Reactivity of a β-diketiminate-supported magnesium alkyl complex toward small molecules.
Ren, Wenshan; Zhang, Shaohui; Xu, Ziyi; Ma, Xuebing; Dalton transactions (Cambridge, England : 2003) 48 (2019) 3109–3115; doi:10.1039/c9dt00090a

data_7048867
_publ_section_title
;
 Reactivity of a \b-diketiminate-supported magnesium alkyl complex toward
 small molecules.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3109
_journal_page_last               3115
_journal_paper_doi               10.1039/c9dt00090a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C37 H55.92 Mg N2 O Se2'
_chemical_formula_sum            'C37 H55.92 Mg N2 O Se2'
_chemical_formula_weight         726.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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
_audit_creation_date             2018-12-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2018-12-17 deposited with the CCDC.
2019-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.036(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.0510(5)
_cell_length_b                   10.0565(2)
_cell_length_c                   16.8071(4)
_cell_measurement_reflns_used    15752
_cell_measurement_temperature    150(10)
_cell_measurement_theta_max      71.2110
_cell_measurement_theta_min      4.8250
_cell_volume                     3704.65(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      150(10)
_diffrn_detector_area_resol_mean 8.0243
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34408
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.019
_diffrn_reflns_theta_min         4.838
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.875
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         7141
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0581P)^2^+4.7491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1160
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6343
_reflns_number_total             7141
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00090a2.cif
_cod_data_source_block           p21c
_cod_depositor_comments
'Adding full bibliography for 7048864--7048869.cif.'
_cod_database_code               7048867
_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
 C35-C37A
 1.44 with sigma of 0.02
 C35-C37B
 1.44 with sigma of 0.02
 C35-C36A
 1.44 with sigma of 0.02
 C16-C17A
 1.44 with sigma of 0.04
 C16-C17B
 1.44 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C29: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Se1A) \\sim Ueq, Uanis(Se2A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.001
4. Others
 Sof(Se1A)=Sof(Se2A)=1-FVAR(1)
 Sof(H1A)=Sof(H1B)=Sof(H2A)=Sof(H2B)=Sof(Se1)=Sof(Se2)=FVAR(1)
 Fixed Sof: H16(0.4) C17A(0.6) H17A(0.6) H17B(0.6) H17C(0.6) C17B(0.4)
 H17D(0.4) H17E(0.4) H17F(0.4) H27(0.5) C28A(0.5) H28A(0.5) H28B(0.5) H28C(0.5)
 C28B(0.5) H28D(0.5) H28E(0.5) H28F(0.5) H35(0.5) C36A(0.5) H36A(0.5) H36B(0.5)
 H36C(0.5) C37A(0.5) H37A(0.5) H37B(0.5) H37C(0.5) C36B(0.5) H36D(0.5)
 H36E(0.5) H36F(0.5) C37B(0.5) H37D(0.5) H37E(0.5) H37F(0.5)
5.a Ternary CH refined with riding coordinates:
 C16(H16), C20(H20), C27(H27), C35(H35)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B)
5.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C14(H14), C23(H23), C30(H30), C31(H31), C32(H32)
5.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C15(H15A,H15B,H15C), C17A(H17A,H17B,H17C), C17B(H17D,H17E,
 H17F), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C25(H25A,
 H25B,H25C), C26(H26A,H26B,H26C), C28A(H28A,H28B,H28C), C28B(H28D,H28E,H28F),
 C36A(H36A,H36B,H36C), C37A(H37A,H37B,H37C), C36B(H36D,H36E,H36F), C37B(H37D,
 H37E,H37F)
;
_shelx_shelxl_version_number     2017/1
_olex2_submission_special_instructions 'No special instructions were received'