Iron(II) Complexes of 2,6-Bis(imidazo[1,2‑a]pyridin-2-yl)pyridine and Related Ligands with Annelated Distal Heterocyclic Donors
Kulmaczewski, Rafal; Halcrow, Malcolm; Dalton Transactions  (2023) –; doi:10.1039/D3DT02747C

data_7714093
_publ_section_title
;
 Iron(II) Complexes of 2,6-Bis(imidazo[1,2&#x2011;a]pyridin-2-yl)pyridine
 and Related Ligands with Annelated Distal Heterocyclic Donors
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02747C
_journal_year                    2023
_chemical_formula_moiety
'C46 H30 Fe N6, 2(B F4), 1.39(C2 H3 N), 0.125(C4 H10 O), 0.25(H2 O)'
_chemical_formula_sum            'C49.28 H35.93 B2 F8 Fe N7.39 O0.38'
_chemical_formula_weight         967.16
_chemical_name_systematic
'Bis[2,6-bis(quinolin-2-yl)pyridine]iron(II) ditetrafluoroborateacetonitrile diethyl ether hydrate 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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-08-11
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_audit_update_record
;
2023-08-15 deposited with the CCDC.	2023-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.963(2)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   18.9083(3)
_cell_length_b                   48.0111(9)
_cell_length_c                   20.0833(3)
_cell_measurement_reflns_used    15426
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.24
_cell_measurement_theta_min      3.29
_cell_volume                     18188.2(5)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120.15
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_k_min       -57
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            71868
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        71.996
_diffrn_reflns_theta_max         71.996
_diffrn_reflns_theta_min         3.452
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.335
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             7910
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile/diethyl ether'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.946
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2412
_refine_ls_number_reflns         35207
_refine_ls_number_restraints     107
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1441
_refine_ls_R_factor_gt           0.1128
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1306P)^2^+54.1432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2885
_refine_ls_wR_factor_ref         0.3062
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24981
_reflns_number_total             35207
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02747c2.cif
_cod_data_source_block           rk178
_cod_database_code               7714093
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B59-F60A = B59-F61A = B59-F62A = B59-F63A
 1.38489 with sigma of 0.02
 B59-F60B = B59-F61B = B59-F62B = B59-F63B
 1.38489 with sigma of 0.02
 B59-F60C = B59-F61C = B59-F62C = B59-F63C
 1.38489 with sigma of 0.02
 F60A-F61A = F60A-F62A = F60A-F63A = F61A-F62A = F61A-F63A = F62A-F63A
 2.261525 with sigma of 0.02
 F60B-F61B = F60B-F62B = F60B-F63B = F61B-F62B = F61B-F63B = F62B-F63B
 2.261525 with sigma of 0.02
