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_1569742
_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 H26 Fe N8, F6 P'
_chemical_formula_sum            'C28 H26 F6 Fe N8 P'
_chemical_formula_weight         675.39
_chemical_name_systematic        FeIIICAB-2CM-150K
_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     dual
_audit_creation_date             2023-04-27
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-04-27 deposited with the CCDC.	2023-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.186(2)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   23.1820(6)
_cell_length_b                   19.7134(3)
_cell_length_c                   20.7973(4)
_cell_measurement_reflns_used    16790
_cell_measurement_temperature    150
_cell_measurement_theta_max      23.5330
_cell_measurement_theta_min      3.5640
_cell_volume                     9290.1(3)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_device_type  'Agilent Enhance'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1003
_diffrn_reflns_av_unetI/netI     0.1082
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            148479
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.562
_diffrn_reflns_theta_min         3.325
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'metallic bluish violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       block
_exptl_crystal_F_000             4140
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.010
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1201
_refine_ls_number_reflns         22767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0706P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11895
_reflns_number_total             22767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02806b2.cif
_cod_data_source_block           FeIIICAB-2CM_150
_cod_depositor_comments
'Adding full bibliography for 1569741--1569742.cif.'
_cod_database_code               1569742
_shelx_shelxl_version_number     2018/3
_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), C03G(H03G), C4(H4), C5(H5), C8(H8), C9(H9), C12(H12), C13(H13),
 C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C26(H26), C27(H27), C31(H31),
  C32(H32), C33(H33), C35(H35), C36(H36), C39(H39), C40(H40), C45(H45),
 C46(H46), C47(H47), C50(H50), C51(H51), C55(H55), C56(H56), C59(H59), C60(H60),
  C61(H61), C63(H63), C64(H64), C67(H67), C68(H68), C73(H73), C75(H75),
 C76(H76), C77(H77), C81(H81), C82(H82)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C28(H28A,H28B,
 H28C), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C), C52(H52A,H52B,H52C), C54(H54A,
 H54B,H54C), C65(H65A,H65B,H65C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C),
 C80(H80A,H80B,H80C)
;
_smtbx_masks_void_probe_radius   0.6
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              92680
_shelx_fab_checksum              90030
_olex2_submission_special_instructions 'No special instructions were received'