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_7714086
_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         'C38 H26 Fe N10, 2(B F4), 1.5(C H4 O)'
_chemical_formula_sum            'C39.5 H32 B2 F8 Fe N10 O1.5'
_chemical_formula_weight         900.22
_chemical_name_systematic
'Bis[2,6-Bis(imidazo[1,2-a]pyridin-2-yl)pyridine]iron(II)ditetrafluoroborate methanol (1.5/1.41) solvate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.2181(6)
_cell_length_b                   12.4550(2)
_cell_length_c                   12.9419(3)
_cell_measurement_reflns_used    5458
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.62
_cell_measurement_theta_min      4.90
_cell_volume                     4064.94(15)
_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 0.988
_diffrn_measured_fraction_theta_max 0.975
_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  0.0282
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10785
_diffrn_reflns_point_group_measured_fraction_full 0.751
_diffrn_reflns_point_group_measured_fraction_max 0.737
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.650
_diffrn_reflns_theta_min         3.505
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.722
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.750
_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_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1836
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol/diethyl ether'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.106
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.498(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         6058
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0995P)^2^+1.8975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1451
_reflns_Friedel_coverage         0.445
_reflns_Friedel_fraction_full    0.490
_reflns_Friedel_fraction_max     0.476
_reflns_number_gt                5723
_reflns_number_total             6058
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02747c2.cif
_cod_data_source_block           146ameoh
_cod_original_formula_sum        'C39.50 H32 B2 F8 Fe N10 O1.50'
_cod_database_code               7714086
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.502(7)
 0.498(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C60A-O61A = C60B-O61B = C62A-O63A = C62B-O63B
 1.42206 with sigma of 0.01
4. Others
 Fixed Sof: C60A(0.5) H60A(0.5) H60B(0.5) H60C(0.5) O61A(0.5) H61A(0.5)
 C62A(0.35) H62A(0.35) H62B(0.35) H62C(0.35) O63A(0.35) H63A(0.35) C60B(0.35)
 H60D(0.35) H60E(0.35) H60F(0.35) O61B(0.35) H61B(0.35) C62B(0.3) H62D(0.3)
 H62E(0.3) H62F(0.3) O63B(0.3) H63B(0.3)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16),
 C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C28(H28), C29(H29), C30(H30),
  C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C44(H44), C45(H45),
 C46(H46), C47(H47), C49(H49)
5.b Idealised Me refined as rotating group:
 C60A(H60A,H60B,H60C), C62A(H62A,H62B,H62C), C60B(H60D,H60E,H60F), C62B(H62D,
 H62E,H62F)
5.c Idealised tetrahedral OH refined as rotating group:
 O61A(H61A), O63A(H63A), O61B(H61B), O63B(H63B)
;
_shelx_res_checksum              98377
_olex2_submission_special_instructions 'No special instructions were received'