Magnesium amide catalyzed selective hydroboration of esters.
Barman, Milan Kr; Baishya, Ashim; Nembenna, Sharanappa; Dalton transactions (Cambridge, England : 2003) 46 (2017) 4152–4156; doi:10.1039/c7dt00556c

data_7042282
_publ_section_title
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 Magnesium amide catalyzed selective hydroboration of esters.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4152
_journal_page_last               4156
_journal_paper_doi               10.1039/c7dt00556c
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C33 H58 Mg N4 O Si2'
_chemical_formula_sum            'C33 H58 Mg N4 O Si2'
_chemical_formula_weight         607.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-09-25
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-09-26 deposited with the CCDC.
2017-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.992(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.059(5)
_cell_length_b                   19.808(5)
_cell_length_c                   15.024(5)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.52
_cell_volume                     7899(4)
_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)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            78753
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         30.585
_diffrn_reflns_theta_min         1.283
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0788 before and 0.0531 after correction.
The Ratio of minimum to maximum transmission is 0.8381.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.021
_exptl_crystal_description       block
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         12074
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+0.9980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1316
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8923
_reflns_number_total             12074
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00556c2.cif
_cod_data_source_block           sn_mb_290
_cod_depositor_comments
'Adding full bibliography for 7042282--7042283.cif.'
_cod_database_code               7042282
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C18(H18), C21(H21)
2.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B)
2.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C13(H13), C5(H5), C14(H14), C7(H7), C6(H6)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C4(H4A,H4B,H4C), C9(H9A,H9B,H9C), C19(H19A,H19B,H19C), C29(H29A,H29B,
 H29C), C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              69026
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'