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_7048868
_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         'C47 H58.67 Mg N4 S2'
_chemical_formula_sum            'C47 H58.67 Mg N4 S2'
_chemical_formula_weight         768.07
_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                 105.9520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.2566(2)
_cell_length_b                   17.0216(2)
_cell_length_c                   13.6278(2)
_cell_measurement_reflns_used    14320
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.7910
_cell_measurement_theta_min      5.0440
_cell_volume                     4740.95(10)
_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(2)
_diffrn_detector_area_resol_mean 8.0243
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            35040
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.423
_diffrn_reflns_theta_min         3.379
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.393
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42789
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1651
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
The Platon SQUEEZE procedure was applied to recover 68 electrons per
unit cell in one void (total volume 766 ^A^3); that is 17 electrons
per formula unit. Lattice solvent benzene molecules (42 electrons/C6H6)
were present, and the electrons recovered by SQUEEZE have been assigned
as 0.5 benzene molecules per formula unit. These benzene molecules have
been included in the formula for the calculation of intensive
properties.
;
_refine_diff_density_max         0.885
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         9328
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0689P)^2^+3.8901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.1575
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6872
_reflns_number_total             9328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00090a2.cif
_cod_data_source_block           p21c_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7048864--7048869.cif.'
_cod_database_code               7048868
_platon_squeeze_void_probe_radius 1.20
_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. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim C4 \\sim C5A \\sim C5B \\sim C5C: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: H4A(0.33333) H4B(0.33333) C5A(0.33333) H5AA(0.33333) H5AB(0.33333)
 H5AC(0.33333) C5B(0.33333) H5BA(0.33333) H5BB(0.33333) H5BC(0.33333)
 C5C(0.33333) H5CA(0.33333) H5CB(0.33333) H5CC(0.33333)
4.a Ternary CH refined with riding coordinates:
 C26(H26), C45(H45), C21(H21), C38(H38), C14(H14)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
4.c Aromatic/amide H refined with riding coordinates:
 C29(H29), C43(H43), C30(H30), C41(H41), C42(H42), C11(H11), C10(H10),
 C17(H17), C8(H8), C7(H7), C33(H33), C31(H31), C9(H9), C19(H19), C18(H18),
 C32(H32)
4.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C35(H35A,H35B,
 H35C), C25(H25A,H25B,H25C), C22(H22A,H22B,H22C), C16(H16A,H16B,H16C), C23(H23A,
 H23B,H23C), C15(H15A,H15B,H15C), C39(H39A,H39B,H39C), C5A(H5AA,H5AB,H5AC),
 C5B(H5BA,H5BB,H5BC), C5C(H5CA,H5CB,H5CC)
;
_shelx_shelxl_version_number     2017/1
_olex2_submission_special_instructions 'No special instructions were received'