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_7048864
_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         'C33 H50 Mg N2 S'
_chemical_formula_sum            'C66 H100 Mg2 N4 S2'
_chemical_formula_weight         1062.24
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.23 svn.r2946 for OlexSys, GUI svn.r4855)
;
_audit_update_record
;
2018-12-17 deposited with the CCDC.
2019-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.3880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.01460(10)
_cell_length_b                   20.5390(2)
_cell_length_c                   14.3234(2)
_cell_measurement_reflns_used    11833
_cell_measurement_temperature    150.00(2)
_cell_measurement_theta_max      73.0160
_cell_measurement_theta_min      5.2960
_cell_volume                     3476.62(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150.00(2)
_diffrn_detector_area_resol_mean 8.0243
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.980
_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  0.0239
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25706
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.076
_diffrn_reflns_theta_min         3.805
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.142
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10005
_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    1.015
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
The Platon SQUEEZE procedure was applied to recover 72 electrons per
unit cell in one void (total volume 530 ^A^3); that is 36 electrons
per formula unit. Lattice solvent benzene molecules (42 electrons/C6H6)
were present, and the electrons recovered by SQUEEZE have been assigned
as 1 benzene molecule per formula unit. These benzene molecules have
been included in the formula for the calculation of intensive
properties.
;
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         6800
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0550P)^2^+1.6400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1154
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5849
_reflns_number_total             6800
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00090a2.cif
_cod_data_source_block           rws180123_sqd
_cod_depositor_comments
'Adding full bibliography for 7048864--7048869.cif.'
_cod_database_code               7048864
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014-1
_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:
 C14(H14), C31(H31), C7(H7), C24(H24)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C2(H2A,H2B)
2.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C10(H10), C29(H29), C28(H28), C11(H11), C12(H12)
2.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C33(H33A,H33B,H33C), C15(H15A,H15B,H15C), C32(H32A,H32B,
 H32C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C9(H9A,H9B,H9C), C8(H8A,H8B,
 H8C), C4(H4A,H4B,H4C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              66820
_olex2_submission_special_instructions 'No special instructions were received'