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_4345277
_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 H26 Cl2 Co N3'
_chemical_formula_weight         486.31
_chemical_name_systematic
;
dichloro(1E,1'E)-1,1'-(1H-pyrrolyl-2,5-diyl)bis(N-phenylmethanimine)cobalt(II)
dichloromethane solvate
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_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                 108.344(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.453(2)
_cell_length_b                   11.3132(17)
_cell_length_c                   15.240(2)
_cell_measurement_reflns_used    9227
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      2.29
_cell_volume                     2692.6(6)
_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      100.02
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_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  0.0321
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18378
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.017
_diffrn_reflns_theta_min         2.223
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.849
_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    1.200
_exptl_crystal_description       plate
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
Disordered solvent removed by squeeze was consistent with two dichloromethane
molecules per unit cell (84 electrons) or 0.5 DCM per formula unit. The composition 
is also consistent with CHN elemental analysis which fit best with 0.4 DCM per
formula unit.
;
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         6463
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0609
_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^)+(0.0137P)^2^+6.3685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1290
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5080
_reflns_number_total             6463
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02898_si_002.cif
_cod_data_source_block           CoMes2pyrCl2.0.5DCM
_cod_depositor_comments
'Adding full bibliography for 4345276--4345278.cif.'
_cod_original_cell_volume        2692.6(7)
_cod_database_code               4345277
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.728
_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
 Cl1, Cl1A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl1A: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.005
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:
 C6(H6), C3(H3), C4(H4), C1(H1), C15(H15), C13(H13), C35(H35), C33(H33)
5.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C37(H37A,H37B,
 H37C), C39(H39A,H39B,H39C), C38(H38A,H38B,H38C)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              34271
_shelx_hkl_checksum              37265
_shelx_fab_checksum              51818
_olex2_submission_special_instructions 'No special instructions were received'