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_4349218
_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_formula_moiety
'C66 H98 Mg2 N4 O2 S2, C66 H100 Mg2 N4 O2 S2 '
_chemical_formula_sum            'C132 H198 Mg4 N8 O4 S4'
_chemical_formula_weight         2186.46
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-06-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 117.4980(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   24.5406(3)
_cell_length_b                   13.96620(10)
_cell_length_c                   23.0002(2)
_cell_measurement_reflns_used    30795
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.5530
_cell_measurement_theta_min      4.7830
_cell_volume                     6992.49(13)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  "'SuperNova, Dual, Cu at zero, EosS2"
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            52199
_diffrn_reflns_theta_full        71.61
_diffrn_reflns_theta_max         71.61
_diffrn_reflns_theta_min         4.36
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.170
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30160
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_density_diffrn    1.039
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.394
_refine_diff_density_min         -1.070
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         13385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0716
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1107P)^2^+8.5462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1938
_refine_ls_wR_factor_ref         0.2004
_reflns_number_gt                11981
_reflns_number_total             13385
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02114_si_002.cif
_cod_data_source_block           compound6
_cod_original_cell_volume        6992.49(12)
_cod_database_code               4349218
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C73) = Uanis(C72) = Uanis(C71)
3. Others
 Fixed Sof: C8A(0.5) H8A1(0.5) H8A2(0.5) H8A3(0.5) C9A(0.5) H9A(0.5) C10A(0.5)
 H10A(0.5) H10B(0.5) H10C(0.5) C8B(0.5) H8B1(0.5) H8B2(0.5) H8B3(0.5) C9B(0.5)
 H9B(0.5) C10B(0.5) H10D(0.5) H10E(0.5) H10F(0.5) C63A(0.5) H63A(0.5) H63B(0.5)
 H63C(0.5) C67A(0.5) H67A(0.5) H67B(0.5) H67C(0.5) C67B(0.5) H67D(0.5)
 H67E(0.5) H67F(0.5) C63B(0.5) H63D(0.5) H63E(0.5) H63F(0.5)
 Fixed Uiso: H3(0.08) H5(0.08) H8A1(0.08) H8A2(0.08) H8A3(0.08) H10A(0.08)
 H10B(0.08) H10C(0.08) H8B1(0.08) H8B2(0.08) H8B3(0.08) H10D(0.08) H10E(0.08)
 H10F(0.08) H11A(0.08) H11B(0.08) H12A(0.08) H12B(0.08) H14A(0.08) H14B(0.08)
 H14C(0.08) H15A(0.08) H15B(0.08) H17A(0.08) H17B(0.08) H17C(0.08) H20(0.08)
 H21(0.08) H22(0.08) H28A(0.08) H28B(0.08) H28C(0.08) H29A(0.08) H29B(0.08)
 H29C(0.08) H30A(0.08) H30B(0.08) H33A(0.08) H33B(0.08) H36(0.08) H37(0.08)
 H38(0.08) H41A(0.08) H41B(0.08) H41C(0.08) H42A(0.08) H42B(0.08) H42C(0.08)
 H44A(0.08) H44B(0.08) H44C(0.08) H45A(0.08) H45B(0.08) H45C(0.08) H47A(0.08)
 H47B(0.08) H47C(0.08) H48A(0.08) H48B(0.08) H50A(0.08) H50B(0.08) H50C(0.08)
 H53(0.08) H54(0.08) H55(0.08) H58A(0.08) H58B(0.08) H58C(0.08) H61A(0.08)
 H61B(0.08) H61C(0.08) H62A(0.08) H62B(0.08) H62C(0.08) H64A(0.08) H64B(0.08)
 H65A(0.08) H65B(0.08) H68(0.08) H70A(0.08) H70B(0.08) H72A(0.08) H72B(0.08)
 H72C(0.08) H74A(0.08) H74B(0.08) H69A(0.08) H69B(0.08) H69C(0.08) H63A(0.08)
 H63B(0.08) H63C(0.08) H67A(0.08) H67B(0.08) H67C(0.08) H67D(0.08) H67E(0.08)
 H67F(0.08) H63D(0.08) H63E(0.08) H63F(0.08)
4.a Ternary CH refined with everything fixed:
 C9A(H9A), C9B(H9B), C27(H27), C40(H40), C43(H43), C57(H57), C60(H60), C71(H71)
4.b Secondary CH2 refined with everything fixed:
 C11(H11A,H11B), C12(H12A,H12B), C15(H15A,H15B), C30(H30A,H30B), C33(H33A,
 H33B), C48(H48A,H48B), C64(H64A,H64B), C65(H65A,H65B), C70(H70A,H70B),
 C74(H74A,H74B)
4.c Me refined with everything fixed:
 C8A(H8A1,H8A2,H8A3), C10A(H10A,H10B,H10C), C8B(H8B1,H8B2,H8B3), C10B(H10D,
 H10E,H10F), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C28(H28A,H28B,H28C),
 C29(H29A,H29B,H29C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C50(H50A,H50B,H50C), C58(H58A,
 H58B,H58C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C72(H72A,H72B,H72C),
 C73(H73A,H73B,H73C), C69(H69A,H69B,H69C), C63A(H63A,H63B,H63C), C67A(H67A,H67B,
 H67C), C67B(H67D,H67E,H67F), C63B(H63D,H63E,H63F)
4.d Aromatic/amide H refined with everything fixed:
 C3(H3), C5(H5), C20(H20), C21(H21), C22(H22), C36(H36), C37(H37), C38(H38),
 C53(H53), C54(H54), C55(H55), C68(H68)
;
_olex2_submission_special_instructions 'No special instructions were received'