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_7714088
_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), 0.8(C H3 N O2)'
_chemical_formula_sum            'C38.8 H28.4 B2 F8 Fe N10.8 O1.6'
_chemical_formula_weight         900.99
_chemical_name_systematic
'Bis[2,6-Bis(imidazo[1,2-a]pyridin-2-yl)pyridine]iron(II)ditetrafluoroborate nitromethane (1/0.8) solvate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-07-26
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_audit_update_record
;
2023-09-27 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                   12.3988(5)
_cell_length_b                   12.9182(4)
_cell_length_c                   25.2840(9)
_cell_measurement_reflns_used    4303
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      73.79
_cell_measurement_theta_min      4.88
_cell_volume                     4049.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_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_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            10459
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.777
_diffrn_reflns_theta_min         3.496
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.746
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1830
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: nitromethane/diethyl ether'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         3990
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0594
_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^)+(0.1116P)^2^+1.4224P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1644
_refine_ls_wR_factor_ref         0.1826
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3034
_reflns_number_total             3990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02747c2.cif
_cod_data_source_block           rk146a_r
_cod_original_formula_sum        'C38.80 H28.40 B2 F8 Fe N10.80 O1.60'
_cod_database_code               7714088
_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. Restrained distances
 C34A-N35A = C34B-N35B
 1.45 with sigma of 0.02
 N35A-O36A = N35A-O37A = N35B-O36B = N35B-O37B
 1.22 with sigma of 0.02
 O36A-O37A = O36B-O37B
 2.09 with sigma of 0.02
 C34A-O36A = C34A-O37A = C34B-O36B = C34B-O37B
 2.3 with sigma of 0.02
3. Others
 Fixed Sof: B29(0.5) F30(0.5) F31(0.5) F32(0.5) C34A(0.25) H34D(0.25)
 H34E(0.25) H34F(0.25) N35A(0.25) O36A(0.25) O37A(0.25) C34B(0.15) H34A(0.15)
 H34B(0.15) H34C(0.15) N35B(0.15) O36B(0.15) O37B(0.15)
4.a Me refined with riding coordinates:
 C34A(H34D,H34E,H34F), C34B(H34A,H34B,H34C)
4.b 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)
;
_shelx_res_checksum              67
_olex2_submission_special_instructions 'No special instructions were received'