_min      21.35
_cell_volume                     1191.6(6)
_computing_cell_refinement       'AFC7S DIFFRACTOMETER CONTROL'
_computing_data_collection       'AFC7S DIFFRACTOMETER CONTROL'
_computing_data_reduction        TEXSAN
_computing_molecular_graphics    ORTEP
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku AFC7S Diffractometer'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
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_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6084
_diffrn_reflns_theta_full        28.03
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.185
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.365
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_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5746
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_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+0.7217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1417
_reflns_number_gt                4652
_reflns_number_total             5746
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            903784esup1.cif
_cod_data_source_block           h15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+0.7217P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+0.7217P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1191.5(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110589