The effect of tether groups on the spin states of iron(II)/bis[2,6-di(pyrazol-1-yl)pyridine] complexes.
Capel Berdiell, Izar; García-López, Victor; Howard, Mark J.; Clemente-León, Miguel; Halcrow, Malcolm A.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 7417–7426; doi:10.1039/d1dt01076j

data_7707341
_publ_section_title
;
 The effect of tether groups on the spin states of
 iron(II)/bis[2,6-di(pyrazol-1-yl)pyridine] complexes.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7417
_journal_page_last               7426
_journal_paper_doi               10.1039/d1dt01076j
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C28 H24 Fe N12 O6, 2(Cl O4), C2 H3 N'
_chemical_formula_sum            'C30 H27 Cl2 Fe N13 O14'
_chemical_formula_weight         920.39
_chemical_name_systematic
'Bis[(2,6-di{pyrazol-1-yl}pyridine-4-carbonyl)amino]acetic acid iron(II) diperchlorate acetonitrile solvate ([Fe(L5)2][ClO4]2.MeCN)'
_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
_audit_creation_date             2020-07-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.16 svn.r6f6c53a7 for OlexSys, GUI svn.r6139)
;
_audit_update_record
;
2021-03-30 deposited with the CCDC.	2021-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.0283(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7327(2)
_cell_length_b                   16.1080(2)
_cell_length_c                   16.7324(3)
_cell_measurement_reflns_used    6246
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.38
_cell_measurement_theta_min      3.83
_cell_volume                     3692.17(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14682
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.452
_diffrn_reflns_theta_min         3.814
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.384
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1880
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile/diethyl ether'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.569
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         7220
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0684
_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^)+(0.1345P)^2^+3.7570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1966
_refine_ls_wR_factor_ref         0.2082
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6171
_reflns_number_total             7220
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01076j2.cif
_cod_data_source_block           conma-fe
_cod_depositor_comments
'Adding full bibliography for 7707339--7707346.cif.'
_cod_original_cell_volume        3692.16(9)
_cod_database_code               7707341
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl48-O49A = Cl48-O50A = Cl48-O51A = Cl48-O52A
 1.43287 with sigma of 0.02
 Cl48-O49B = Cl48-O50B = Cl48-O51B = Cl48-O52B
 1.43287 with sigma of 0.02
 O49A-O50A = O49A-O51A = O49A-O52A = O50A-O51A = O50A-O52A = O51A-O52A
 2.339877 with sigma of 0.02
 O49B-O50B = O49B-O51B = O49B-O52B = O50B-O51B = O50B-O52B = O51B-O52B
 2.339877 with sigma of 0.02
 Cl5A-O54A = Cl5A-O55A = Cl5A-O56A = Cl5A-O57A
 1.43287 with sigma of 0.02
 Cl5B-O54B = Cl5B-O55B = Cl5B-O56B = Cl5B-O57B
 1.43287 with sigma of 0.02
 O54A-O55A = O54A-O56A = O54A-O57A = O55A-O56A = O55A-O57A = O56A-O57A
 2.339877 with sigma of 0.02
 O54B-O55B = O54B-O56B = O54B-O57B = O55B-O56B = O55B-O57B = O56B-O57B
 2.339877 with sigma of 0.02
 O42-O54B_$3
 -2.9 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: O49A(0.9) O50A(0.9) O51A(0.9) O52A(0.9) O49B(0.1) O50B(0.1)
 O51B(0.1) O52B(0.1) Cl5A(0.87) O54A(0.87) O55A(0.87) O56A(0.87) O57A(0.87)
 Cl5B(0.13) O54B(0.13) O55B(0.13) O56B(0.13) O57B(0.13)
4.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C44(H44A,H44B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 N20(H20), C27(H27), C29(H29), C33(H33), C34(H34), C35(H35), C38(H38), C39(H39),
  C40(H40), N43(H43)
4.c Tetrahedral OH refined with riding coordinates:
 O24(H24), O47(H47)
4.d Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C)
;
_shelx_res_checksum              69133
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.602
_oxdiff_exptl_absorpt_empirical_full_min 0.682