Spin transitions in a series of [Fe(pybox)2]2+ complexes modulated by ligand structures, counter anions, and solvents
Zhu, Yuan-Yuan; Li, Hong-Qing; Ding, Zhong-Yu; Lü, Xiao-Jin; Zhao, Liang; Meng, Yin-Shan; Liu, Tao; Gao, Song; Inorganic Chemistry Frontiers 3 (2016) 1624–; doi:10.1039/C6QI00417B

data_4349576
_publ_section_title
;
 Spin transitions in a series of [Fe(pybox)2]2+ complexes modulated by
 ligand structures, counter anions, and solvents
;
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1624
_journal_paper_doi               10.1039/C6QI00417B
_journal_volume                  3
_journal_year                    2016
_chemical_compound_source        no
_chemical_formula_moiety         'C24 H20 B, 2(C5.5 H5.5 Fe0.25 N1.5 O)'
_chemical_formula_sum            'C35 H31 B Fe0.5 N3 O2'
_chemical_formula_weight         564.36
_chemical_name_common            8-3
_chemical_name_systematic        8-3
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-03-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-03-16 deposited with the CCDC.
2016-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   17.6175(3)
_cell_length_b                   17.6175(3)
_cell_length_c                   37.7194(10)
_cell_measurement_reflns_used    17606
_cell_measurement_temperature    300.00(10)
_cell_measurement_theta_max      24.1550
_cell_measurement_theta_min      3.4900
_cell_volume                     11707.2(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      300.00(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega    4.00   73.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628 -128.0000   55.1197 69

  2 omega   -1.00   87.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628   77.0000  -60.0000 88

  3 omega    9.00   92.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628   77.0000 -180.0000 83

  4 omega  -57.00   41.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628  -57.0000 -180.0000 98

  5 omega  -20.00   54.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628   77.0000   90.0000 74

  6 omega  -62.00   43.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628  -77.0000  -60.0000 105

  7 omega  -55.00   47.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628  -77.0000   90.0000 102

  8 omega  -76.00  -50.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  131.0000  118.1645 26
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0375454000
_diffrn_orient_matrix_UB_12      0.0085646000
_diffrn_orient_matrix_UB_13      -0.0054656000
_diffrn_orient_matrix_UB_21      -0.0135853000
_diffrn_orient_matrix_UB_22      -0.0094849000
_diffrn_orient_matrix_UB_23      0.0171373000
_diffrn_orient_matrix_UB_31      0.0050618000
_diffrn_orient_matrix_UB_32      0.0381842000
_diffrn_orient_matrix_UB_33      0.0054789000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            86298
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.005
_diffrn_reflns_theta_min         2.937
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4736
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         5738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0476P)^2^+8.9124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1202
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3953
_reflns_number_total             5738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qi00417b2.cif
_cod_data_source_block           8-3
_cod_original_cell_volume        11707.2(5)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'C35 H31 B Fe0.50 N3 O2'
_cod_database_code               4349576
_chemical_oxdiff_formula         'c43 h54 n6 B1 Fe1'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C7(H7A,H7B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
  C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C5(H5), C6(H6), C11(H11),
 C12(H12)
;
_shelx_res_checksum              2900
_shelx_hkl_checksum              41944
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method acetonitrile/ether