 F60C-F61C = F60C-F62C = F60C-F63C = F61C-F62C = F61C-F63C = F62C-F63C
 2.261525 with sigma of 0.02
 B69A-F70 = B69A-F71A = B69A-F72A = B69A-F73A
 1.38489 with sigma of 0.02
 B69B-F70 = B69B-F71B = B69B-F72B = B69B-F73B
 1.38489 with sigma of 0.02
 F70-F71A = F70-F72A = F70-F73A = F71A-F72A = F71A-F73A = F72A-F73A
 2.261525 with sigma of 0.02
 F70-F71B = F70-F72B = F70-F73B = F71B-F72B = F71B-F73B = F72B-F73B
 2.261525 with sigma of 0.02
 B74A-F75A = B74A-F76A = B74A-F77A = B74A-F78A
 1.38489 with sigma of 0.02
 B74A-F75B = B74A-F76B = B74A-F77B = B74A-F78B
 1.38489 with sigma of 0.02
 B74C-F75C = B74C-F76C = B74C-F77C = B74C-F78C
 1.38489 with sigma of 0.02
 F75A-F76A = F75A-F77A = F75A-F78A = F76A-F77A = F76A-F78A = F77A-F78A
 2.261525 with sigma of 0.02
 F75B-F76B = F75B-F77B = F75B-F78B = F76B-F77B = F76B-F78B = F77B-F78B
 2.261525 with sigma of 0.02
 F75C-F76C = F75C-F77C = F75C-F78C = F76C-F77C = F76C-F78C = F77C-F78C
 2.261525 with sigma of 0.02
 C15E-C16E = C18E-C19E = C15F-C16F = C18F-C19F
 1.52 with sigma of 0.02
 C16E-O17E = O17E-C18E
 1.43 with sigma of 0.02
 C16E-C18E = C16F-C18F
 2.34 with sigma of 0.02
 C15E-O17E = O17E-C19E = C15F-O17F = O17F-C19F
 2.42 with sigma of 0.02
 C97A-C98A = C97B-C98B
 1.48 with sigma of 0.02
 C98A-N99A = C98B-N99B
 1.15 with sigma of 0.02
 C97A-N99A = C97B-N99B
 2.63 with sigma of 0.02
 C12E-C13E = C12F-C13F = C12G-C13G
 1.48 with sigma of 0.02
 C13E-N14E = C13F-N14F = C13G-N14G
 1.15 with sigma of 0.02
 C12E-N14E = C12F-N14F = C12G-N14G
 2.63 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: N28B(0.61) C29B(0.61) C30B(0.61) H30B(0.61) C31B(0.61) H31B(0.61)
 C32B(0.61) H32B(0.61) C33B(0.61) C34B(0.61) N35B(0.61) C36B(0.61) C37B(0.61)
 H37B(0.61) C38B(0.61) H38B(0.61) C39B(0.61) H39B(0.61) C40B(0.61) H40B(0.61)
 C41B(0.61) C42B(0.61) H42B(0.61) C43B(0.61) H43B(0.61) C44B(0.61) N45B(0.61)
 C46B(0.61) C47B(0.61) H47B(0.61) C48B(0.61) H48B(0.61) C49B(0.61) H49B(0.61)
 C50B(0.61) H50B(0.61) C51B(0.61) C52B(0.61) H52B(0.61) C53B(0.61) H53B(0.61)
 N28E(0.39) C29E(0.39) C30E(0.39) H30E(0.39) C31E(0.39) H31E(0.39) C32E(0.39)
 H32E(0.39) C33E(0.39) N35E(0.39) C34E(0.39) C43E(0.39) H43E(0.39) C42E(0.39)
 H42E(0.39) C41E(0.39) C36E(0.39) C37E(0.39) H37E(0.39) C38E(0.39) H38E(0.39)
 C39E(0.39) H39E(0.39) C40E(0.39) H40E(0.39) N45E(0.39) C44E(0.39) C53E(0.39)
 H53E(0.39) C52E(0.39) H52E(0.39) C51E(0.39) C46E(0.39) C47E(0.39) H47E(0.39)
 C48E(0.39) H48E(0.39) C49E(0.39) H49E(0.39) C50E(0.39) H50E(0.39) F60A(0.34)
 F61A(0.34) F62A(0.34) F63A(0.34) F60B(0.33) F61B(0.33) F62B(0.33) F63B(0.33)
 F60C(0.33) F61C(0.33) F62C(0.33) F63C(0.33) B69A(0.7) F71A(0.7) F72A(0.7)
 F73A(0.7) B69B(0.3) F71B(0.3) F72B(0.3) F73B(0.3) B74A(0.67) F75A(0.34)
 F76A(0.34) F77A(0.34) F78A(0.34) F76B(0.33) F75B(0.33) F77B(0.33) F78B(0.33)
 B74C(0.33) F75C(0.33) F76C(0.33) F77C(0.33) F78C(0.33) H94A(0.5) H94B(0.5)
 H94C(0.5) C95(0.5) N96(0.5) C97A(0.7) H97A(0.7) H97B(0.7) H97C(0.7) C98A(0.7)
 N99A(0.7) C97B(0.3) H97D(0.3) H97E(0.3) H97F(0.3) C98B(0.3) N99B(0.3)
 C100(0.8) H10A(0.8) H10B(0.8) H10C(0.8) C101(0.8) N102(0.8) C103(0.8)
 H10D(0.8) H10E(0.8) H10F(0.8) C104(0.8) N105(0.8) C106(0.8) H10G(0.8)
