Organomagnesium amide catalyzed cross-dehydrocoupling of organosilanes with amines.
Baishya, Ashim; Peddarao, Thota; Nembenna, Sharanappa; Dalton transactions (Cambridge, England : 2003)  (2017) –; doi:10.1039/c7dt00806f

data_7043786
_publ_section_title
;
 Organomagnesium amide catalyzed cross-dehydrocoupling of organosilanes
 with amines.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/c7dt00806f
_journal_year                    2017
_chemical_formula_moiety         'C36 H53 Mg N3 Si2'
_chemical_formula_sum            'C36 H53 Mg N3 Si2'
_chemical_formula_weight         608.30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_date             2015-01-05
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.12.26 svn.r3119 for OlexSys, GUI svn.r4975)
;
_audit_update_record
;
2016-11-16 deposited with the CCDC.
2017-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                85.9850(10)
_cell_angle_beta                 77.6490(10)
_cell_angle_gamma                77.783(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1877(3)
_cell_length_b                   11.2375(3)
_cell_length_c                   18.5799(5)
_cell_measurement_reflns_used    7516
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.19
_cell_measurement_theta_min      2.88
_cell_volume                     1830.86(9)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29800
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.570
_diffrn_reflns_theta_min         2.245
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.141
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0843 before and 0.0486 after correction.
The Ratio of minimum to maximum transmission is 0.8519.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         10999
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0808P)^2^+0.3185P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1521
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8168
_reflns_number_total             10999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00806f2.cif
_cod_data_source_block           try1
_cod_database_code               7043786
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H12A,H12B,H12C} of C12
 At 1.5 times of:
  {H28A,H28B,H28C} of C28, {H36A,H36B,H36C} of C36, {H37A,H37B,H37C} of C37,
  {H35A,H35B,H35C} of C35, {H34A,H34B,H34C} of C34, {H17A,H17B,H17C} of C17,
  {H33A,H33B,H33C} of C33, {H32A,H32B,H32C} of C32, {H11A,H11B,H11C} of C11,
  {H10A,H10B,H10C} of C10, {H31A,H31B,H31C} of C31, {H30A,H30B,H30C} of C30,
  {H20A,H20B,H20C} of C20, {H21A,H21B,H21C} of C21
2.a Aromatic/amide H refined with riding coordinates:
 C27(H27), C18(H18), C2(H2), C3(H3), C6(H6), C8(H8), C15(H15), C24(H24)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C28(H28A,H28B,H28C), C17(H17A,H17B,H17C), C33(H33A,H33B,
 H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C), C32(H32A,H32B,H32C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C31(H31A,H31B,H31C), C30(H30A,H30B,
 H30C)
;
_shelx_res_checksum              10218
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'