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_4349565
_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         'C30 H38 Fe N6 O4, 2(B F4)'
_chemical_formula_sum            'C30 H38 B2 F8 Fe N6 O4'
_chemical_formula_weight         776.13
_chemical_name_common            2a
_chemical_name_systematic        2a
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-07-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_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            8
_cell_length_a                   13.6828(4)
_cell_length_b                   19.9361(6)
_cell_length_c                   25.5286(8)
_cell_measurement_reflns_used    16562
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      28.3000
_cell_measurement_theta_min      3.5000
_cell_volume                     6963.7(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      180.00(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_details
;
  1 omega  -60.00    6.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628  -38.0000  -30.0000 66

  2 omega  -51.00   79.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628    0.0000 -180.0000 130

  3 omega  -20.00    5.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  -99.0000 -150.0000 25

  4 omega  -20.00   18.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  -99.0000  -30.0000 38

  5 omega -103.00  -71.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  178.0000    0.0000 32

  6 omega  -20.00    6.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  -99.0000   60.0000 26

  7 omega -103.00  -71.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  178.0000  120.0000 32

  8 omega  -95.00  -62.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566 -178.0000   60.0000 33

  9 omega  -20.00   26.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  -99.0000 -120.0000 46
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0011298000
_diffrn_orient_matrix_UB_12      0.0355657000
_diffrn_orient_matrix_UB_13      0.0009430000
_diffrn_orient_matrix_UB_21      -0.0086222000
_diffrn_orient_matrix_UB_22      -0.0013181000
_diffrn_orient_matrix_UB_23      0.0273743000
_diffrn_orient_matrix_UB_31      0.0510883000
_diffrn_orient_matrix_UB_32      0.0005740000
_diffrn_orient_matrix_UB_33      0.0046380000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            76606
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.509
_diffrn_reflns_theta_min         2.990
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.521
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78931
_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    1.481
_exptl_crystal_description       block
_exptl_crystal_F_000             3200
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.885
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         9640
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0531
_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^)+(0.0552P)^2^+7.8990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1486
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6564
_reflns_number_total             9640
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qi00417b2.cif
_cod_data_source_block           2a
_cod_database_code               4349565
_chemical_oxdiff_formula         'c70 h100 fe1 b1 f4 n6 o6 '
_reflns_odcompleteness_completeness 99.73
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(F6B)=Sof(F7B)=Sof(F8B)=1-FVAR(1)
 Sof(F6A)=Sof(F7A)=Sof(F8A)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C12(H12A,H12B), C19(H19A,H19B), C27(H27A,H27B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C22(H22), C23(H23), C24(H24)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C)
;
_shelx_res_checksum              94254
_shelx_hkl_checksum              65205
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method methanol