 H10H(0.8) H10I(0.8) C107(0.8) N108(0.8) C109(0.67) H10J(0.67) H10K(0.67)
 H10L(0.67) C110(0.67) N111(0.67) C12E(0.34) H12E(0.34) H12F(0.34) H12G(0.34)
 C13E(0.34) N14E(0.34) C12F(0.33) H12H(0.33) H12I(0.33) H12J(0.33) C13F(0.33)
 N14F(0.33) C12G(0.33) H12K(0.33) H12L(0.33) H12M(0.33) C13G(0.33) N14G(0.33)
 C15E(0.25) H15A(0.25) H15B(0.25) H15C(0.25) C16E(0.25) H16E(0.25) H16F(0.25)
 O17E(0.25) C18E(0.25) H18A(0.25) H18B(0.25) C19E(0.25) H19A(0.25) H19B(0.25)
 H19C(0.25) C15F(0.25) H15D(0.25) H15E(0.25) H15F(0.25) C16F(0.25) H16G(0.25)
 H16H(0.25) O17F(0.25) C18F(0.25) H18C(0.25) H18D(0.25) C19F(0.25) H19D(0.25)
 H19E(0.25) H19F(0.25) O120(0.75) O121(0.25)
4.a Secondary CH2 refined with riding coordinates:
 C16E(H16E,H16F), C18E(H18A,H18B), C16F(H16G,H16H), C18F(H18C,H18D)
4.b Me refined with riding coordinates:
 C15E(H15A,H15B,H15C), C15F(H15D,H15E,H15F)
4.c Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C5A(H5A), C6A(H6A), C11A(H11A), C12A(H12A), C13A(H13A), C14A(H14A),
 C16A(H16A), C17A(H17A), C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A),
 C26A(H26A), C27A(H27A), C30A(H30A), C31A(H31A), C32A(H32A), C37A(H37A),
 C38A(H38A), C39A(H39A), C40A(H40A), C42A(H42A), C43A(H43A), C47A(H47A),
 C48A(H48A), C49A(H49A), C50A(H50A), C52A(H52A), C53A(H53A), C4B(H4B), C5B(H5B),
  C6B(H6B), C11B(H11B), C12B(H12B), C13B(H13B), C14B(H14B), C16B(H16B),
 C17B(H17B), C21B(H21B), C22B(H22B), C23B(H23B), C24B(H24B), C26B(H26B),
 C27B(H27B), C30B(H30B), C31B(H31B), C32B(H32B), C37B(H37B), C38B(H38B),
 C39B(H39B), C40B(H40B), C42B(H42B), C43B(H43B), C47B(H47B), C48B(H48B),
 C49B(H49B), C50B(H50B), C52B(H52B), C53B(H53B), C30E(H30E), C31E(H31E),
 C32E(H32E), C43E(H43E), C42E(H42E), C37E(H37E), C38E(H38E), C39E(H39E),
 C40E(H40E), C53E(H53E), C52E(H52E), C47E(H47E), C48E(H48E), C49E(H49E),
 C50E(H50E), C4C(H4C), C5C(H5C), C6C(H6C), C11C(H11C), C12C(H12C), C13C(H13C),
 C14C(H14C), C16C(H16C), C17C(H17C), C21C(H21C), C22C(H22C), C23C(H23C),
 C24C(H24C), C26C(H26C), C27C(H27C), C30C(H30C), C31C(H31C), C32C(H32C),
 C37C(H37C), C38C(H38C), C39C(H39C), C40C(H40C), C42C(H42C), C43C(H43C),
 C47C(H47C), C48C(H48C), C49C(H49C), C50C(H50C), C52C(H52C), C53C(H53C),
 C4D(H4D), C5D(H5D), C6D(H6D), C11D(H11D), C12D(H12D), C13D(H13D), C14D(H14D),
 C16D(H16D), C17D(H17D), C21D(H21D), C22D(H22D), C23D(H23D), C24D(H24D),
 C26D(H26D), C27D(H27D), C30D(H30D), C31D(H31D), C32D(H32D), C37D(H37D),
 C38D(H38D), C39D(H39D), C40D(H40D), C42D(H42D), C43D(H43D), C47D(H47D),
 C48D(H48D), C49D(H49D), C50D(H50D), C52D(H52D), C53D(H53D)
4.d Naphthalene refined as free rotating group:
 N35E(C34E,C43E,C42E,C41E,C36E,C37E,C38E,C39E,C40E), N45E(C44E,C53E,C52E,C51E,
 C46E,C47E,C48E,C49E,C50E)
4.e Idealised Me refined as rotating group:
 C94(H94A,H94B,H94C), C97A(H97A,H97B,H97C), C97B(H97D,H97E,H97F), C100(H10A,
 H10B,H10C), C103(H10D,H10E,H10F), C106(H10G,H10H,H10I), C109(H10J,H10K,H10L),
 C12E(H12E,H12F,H12G), C12F(H12H,H12I,H12J), C12G(H12K,H12L,H12M), C19E(H19A,
 H19B,H19C), C19F(H19D,H19E,H19F)
;
_shelx_res_checksum              38330
_olex2_submission_special_instructions 'No special instructions were received'