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_7714091
_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
'C34 H22 Fe N14, 2(B F4), 3.5(C H3 N O2), 0.5(C4 H10 O)'
_chemical_formula_sum            'C39.5 H37.5 B2 F8 Fe N17.5 O7.5'
_chemical_formula_weight         1106.84
_chemical_name_systematic
'Bis[2,6-Bis(imidazo[1,2-a]pyrimidin-2-yl)pyridine]iron(II)ditetrafluoroborate nitromethane/diethyl ether solvate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-07-27
_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                80.455(4)
_cell_angle_beta                 89.884(4)
_cell_angle_gamma                76.630(4)
_cell_formula_units_Z            2
_cell_length_a                   12.6361(6)
_cell_length_b                   13.4938(7)
_cell_length_c                   14.3473(7)
_cell_measurement_reflns_used    6232
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.29
_cell_measurement_theta_min      4.33
_cell_volume                     2345.4(2)
_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 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0460
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16691
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.072
_diffrn_reflns_theta_max         67.072
_diffrn_reflns_theta_min         3.126
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.492
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.604
_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            brown
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1130
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: nitromethane/diethyl ether'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         8101
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0748
_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^)+(0.1224P)^2^+3.2194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1985
_refine_ls_wR_factor_ref         0.2122
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6694
_reflns_number_total             8101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02747c2.cif
_cod_data_source_block           rk172c
_cod_original_formula_sum        'C39.50 H37.50 B2 F8 Fe N17.50 O7.50'
_cod_database_code               7714091
_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
 C64B-C65B = C67B-C68B
 1.54 with sigma of 0.02
 C65B-O66B = O66B-C67B
 1.43 with sigma of 0.02
 C65B-C67B
 2.34 with sigma of 0.02
 C64B-O66B = O66B-C68B
 2.42 with sigma of 0.02
 C64A-N65A
 1.45 with sigma of 0.02
 N65A-O66A = N65A-O67A
 1.22 with sigma of 0.02
 O66A-O67A
 2.09 with sigma of 0.02
 C64A-O66A = C64A-O67A
 2.3 with sigma of 0.02
 C69A-N70A = C69B-N70B = C69C-N70B
 1.45 with sigma of 0.02
 N70A-O71A = N70A-O72A = N70B-O71B = N70B-O72B = N70B-O71C = N70B-O72C
 1.22 with sigma of 0.02
 O71A-O72A = O71B-O72B = O71C-O72C
 2.09 with sigma of 0.02
 C69A-O71A = C69A-O72A = C69B-O71B = C69B-O72B = C69C-O71C = C69C-O72C
 2.3 with sigma of 0.02
 C73A-N74A = C73B-N74B = C73C-N74B
 1.45 with sigma of 0.02
 N74A-O75A = N74A-O76A = N74B-O75B = N74B-O76B = N74B-O75C = N74B-O76C
 1.22 with sigma of 0.02
 O75A-O76A = O75B-O76B = O75C-O76C
 2.09 with sigma of 0.02
 C73A-O75A = C73A-O76A = C73B-O75B = C73B-O76B = C73C-O75C = C73C-O76C
 2.3 with sigma of 0.02
 B50A-F51A = B50A-F52A = B50A-F53A = B50A-F54A
 1.37956 with sigma of 0.02
 B50B-F51B = B50B-F52B = B50B-F53B = B50B-F54B
 1.37956 with sigma of 0.02
 B50C-F51C = B50C-F52C = B50C-F53C = B50C-F54C
 1.37956 with sigma of 0.02
 F51A-F52A = F51A-F53A = F51A-F54A = F52A-F53A = F52A-F54A = F53A-F54A
 2.252821 with sigma of 0.02
 F51B-F52B = F51B-F53B = F51B-F54B = F52B-F53B = F52B-F54B = F53B-F54B
 2.252821 with sigma of 0.02
 F51C-F52C = F51C-F53C = F51C-F54C = F52C-F53C = F52C-F54C = F53C-F54C
 2.252821 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: B50A(0.4) F51A(0.4) F52A(0.4) F53A(0.4) F54A(0.4) B50B(0.4)
 F51B(0.4) F52B(0.4) F53B(0.4) F54B(0.4) B50C(0.2) F51C(0.2) F52C(0.2)
 F53C(0.2) F54C(0.2) C64A(0.5) H64D(0.5) H64E(0.5) H64F(0.5) N65A(0.5)
 O66A(0.5) O67A(0.5) H64A(0.5) H64B(0.5) H64C(0.5) C65B(0.5) H65A(0.5)
 H65B(0.5) O66B(0.5) C67B(0.5) H67A(0.5) H67B(0.5) C68B(0.5) H68A(0.5)
 H68B(0.5) H68C(0.5) C69A(0.5) H69A(0.5) H69B(0.5) H69C(0.5) N70A(0.5)
 O71A(0.5) O72A(0.5) N70B(0.5) C69B(0.4) H69D(0.4) H69E(0.4) H69F(0.4)
 O71B(0.4) O72B(0.4) C69C(0.1) H69G(0.1) H69H(0.1) H69I(0.1) O71C(0.1)
 O72C(0.1) C73A(0.5) H73A(0.5) H73B(0.5) H73C(0.5) N74A(0.5) O75A(0.5)
 O76A(0.5) N74B(0.5) C73B(0.4) H73D(0.4) H73E(0.4) H73F(0.4) O75B(0.4)
 O76B(0.4) C73C(0.1) H73G(0.1) H73H(0.1) H73I(0.1) O75C(0.1) O76C(0.1)
4.a Secondary CH2 refined with riding coordinates:
 C65B(H65A,H65B), C67B(H67A,H67B)
4.b Me refined with riding coordinates:
 C64A(H64D,H64E,H64F), C64B(H64A,H64B,H64C), C68B(H68A,H68B,H68C), C69A(H69A,
 H69B,H69C), C69B(H69D,H69E,H69F), C69C(H69G,H69H,H69I), C73A(H73A,H73B,H73C),
 C73B(H73D,H73E,H73F), C73C(H73G,H73H,H73I)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C12(H12), C13(H13), C14(H14), C16(H16), C21(H21),
 C22(H22), C23(H23), C25(H25), C28(H28), C29(H29), C30(H30), C36(H36), C37(H37),
  C38(H38), C40(H40), C45(H45), C46(H46), C47(H47), C49(H49)
4.d Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C)
;
_shelx_res_checksum              16904
_olex2_submission_special_instructions 'No special instructions were received'