An Azobenzenyl Anion Radical Complex of Magnesium: Synthesis, Structure, and Reactivity Studies.
Ren, Wenshan; Gu, Defa; Inorganic chemistry 55 (2016) 11962–11970; doi:10.1021/acs.inorgchem.6b02114

data_4349219
_publ_section_title
;
 An Azobenzenyl Anion Radical Complex of Magnesium: Synthesis, Structure,
 and Reactivity Studies.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11962
_journal_page_last               11970
_journal_paper_doi               10.1021/acs.inorgchem.6b02114
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration n
_chemical_formula_moiety         'C29 H41 Mg N5'
_chemical_formula_sum            'C29 H41 Mg N5'
_chemical_formula_weight         483.98
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-05-21
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Olex2 1.2
(compiled 2014.06.23 svn.r2946 for OlexSys, GUI svn.r4855)
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_cell_measurement_temperature    100(10)
_cell_measurement_theta_max      71.3670
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      air
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_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -31.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -77.0000  -60.0000 94

  2 omega  -31.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -77.0000 -120.0000 94

  3 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000  -90.0000 84

  4 omega    1.00   76.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -99.0000    0.0000 75

  5 omega  -31.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -57.0000  -60.0000 84

  6 omega   41.00  126.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000  -60.0000 85

  7 omega   87.00  178.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000   90.0000 91

  8 omega   39.00  110.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000 -120.0000 71

  9 omega   38.00   91.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 53

 10 omega   38.00  116.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -112.0000 -180.0000 78

 11 omega  101.00  178.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  112.0000  -90.0000 77

 12 omega   38.00   91.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 53

 13 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000    0.0000 94

 14 omega   57.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203  178.0000 -120.0000 52

 15 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000  150.0000 94

 16 omega   91.00  134.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000    0.0000 43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0000334000
_diffrn_orient_matrix_UB_12      0.0850810000
_diffrn_orient_matrix_UB_13      -0.0415935000
_diffrn_orient_matrix_UB_21      0.0042830000
_diffrn_orient_matrix_UB_22      -0.0633522000
_diffrn_orient_matrix_UB_23      -0.0558157000
_diffrn_orient_matrix_UB_31      -0.1777434000
_diffrn_orient_matrix_UB_32      -0.0015434000
_diffrn_orient_matrix_UB_33      -0.0013062000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14789
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.395
_diffrn_reflns_theta_min         5.027
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24515
_exptl_absorpt_correction_type   multi-scan
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
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_exptl_crystal_density_diffrn    1.155
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 1986 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0344
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_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+0.6331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.0892
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_cod_data_source_file            ic6b02114_si_002.cif
_cod_data_source_block           compound7
_cod_database_code               4349219
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         'C1 H1 O1 N1 Si1 Mg1'
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_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C24(H24), C27(H27)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C15(H15), C19(H19), C20(H20), C21(H21)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
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 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
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_olex2_submission_special_instructions 'No special instructions were received'