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_7714092
_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), 1.5(C2 H3 N)'
_chemical_formula_sum            'C37 H26.5 B2 F8 Fe N15.5'
_chemical_formula_weight         917.71
_chemical_name_systematic
'Bis[2,6-Bis(imidazo[1,2-a]pyrimidin-2-yl)pyridine]iron(II)ditetrafluoroborate sesqui-acetonitrile 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                101.726(4)
_cell_angle_beta                 102.485(3)
_cell_angle_gamma                118.470(4)
_cell_formula_units_Z            2
_cell_length_a                   13.0255(5)
_cell_length_b                   13.5032(6)
_cell_length_c                   13.7441(6)
_cell_measurement_reflns_used    7283
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      72.76
_cell_measurement_theta_min      3.53
_cell_volume                     1938.19(19)
_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(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.932
_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  0.0412
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15897
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.820
_diffrn_reflns_theta_min         3.526
_exptl_absorpt_coefficient_mu    3.931
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.717
_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            'dark red'
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             930
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile/diethyl ether'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         7308
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0877P)^2^+1.0071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1538
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6433
_reflns_number_total             7308
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02747c2.cif
_cod_data_source_block           rk172me
_cod_original_cell_volume        1938.19(16)
_cod_original_formula_sum        'C37 H26.50 B2 F8 Fe N15.50'
_cod_database_code               7714092
_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
 B55A-F56A = B55A-F57A = B55A-F58A = B55A-F59A
 1.38935 with sigma of 0.02
 B55B-F56B = B55B-F57B = B55B-F58B = B55B-F59B
 1.38935 with sigma of 0.02
 F56A-F57A = F56A-F58A = F56A-F59A = F57A-F58A = F57A-F59A = F58A-F59A
 2.268809 with sigma of 0.02
 F56B-F57B = F56B-F58B = F56B-F59B = F57B-F58B = F57B-F59B = F58B-F59B
 2.268809 with sigma of 0.02
 C63-C64
 1.48 with sigma of 0.02
 C64-N65
 1.15 with sigma of 0.02
 C63-N65
 2.63 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: B55A(0.57) F56A(0.57) F57A(0.57) F58A(0.57) F59A(0.57) B55B(0.43)
 F56B(0.43) F57B(0.43) F58B(0.43) F59B(0.43) C63(0.5) H63A(0.5) H63B(0.5)
 H63C(0.5) C64(0.5) N65(0.5)
4.a 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.b Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C63(H63A,H63B,H63C)
;
_shelx_res_checksum              86137
_olex2_submission_special_instructions 'No special instructions were received'