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_4345278
_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 H26 Cl2 Co N3'
_chemical_formula_sum            'C24 H27 Cl2 Co N3'
_chemical_formula_weight         487.31
_chemical_name_systematic
;
dichloro(1E,1'E)-1,1'-(1H-pyrrolyl-2,5-diyl)bis(N-phenylmethanimine)cobalt(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-11-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.5572(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.2416(14)
_cell_length_b                   14.4875(9)
_cell_length_c                   16.1470(11)
_cell_measurement_reflns_used    9227
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      2.29
_cell_volume                     4737.6(5)
_computing_cell_refinement       'SAINT V8.32B (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.32B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.03
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26149
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.857
_diffrn_reflns_theta_min         1.728
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.966
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0640 before and 0.0510 after correction.
The Ratio of minimum to maximum transmission is 0.7779.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       prism
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         5621
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0288P)^2^+7.8148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0715
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5207
_reflns_number_total             5621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02898_si_002.cif
_cod_data_source_block           CoMes2pyrCl2
_cod_depositor_comments
'Adding full bibliography for 4345276--4345278.cif.'
_cod_database_code               4345278
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.901
_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. Rigid bond restraints
 Cl2, Cl2A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
Cl2 \\sim Cl2A: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.002
4. Others
 Sof(Co1A)=Sof(Cl1A)=Sof(Cl2A)=1-FVAR(1)
 Sof(Co1)=Sof(Cl1)=Sof(Cl2)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C15(H15), C13(H13), C3(H3), C4(H4), C35(H35), C33(H33), C6(H6)
5.b Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              61144
_shelx_hkl_checksum              99055
_olex2_submission_special_instructions 'No special instructions were received'