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_7714089
_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, 1.6(B F4), 0.2(F6 Si), 1.7(C H3 N O2), 0.3(C4 H10 O)'
_chemical_formula_sum            'C40.9 H34.1 B1.6 F7.6 Fe N11.7 O3.7 Si0.2'
_chemical_formula_weight         971.86
_chemical_name_systematic
'Bis[2,6-Bis(imidazo[1,2-a]pyridin-2-yl)pyridine]iron(II)tetrafluoroborate (2/1.6) hexafluorosilicate (1/0.2) 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             2023-09-26
_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                79.861(2)
_cell_angle_beta                 78.387(3)
_cell_angle_gamma                64.173(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7520(4)
_cell_length_b                   13.6771(4)
_cell_length_c                   13.9688(4)
_cell_measurement_reflns_used    8866
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      73.80
_cell_measurement_theta_min      3.62
_cell_volume                     2137.25(12)
_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_temperature      120.15
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_details
;
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0667407000
_diffrn_orient_matrix_UB_12      -0.0654294000
_diffrn_orient_matrix_UB_13      -0.0151906000
_diffrn_orient_matrix_UB_21      0.0953565000
_diffrn_orient_matrix_UB_22      -0.0511807000
_diffrn_orient_matrix_UB_23      -0.0858415000
_diffrn_orient_matrix_UB_31      0.0694990000
_diffrn_orient_matrix_UB_32      -0.0944333000
_diffrn_orient_matrix_UB_33      0.0721505000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16955
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.906
_diffrn_reflns_theta_min         3.246
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.677
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.711
_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            black
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             992
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: nitromethane/diethyl ether'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.626
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         8110
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0705
_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^)+(0.1346P)^2^+1.8479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1912
_refine_ls_wR_factor_ref         0.1999
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7287
_reflns_number_total             8110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02747c2.cif
_cod_data_source_block           rk146alt
_cod_original_formula_sum
'C40.90 H34.10 B1.60 F7.60 Fe N11.70 O3.70 Si0.20'
_cod_database_code               7714089
_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
 B50A-F51A
 1.38 with sigma of 0.02
 B50A-F52A
 1.38 with sigma of 0.02
 B50A-F53A
 1.38 with sigma of 0.02
 B50A-F54A
 1.38 with sigma of 0.02
 F51A-F52A
 2.25 with sigma of 0.02
 F51A-F53A
 2.25 with sigma of 0.02
 F51A-F54A
 2.25 with sigma of 0.02
 F52A-F53A
 2.25 with sigma of 0.02
 F52A-F54A
 2.25 with sigma of 0.02
 F53A-F54A
 2.25 with sigma of 0.02
 B50A-F51B
 1.38 with sigma of 0.02
 B50A-F52B
 1.38 with sigma of 0.02
 B50A-F53B
 1.38 with sigma of 0.02
 B50A-F54B
 1.38 with sigma of 0.02
 F51B-F52B
 2.25 with sigma of 0.02
 F51B-F53B
 2.25 with sigma of 0.02
 F51B-F54B
 2.25 with sigma of 0.02
 F52B-F53B
 2.25 with sigma of 0.02
 F52B-F54B
 2.25 with sigma of 0.02
 F53B-F54B
 2.25 with sigma of 0.02
 Si5C-F51C
 1.56 with sigma of 0.02
 Si5C-F52C
 1.56 with sigma of 0.02
 Si5C-F53C
 1.56 with sigma of 0.02
 Si5C-F54C
 1.56 with sigma of 0.02
 Si5C-F55C
 1.56 with sigma of 0.02
 Si5C-F56C
 1.56 with sigma of 0.02
 F51C-F52C
 2.21 with sigma of 0.02
 F52C-F53C
 2.21 with sigma of 0.02
 F53C-F54C
 2.21 with sigma of 0.02
 F51C-F54C
 2.21 with sigma of 0.02
 F51C-F55C
 2.21 with sigma of 0.02
 F52C-F55C
 2.21 with sigma of 0.02
 F53C-F55C
 2.21 with sigma of 0.02
 F54C-F55C
 2.21 with sigma of 0.02
 F51C-F56C
 2.21 with sigma of 0.02
 F52C-F56C
 2.21 with sigma of 0.02
 F53C-F56C
 2.21 with sigma of 0.02
 F54C-F56C
 2.21 with sigma of 0.02
 C66A-N67A
 1.45 with sigma of 0.02
 C66B-N67B
 1.45 with sigma of 0.02
 N67A-O68A
 1.22 with sigma of 0.02
 N67A-O69A
 1.22 with sigma of 0.02
 N67B-O68B
 1.22 with sigma of 0.02
 N67B-O69B
 1.22 with sigma of 0.02
 O68A-O69A
 2.09 with sigma of 0.02
 O68B-O69B
 2.09 with sigma of 0.02
 C66A-O68A
 2.3 with sigma of 0.02
 C66A-O69A
 2.3 with sigma of 0.02
 C66B-O68B
 2.3 with sigma of 0.02
 C66B-O69B
 2.3 with sigma of 0.02
 C66C-C67C
 1.52 with sigma of 0.02
 C67C-O68C
 1.43 with sigma of 0.02
 O68C-C69C
 1.43 with sigma of 0.02
 C69C-C70C
 1.52 with sigma of 0.02
 C66C-O68C
 2.42 with sigma of 0.02
 C67C-C69C
 2.34 with sigma of 0.02
 O68C-C70C
 2.42 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C66A \\sim N67A \\sim O68A \\sim O69A: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2A
C66B \\sim N67B \\sim O68B \\sim O69B: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2A
C66C \\sim C67C \\sim O68C \\sim C69C \\sim C70C: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 2A
B50A \\sim F51A \\sim F52A \\sim F53A \\sim F54A \\sim F51B \\sim F52B \\sim
F53B \\sim F54B: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.01 within 2A
Si5C \\sim F51C \\sim F52C \\sim F53C \\sim F54C \\sim F55C \\sim F56C: within
2A with sigma of 0.002 and sigma for terminal atoms of 0.01 within 2A
4. Others
 Fixed Sof: B50A(0.6) F51A(0.3) F52A(0.3) F53A(0.3) F54A(0.3) F51B(0.3)
 F52B(0.3) F53B(0.3) F54B(0.3) Si5C(0.2) F51C(0.2) F52C(0.2) F53C(0.2)
 F54C(0.2) F55C(0.2) F56C(0.2) C66A(0.55) H66D(0.55) H66E(0.55) H66F(0.55)
 N67A(0.55) O68A(0.55) O69A(0.55) C66B(0.15) H66G(0.15) H66H(0.15) H66I(0.15)
 N67B(0.15) O68B(0.15) O69B(0.15) C66C(0.3) H66A(0.3) H66B(0.3) H66C(0.3)
 C67C(0.3) H67A(0.3) H67B(0.3) O68C(0.3) C69C(0.3) H69A(0.3) H69B(0.3)
 C70C(0.3) H70A(0.3) H70B(0.3) H70C(0.3)
5.a Secondary CH2 refined with riding coordinates:
 C67C(H67A,H67B), C69C(H69A,H69B)
5.b Me refined with riding coordinates:
 C66A(H66D,H66E,H66F), C66B(H66G,H66H,H66I), C66C(H66A,H66B,H66C), C70C(H70A,
 H70B,H70C)
5.c 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.d Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C)
;
_shelx_res_checksum              60515
_olex2_submission_special_instructions 'No special instructions were received'