Ferrous and ferric complexes with cyclometalating N-heterocyclic carbene ligands: a case of dual emission revisited.
Johnson, Catherine Ellen; Schwarz, Jesper; Deegbey, Mawuli; Prakash, Om; Sharma, Kumkum; Huang, Ping; Ericsson, Tore; Häggström, Lennart; Bendix, Jesper; Gupta, Arvind Kumar; Jakubikova, Elena; Wärnmark, Kenneth; Lomoth, Reiner; Chemical science 14 (2023) 10129–10139; doi:10.1039/d3sc02806b

data_1569741
_publ_section_title
;
 Ferrous and ferric complexes with cyclometalating N-heterocyclic carbene
 ligands: a case of dual emission revisited.
;
_journal_issue                   37
_journal_name_full               'Chemical science'
_journal_page_first              10129
_journal_page_last               10139
_journal_paper_doi               10.1039/d3sc02806b
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C28 H22 Fe N8'
_chemical_formula_sum            'C28 H22 Fe N8'
_chemical_formula_weight         526.38
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-04-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-04-05 deposited with the CCDC.	2023-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.36140(10)
_cell_length_b                   8.36140(10)
_cell_length_c                   18.0048(6)
_cell_measurement_reflns_used    3055
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.7560
_cell_measurement_theta_min      4.0990
_cell_volume                     1258.77(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13245
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.404
_diffrn_reflns_theta_min         3.446
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       plate
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.375
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.162
_refine_ls_abs_structure_details
;
 Flack x determined using 558 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.469(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1592
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0893
_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^)+(0.1312P)^2^+12.0033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2242
_refine_ls_wR_factor_ref         0.2463
_reflns_Friedel_coverage         0.871
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.884
_reflns_number_gt                1356
_reflns_number_total             1592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02806b2.cif
_cod_data_source_block           FeIICAB-2CM
_cod_depositor_comments
'Adding full bibliography for 1569741--1569742.cif.'
_cod_database_code               1569741
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.843
_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. Restrained distances
 C4-N1 \\sim C4-N2
 with sigma of 0.002
 C3-N2 \\sim C2-N1
 with sigma of 0.002
3. Restrained planarity
 N2, C3, C2, N1, C4
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N2) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.01
Uanis(C8) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 Fe1, C6, N1, N2, C5, C3, C2, C7, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6, C5, C7, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C2(H2), C7(H7)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_smtbx_masks_void_probe_radius   0.0
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              84408
_shelx_fab_checksum              61006
_olex2_submission_special_instructions 'No special instructions were received'