Synthesis and Structure of 2,5-Bis[N-(2,6-mesityl)iminomethyl]pyrrolylcobalt(II): Evidence for One-Electron-Oxidized, Redox Noninnocent Ligand Behavior.
Peters, Garvin M.; Winegrad, Jacob B.; Gau, Michael R.; Imler, Gregory H.; Xu, Beibei; Ren, Shenqiang; Wayland, Bradford B.; Zdilla, Michael J.; Inorganic chemistry 56 (2017) 3377–3385; doi:10.1021/acs.inorgchem.6b02898

data_4345276
_publ_section_title
;
 Synthesis and Structure of
 2,5-Bis[N-(2,6-mesityl)iminomethyl]pyrrolylcobalt(II): Evidence for
 One-Electron-Oxidized, Redox Noninnocent Ligand Behavior.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3377
_journal_page_last               3385
_journal_paper_doi               10.1021/acs.inorgchem.6b02898
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C24 H27 N3'
_chemical_formula_sum            'C24 H27 N3'
_chemical_formula_weight         357.48
_chemical_name_systematic
;
(1E,1'E)-1,1'-(1H-pyrrole-2,5-diyl)bis(N-phenylmethanimine)
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-11-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_cell_angle_alpha                90
_cell_angle_beta                 118.462(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1829(14)
_cell_length_b                   34.929(6)
_cell_length_c                   8.2568(15)
_cell_measurement_reflns_used    1468
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.487
_cell_measurement_theta_min      2.866
_cell_volume                     2074.7(6)
_computing_cell_refinement       'SAINT (Bruker AXS)'
_computing_data_collection       'COSMO (Bruker AXS)'
_computing_data_reduction        'SADABS (Bruker AXS)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.02
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEX II DUO'
_diffrn_measurement_method       '\f \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0790
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11993
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.354
_diffrn_reflns_theta_min         2.332
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
12173 Corrected reflections written to file mo_1797_0m.hkl
 Estimated minimum and maximum transmission:  0.6604  0.7454
 The ratio of these values is more reliable than their absolute values!
 Additional spherical absorption correction applied with mu*r =  0.2000
 Lambda/2 correction factor = 0.0015
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_description       plate
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4232
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0499P)^2^+0.2847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1222
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2653
_reflns_number_total             4232
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02898_si_002.cif
_cod_data_source_block           Mes2pyrH
_cod_depositor_comments
'Adding full bibliography for 4345276--4345278.cif.'
_cod_database_code               4345276
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.987
_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 Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C20(H20), C18(H18), C1(H1), C9(H9), C11(H11)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C15(H15A,H15B,
 H15C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              16342
_shelx_hkl_checksum              98651
_olex2_submission_special_instructions 'No special instructions were received'