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_4349568
_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(C24 H20 B)'
_chemical_formula_sum            'C78 H78 B2 Fe N6 O4'
_chemical_formula_weight         1240.93
_chemical_name_common            4-1
_chemical_name_systematic        4-1
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-03-16 deposited with the CCDC.
2016-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.454(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.3002(4)
_cell_length_b                   13.24618(16)
_cell_length_c                   24.3060(4)
_cell_measurement_reflns_used    10115
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      73.6520
_cell_measurement_theta_min      3.3070
_cell_volume                     6828.8(2)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
  1 omega  -46.00    1.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7931   38.0000  120.0000 47

  2 omega -119.00   -3.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7931  -19.0000   90.0000 116

  3 omega   23.00   68.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       40.7931 -125.0000   90.0000 45

  4 omega   39.00   94.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       40.7931 -125.0000  -60.0000 55

  5 omega   29.00   77.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3775  -30.0000   90.0000 48

  6 omega   33.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3775  -45.0000  -90.0000 65

  7 omega   84.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3775   77.0000   30.0000 94

  8 omega  102.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3775   77.0000    0.0000 76

  9 omega   68.00   96.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3775  -45.0000  -60.0000 28

 10 omega   71.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3775  -94.0000 -150.0000 35

 11 omega  111.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3775   61.0000  -30.0000 67

 12 omega  153.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3775   68.0000   53.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0034195000
_diffrn_orient_matrix_UB_12      -0.0880667000
_diffrn_orient_matrix_UB_13      -0.0399985000
_diffrn_orient_matrix_UB_21      -0.0685643000
_diffrn_orient_matrix_UB_22      0.0208449000
_diffrn_orient_matrix_UB_23      -0.0447816000
_diffrn_orient_matrix_UB_31      0.0237343000
_diffrn_orient_matrix_UB_32      0.0730993000
_diffrn_orient_matrix_UB_33      -0.0352540000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27190
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.127
_diffrn_reflns_theta_min         3.889
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.191
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77540
_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    1.207
_exptl_crystal_description       block
_exptl_crystal_F_000             2624
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
The disordered solvent molecules cannot be modeled and were treated 
by SQUEEZE,PLATON.
There are total 78e per unit cell, which are accumulated which corresponds 
to 19.5e per formula(C78H78B2FeN6O4). The 19.5e might come from one 
ether molecule and are not included in the formula.
;
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.038
_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     828
_refine_ls_number_reflns         13256
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+1.0789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10991
_reflns_number_total             13256
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qi00417b2.cif
_cod_data_source_block           4-1
_cod_database_code               4349568
_chemical_oxdiff_formula         'C84 H93 Fe1 B2 N7 O2'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C12(H12A,H12B), C19(H19A,H19B), C27(H27A,H27B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C22(H22), C23(H23), C24(H24), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51),
 C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60),
  C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68),
 C69(H69), C70(H70), C71(H71), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78)
2.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              86006
_shelx_hkl_checksum              22738
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method acetonitrile/ether