Catalytic C–C Bond Formation Promoted by Organo- and Amidomagnesium(II) Compounds
Schwamm, Ryan J.; Coles, Martyn P.; Organometallics 32 (2013) 5277–; doi:10.1021/om400909e

data_4081707
_publ_section_title
;
 Catalytic C--C Bond Formation Promoted by Organo- and Amidomagnesium(II)
 Compounds
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5277
_journal_paper_doi               10.1021/om400909e
_journal_volume                  32
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C30 H72 Mg N6 O Si4'
_chemical_formula_sum            'C30 H72 Mg N6 O Si4'
_chemical_formula_weight         669.61
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
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_audit_creation_date             2013-06-26T11:35:40-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 114.059(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9306(2)
_cell_length_b                   24.2870(4)
_cell_length_c                   18.9646(4)
_cell_measurement_reflns_used    25144
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      73.7640
_cell_measurement_theta_min      4.8750
_cell_measurement_wavelength     1.5418
_cell_volume                     4176.61(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector_area_resol_mean 5.3250
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_orient_matrix_UB_11      -0.1255083000
_diffrn_orient_matrix_UB_12      0.0101999000
_diffrn_orient_matrix_UB_13      -0.0596862000
_diffrn_orient_matrix_UB_21      -0.0427923000
_diffrn_orient_matrix_UB_22      0.0479889000
_diffrn_orient_matrix_UB_23      0.0493246000
_diffrn_orient_matrix_UB_31      0.0829799000
_diffrn_orient_matrix_UB_32      0.0402101000
_diffrn_orient_matrix_UB_33      -0.0437408000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            53241
_diffrn_reflns_theta_full        66.9682
_diffrn_reflns_theta_max         73.8056
_diffrn_reflns_theta_min         3.1300
_exptl_absorpt_coefficient_mu    1.683
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         8369
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0799
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+4.3794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.13
_reflns_number_gt                7105
_reflns_number_total             8369
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400909e_si_002.cif
_cod_data_source_block           Compound-3
_cod_original_cell_volume        4176.61(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4081707
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1