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_7042283
_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         'C41 H74 Mg N4 O Si2'
_chemical_formula_sum            'C41 H74 Mg N4 O Si2'
_chemical_formula_weight         719.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-08-31
_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                90.000(5)
_cell_angle_beta                 107.486(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   10.752(5)
_cell_length_b                   36.875(5)
_cell_length_c                   11.551(5)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.531
_cell_measurement_theta_min      2.588
_cell_volume                     4368(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.969
_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  0.0593
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            64589
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         29.626
_diffrn_reflns_theta_min         2.061
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6311
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1341 before and 0.0534 after correction.
The Ratio of minimum to maximum transmission is 0.8461.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.094
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         11918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0602
_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^)+(0.0415P)^2^+3.8654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1355
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9522
_reflns_number_total             11918
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00556c2.cif
_cod_data_source_block           sn_mb_205_m
_cod_depositor_comments
'Adding full bibliography for 7042282--7042283.cif.'
_cod_database_code               7042283
_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:
 C11(H11), C26(H26), C8(H8), C29(H29), C20(H20), C23(H23)
2.b Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C41(H41A,H41B), C40(H40A,H40B), C39(H39A,H39B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C18(H18), C4(H4), C16(H16), C17(H17), C5(H5)
2.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C10(H10A,H10B,H10C), C31(H31A,H31B,H31C), C21(H21A,H21B,
 H21C), C9(H9A,H9B,H9C), C22(H22A,H22B,H22C), C13(H13A,H13B,H13C), C25(H25A,
 H25B,H25C), C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C34(H34A,H34B,H34C),
 C35(H35A,H35B,H35C), C12(H12A,H12B,H12C), C36(H36A,H36B,H36C), C32(H32A,H32B,
 H32C), C37(H37A,H37B,H37C), C33(H33A,H33B,H33C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              45030
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'