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_7707345
_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             2020-07-28
_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                 95.073(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8756(4)
_cell_length_b                   16.2798(7)
_cell_length_c                   17.2477(10)
_cell_measurement_reflns_used    3863
_cell_measurement_temperature    330(2)
_cell_measurement_theta_max      72.56
_cell_measurement_theta_min      4.16
_cell_volume                     3880.9(3)
_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      330(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.857
_diffrn_measured_fraction_theta_max 0.840
_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  0.0234
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.857
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11526
_diffrn_reflns_point_group_measured_fraction_full 0.857
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.635
_diffrn_reflns_theta_min         3.741
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.123
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.542
_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    1.575
_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         0.478
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         6591
_refine_ls_number_restraints     181
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0755
_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^)+(0.1387P)^2^+2.0117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2188
_refine_ls_wR_factor_ref         0.2527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4326
_reflns_number_total             6591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01076j2.cif
_cod_data_source_block           conma-ht
_cod_depositor_comments
'Adding full bibliography for 7707339--7707346.cif.'
_cod_database_code               7707345
_shelx_shelxl_version_number     2018/3
_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
 Cl4A-O49A = Cl4A-O50A = Cl4A-O51A = Cl4A-O52A
 1.44322 with sigma of 0.02
 Cl4B-O49B = Cl4B-O50B = Cl4B-O51B = Cl4B-O52B
 1.44322 with sigma of 0.02
 Cl4C-O49C = Cl4C-O50C = Cl4C-O51C = Cl4C-O52C
 1.44322 with sigma of 0.02
 O49A-O50A = O49A-O51A = O49A-O52A = O50A-O51A = O50A-O52A = O51A-O52A
 2.356778 with sigma of 0.02
 O49B-O50B = O49B-O51B = O49B-O52B = O50B-O51B = O50B-O52B = O51B-O52B
 2.356778 with sigma of 0.02
 O49C-O50C = O49C-O51C = O49C-O52C = O50C-O51C = O50C-O52C = O51C-O52C
 2.356778 with sigma of 0.02
 Cl5A-O54A = Cl5A-O55A = Cl5A-O56A = Cl5A-O57A
 1.44322 with sigma of 0.02
 Cl5B-O54B = Cl5B-O55B = Cl5B-O56B = Cl5B-O57B
 1.44322 with sigma of 0.02
 Cl5C-O54C = Cl5C-O55C = Cl5C-O56C = Cl5C-O57C
 1.44322 with sigma of 0.02
 O54A-O55A = O54A-O56A = O54A-O57A = O55A-O56A = O55A-O57A = O56A-O57A
 2.356778 with sigma of 0.02
 O54B-O55B = O54B-O56B = O54B-O57B = O55B-O56B = O55B-O57B = O56B-O57B
 2.356778 with sigma of 0.02
 O54C-O55C = O54C-O56C = O54C-O57C = O55C-O56C = O55C-O57C = O56C-O57C
 2.356778 with sigma of 0.02
 C41-O42A = C41-O42B
 1.22 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl4A \\sim O49A \\sim O50A \\sim O51A \\sim O52A \\sim Cl4B \\sim O49B \\sim
O50B \\sim O51B \\sim O52B \\sim Cl4C \\sim O49C \\sim O50C \\sim O51C \\sim
O52C: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
Cl5A \\sim O54A \\sim O55A \\sim O56A \\sim O57A \\sim Cl5B \\sim O54B \\sim
O55B \\sim O56B \\sim O57B \\sim Cl5C \\sim O54C \\sim O55C \\sim O56C \\sim
O57C: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
4. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: O42A(0.67) O42B(0.33) Cl4A(0.34) O49A(0.34) O50A(0.34) O51A(0.34)
 O52A(0.34) Cl4B(0.33) O49B(0.33) O50B(0.33) O51B(0.33) O52B(0.33) Cl4C(0.33)
 O49C(0.33) O50C(0.33) O51C(0.33) O52C(0.33) Cl5A(0.34) O54A(0.34) O55A(0.34)
 O56A(0.34) O57A(0.34) Cl5B(0.33) O54B(0.33) O55B(0.33) O56B(0.33) O57B(0.33)
 Cl5C(0.33) O54C(0.33) O55C(0.33) O56C(0.33) O57C(0.33)
5.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C44(H44A,H44B)
5.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)
5.c Tetrahedral OH refined with riding coordinates:
 O24(H24), O47(H47)
5.d Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C)
;
_shelx_res_checksum              16645
_olex2_submission_special_instructions 'No special instructions were received'