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_7714087
_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         'C37 H27 Br Fe N7, Br, 0.5(H2 O)'
_chemical_formula_sum            'C37 H28 Br2 Fe N7 O0.5'
_chemical_formula_weight         794.33
_chemical_name_systematic
'Bromo[2,6-bis(imidazo[1,2\^a\/E?a]quinolin-2-yl)pyridine]bis(pyridine)iron(II)  bromide hemihydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 108.553(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8813(4)
_cell_length_b                   14.1735(4)
_cell_length_c                   19.6258(5)
_cell_measurement_reflns_used    5091
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.38
_cell_measurement_theta_min      3.90
_cell_volume                     3396.93(18)
_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 0.989
_diffrn_measured_fraction_theta_max 0.972
_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  0.0398
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14343
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.704
_diffrn_reflns_theta_min         3.619
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.630
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.817
_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 brown'
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1596
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 2,2,2-trifluoroethanol/pyridine'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         6680
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0893P)^2^+3.3533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1499
_refine_ls_wR_factor_ref         0.1639
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5235
_reflns_number_total             6680
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02747c2.cif
_cod_data_source_block           exp_1577
_cod_original_formula_sum        'C37 H28 Br2 Fe N7 O0.50'
_cod_database_code               7714087
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: Br7A(0.5) O1(0.5) Br7B(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16),
 C17(H17), C20(H20), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30),
  C33(H33), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42),
 C43(H43), C44(H44), C45(H45), C46(H46)
;
_shelx_res_checksum              9255
_olex2_submission_special_instructions 'No special instructions were received'