Alkali-metal organomagnesiate complexes as catalysts for highly chemoselective crossed-Tishchenko reactions.
Guo, Zhiqiang; Pang, Tengfei; Wang, Yakong; Zhang, Yongbin; Wei, Xuehong; Dalton transactions (Cambridge, England : 2003) 49 (2020) 6418–6424; doi:10.1039/d0dt01114b

data_7704184
_publ_section_title
;
 Alkali-metal organomagnesiate complexes as catalysts for highly
 chemoselective crossed-Tishchenko reactions.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6418
_journal_page_last               6424
_journal_paper_doi               10.1039/d0dt01114b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'C32.087 H61.218 Mg2 N4 Na2 O1.522, 0.478(C4 H10 O1)'
_chemical_formula_sum            'C34 H66 Mg2 N4 Na2 O2'
_chemical_formula_weight         657.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-04-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-04-20 deposited with the CCDC.	2020-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.2336(6)
_cell_length_b                   19.0795(6)
_cell_length_c                   24.5532(8)
_cell_measurement_reflns_used    9682
_cell_measurement_temperature    136(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.89
_cell_volume                     8073.3(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      135.93
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0315
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            57700
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.888
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.082
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.0019(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7087
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0726P)^2^+10.2194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1617
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6027
_reflns_number_total             7087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01114b2.cif
_cod_data_source_block           mo_161019a_0m_a
_cod_depositor_comments
'Adding full bibliography for 7704180--7704184.cif.'
_cod_database_code               7704184
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.967
_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. Restrained distances
 O2B-C52B = C52A-O2A
 1.59 with sigma of 0.02
3. Rigid bond restraints
 O2B, C50B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Sof(O2B)=Sof(C50B)=Sof(H50C)=Sof(H50D)=Sof(C51B)=Sof(H51D)=Sof(H51E)=
 Sof(H51F)=Sof(C52B)=Sof(H52C)=Sof(H52D)=Sof(C53B)=Sof(H53D)=Sof(H53E)=
 Sof(H53F)=1-FVAR(1)
 Sof(O2A)=Sof(C50A)=Sof(H50A)=Sof(H50B)=Sof(C51A)=Sof(H51A)=Sof(H51B)=
 Sof(H51C)=Sof(C52A)=Sof(H52A)=Sof(H52B)=Sof(C53A)=Sof(H53A)=Sof(H53B)=
 Sof(H53C)=FVAR(1)
5.a Everything fixed:
 C3
5.b Riding coordinates:
 C1(H1), C2(H2), C3(H3), C11(H11), C12(H12), C50A(H50A,H50B), C52A(H52A,H52B),
 C50B(H50C,H50D), C52B(H52C,H52D)
5.c Ternary CH refined with riding coordinates:
 C10(H10)
5.d Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C14(H14A,H14B), C20(H20A,H20B), C21(H21A,H21B), C23(H23A,H23B),
 C24A(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B), C29(H29A,H29B)
5.e Me refined with riding coordinates:
 C51A(H51A,H51B,H51C), C53A(H53A,H53B,H53C), C51B(H51D,H51E,H51F), C53B(H53D,
 H53E,H53F)
5.f Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              43705
_olex2_submission_special_instructions 'No special instructions were received'