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_4349577
_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        none
_chemical_formula_moiety         '2(C30 H38 Fe N6 O4), 4(B F4)'
_chemical_formula_sum            'C60 H76 B4 F16 Fe2 N12 O8'
_chemical_formula_weight         1552.26
_chemical_name_common            1(BF4)
_chemical_name_systematic        1(BF4)-LP
_chemical_properties_physical    ', Moisture-sensitive'
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-09-28 deposited with the CCDC.
2016-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.184(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6930(5)
_cell_length_b                   19.5154(7)
_cell_length_c                   24.9934(11)
_cell_measurement_reflns_used    16106
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.1620
_cell_measurement_theta_min      2.8490
_cell_volume                     6674.0(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.40t (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.40t (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.40t (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13091
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.921
_diffrn_reflns_theta_min         2.873
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.440
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Higashi, T. (1995).'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_description       block
_exptl_crystal_F_000             3200
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.33
_refine_diff_density_max         3.074
_refine_diff_density_min         -1.096
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     955
_refine_ls_number_reflns         13091
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.1298
_refine_ls_R_factor_gt           0.1187
_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^)+(0.1426P)^2^+57.9062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3433
_refine_ls_wR_factor_ref         0.3517
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10986
_reflns_number_total             13091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qi00417b2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4349577
_shelx_estimated_absorpt_t_max   1.767
_shelx_estimated_absorpt_t_min   0.546
_exptl_absorpt_special_details   SADABS
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.540(5) 0.460(5)
2. 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
3. Restrained distances
 B4-F13 \\sim B4-F14 \\sim B4-F15A \\sim B4-F15B \\sim B4-F16A \\sim B4-F16B
 with sigma of 0.01
 F13-F14 \\sim F13-F15A \\sim F13-F16A \\sim F14-F15A \\sim F14-F16A \\sim
F15A-F16A
 with sigma of 0.02
 F13-F14 \\sim F13-F15B \\sim F13-F16B \\sim F14-F15B \\sim F14-F16B \\sim
F15B-F16B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(F15A) \\sim Ueq, Uanis(F15B) \\sim Ueq, Uanis(F16A) \\sim Ueq,
Uanis(F16B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(F15B)=Sof(F16B)=1-FVAR(1)
 Sof(F15A)=Sof(F16A)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C12(H12A,H12B), C19(H19A,H19B), C27(H27A,H27B), C34(H34A,H34B),
 C42(H42A,H42B), C49(H49A,H49B), C57(H57A,H57B)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C22(H22), C23(H23), C24(H24), C37(H37), C38(H38),
 C39(H39), C52(H52), C53(H53), C54(H54)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C59(H59A,H59B,H59C),
 C60(H60A,H60B,H60C)
;
_shelx_res_checksum              32139
_shelx_hkl_checksum              54290
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'