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_4349570
_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         'C22 H22 Fe N6 O4, 2(Cl O4)'
_chemical_formula_sum            'C22 H22 Cl2 Fe N6 O12'
_chemical_formula_weight         689.20
_chemical_name_common            5
_chemical_name_systematic        5
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-11
_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                 103.31(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.386(3)
_cell_length_b                   10.700(2)
_cell_length_c                   16.934(3)
_cell_measurement_reflns_used    8809
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4849
_cell_measurement_theta_min      1.2356
_cell_volume                     2713.0(9)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_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
;
????
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 270.0000
	             XTD: 39.9087
	          2theta: -20.0080
scan:
	Number of images: 180
	           Slice: -110.0000 - -20.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 39.9087
	          2theta: -20.0080
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0619
_diffrn_orient_matrix_UB_12      -0.0041
_diffrn_orient_matrix_UB_13      -0.0249
_diffrn_orient_matrix_UB_21      -0.0328
_diffrn_orient_matrix_UB_22      -0.0211
_diffrn_orient_matrix_UB_23      0.0850
_diffrn_orient_matrix_UB_31      -0.0212
_diffrn_orient_matrix_UB_32      0.0566
_diffrn_orient_matrix_UB_33      0.0059
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17804
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.487
_diffrn_reflns_theta_min         1.613
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5755
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_primary    'dark red'
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.175
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6190
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0332P)^2^+2.7994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1227
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5410
_reflns_number_total             6190
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qi00417b2.cif
_cod_data_source_block           5
_cod_original_cell_volume        2713.2(10)
_cod_database_code               4349570
_diffrn_number_total             6525
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O9B-O10B = O9B-O11B = O9B-O12B = O10B-O11B = O10B-O12B = O11B-O12B
 2.35 with sigma of 0.02
 O9A-O10A = O9A-O11A = O9A-O12A = O10A-O11A = O10A-O12A = O11A-O12A
 2.35 with sigma of 0.02
 Cl2-O9A = Cl2-O10A = Cl2-O11A = Cl2-O12A = Cl2-O9B = Cl2-O10B = Cl2-O11B
 1.44 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O9B) \\sim Ueq, Uanis(O10B) \\sim Ueq, Uanis(O11B) \\sim Ueq, Uanis(O12B)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O9A) \\sim Ueq, Uanis(O10A) \\sim Ueq, Uanis(O11A) \\sim Ueq, Uanis(O12A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(O9B)=Sof(O10B)=Sof(O11B)=Sof(O12B)=1-FVAR(1)
 Sof(O9A)=Sof(O10A)=Sof(O11A)=Sof(O12A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C21(H21A,H21B), C22(H22A,H22B)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C16(H16), C17(H17), C18(H18)
;
_shelx_res_checksum              79862
_shelx_hkl_checksum              4256
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method acetonitrile/ether