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_7707340
_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         'C30 H28 Fe N12 O6, 2(Cl O4), 2(C2 H3 N)'
_chemical_formula_sum            'C34 H34 Cl2 Fe N14 O14'
_chemical_formula_weight         989.50
_chemical_name_systematic
'Bis[(2,6-di{pyrazol-1-yl}pyridine-4-carbonyl)amino]propionic acid iron(II) diperchlorate bis-acetonitrile solvate ([Fe(L6)2][ClO4]2.2MeCN)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                78.756(3)
_cell_angle_beta                 84.199(2)
_cell_angle_gamma                79.817(2)
_cell_formula_units_Z            6
_cell_length_a                   13.6682(3)
_cell_length_b                   17.9378(5)
_cell_length_c                   26.8890(8)
_cell_measurement_reflns_used    11642
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      73.14
_cell_measurement_theta_min      4.43
_cell_volume                     6349.0(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      290(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.929
_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  0.0525
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            54085
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.869
_diffrn_reflns_theta_min         3.360
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.748
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.723
_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    1.553
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3048
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile/diethyl ether'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.865
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1733
_refine_ls_number_reflns         23886
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1460
_refine_ls_R_factor_gt           0.0984
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2777
_refine_ls_wR_factor_ref         0.3331
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13395
_reflns_number_total             23886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01076j2.cif
_cod_data_source_block           conea-rt
_cod_depositor_comments
'Adding full bibliography for 7707339--7707346.cif.'
_cod_database_code               7707340
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H49C of O49C, H25A of O25A, H25B of O25B, H49A of O49A,
  H25C of O25C, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H49B of O49B
2. Restrained distances
 Cl0A-O51A = Cl0A-O52A = Cl0A-O53A = Cl0A-O54A
 1.42089 with sigma of 0.02
 Cl0B-O51B = Cl0B-O52B = Cl0B-O53B = Cl0B-O54B
 1.42089 with sigma of 0.02
 O51A-O52A = O51A-O53A = O51A-O54A = O52A-O53A = O52A-O54A = O53A-O54A
 2.320313 with sigma of 0.02
 O51B-O52B = O51B-O53B = O51B-O54B = O52B-O53B = O52B-O54B = O53B-O54B
 2.320313 with sigma of 0.02
 Cl1A-O56A = Cl1A-O57A = Cl1A-O58A = Cl1A-O59A
 1.42089 with sigma of 0.02
 Cl1B-O56B = Cl1B-O57B = Cl1B-O58B = Cl1B-O59B
 1.42089 with sigma of 0.02
 O56A-O57A = O56A-O58A = O56A-O59A = O57A-O58A = O57A-O59A = O58A-O59A
 2.320313 with sigma of 0.02
 O56B-O57B = O56B-O58B = O56B-O59B = O57B-O58B = O57B-O59B = O58B-O59B
 2.320313 with sigma of 0.02
 Cl2A-O61A = Cl2A-O62A = Cl2A-O63A = Cl2A-O64A
 1.42089 with sigma of 0.02
 Cl2B-O61B = Cl2B-O62B = Cl2B-O63B = Cl2B-O64B
 1.42089 with sigma of 0.02
 O61A-O62A = O61A-O63A = O61A-O64A = O62A-O63A = O62A-O64A = O63A-O64A
 2.320313 with sigma of 0.02
 Cl3A-O66A = Cl3A-O67A = Cl3A-O68A = Cl3A-O69A
 1.42089 with sigma of 0.02
 Cl3B-O66B = Cl3B-O67B = Cl3B-O68B = Cl3B-O69B
 1.42089 with sigma of 0.02
 O66A-O67A = O66A-O68A = O66A-O69A = O67A-O68A = O67A-O69A = O68A-O69A
 2.320313 with sigma of 0.02
 O66B-O67B = O66B-O68B = O66B-O69B = O67B-O68B = O67B-O69B = O68B-O69B
 2.320313 with sigma of 0.02
 Cl4A-O71A = Cl4A-O72A = Cl4A-O73A = Cl4A-O74A
 1.42089 with sigma of 0.02
 Cl4B-O71B = Cl4B-O72B = Cl4B-O73B = Cl4B-O74B
 1.42089 with sigma of 0.02
 O71A-O72A = O71A-O73A = O71A-O74A = O72A-O73A = O72A-O74A = O73A-O74A
 2.320313 with sigma of 0.02
 O71B-O72B = O71B-O73B = O71B-O74B = O72B-O73B = O72B-O74B = O73B-O74B
 2.320313 with sigma of 0.02
 Cl5A-O76A = Cl5A-O77A = Cl5A-O78A = Cl5A-O79A
 1.42089 with sigma of 0.02
 Cl5B-O76B = Cl5B-O77B = Cl5B-O78B = Cl5B-O79B
 1.42089 with sigma of 0.02
 O76A-O77A = O76A-O78A = O76A-O79A = O77A-O78A = O77A-O79A = O78A-O79A
 2.320313 with sigma of 0.02
 O76B-O77B = O76B-O78B = O76B-O79B = O77B-O78B = O77B-O79B = O78B-O79B
 2.320313 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=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(DFIX)=1(DFIX)=1(DFIX)=
 1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: Cl0A(0.5) O51A(0.5) O52A(0.5) O53A(0.5) O54A(0.5) Cl0B(0.5)
 O51B(0.5) O52B(0.5) O53B(0.5) O54B(0.5) Cl1A(0.5) O56A(0.5) O57A(0.5)
 O58A(0.5) O59A(0.5) Cl1B(0.5) O56B(0.5) O57B(0.5) O58B(0.5) O59B(0.5)
 Cl2A(0.5) O61A(0.5) O62A(0.5) O63A(0.5) O64A(0.5) Cl2B(0.5) O61B(0.5)
 O62B(0.5) O63B(0.5) O64B(0.5) Cl3A(0.5) O66A(0.5) O67A(0.5) O68A(0.5)
 O69A(0.5) Cl3B(0.5) O66B(0.5) O67B(0.5) O68B(0.5) O69B(0.5) Cl4A(0.5)
 O71A(0.5) O72A(0.5) O73A(0.5) O74A(0.5) Cl4B(0.5) O71B(0.5) O72B(0.5)
 O73B(0.5) O74B(0.5) Cl5A(0.5) O76A(0.5) O77A(0.5) O78A(0.5) O79A(0.5)
 Cl5B(0.5) O76B(0.5) O77B(0.5) O78B(0.5) O79B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C21A(H21A,H21B), C22A(H22A,H22B), C45A(H45A,H45B), C46A(H46A,H46B), C21B(H21C,
 H21D), C22B(H22C,H22D), C45B(H45C,H45D), C46B(H46C,H46D), C21C(H21E,H21F),
 C22C(H22E,H22F), C45C(H45E,H45F), C46C(H46E,H46F)
4.b Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C6A(H6A), C10A(H10A), C11A(H11A), C12A(H12A), C15A(H15A),
 C16A(H16A), C17A(H17A), N20A(H20A), C28A(H28A), C30A(H30A), C34A(H34A),
 C35A(H35A), C36A(H36A), C39A(H39A), C40A(H40A), C41A(H41A), N44A(H44A),
 C4B(H4B), C6B(H6B), C10B(H10B), C11B(H11B), C12B(H12B), C15B(H15B), C16B(H16B),
  C17B(H17B), N20B(H20B), C28B(H28B), C30B(H30B), C34B(H34B), C35B(H35B),
 C36B(H36B), C39B(H39B), C40B(H40B), C41B(H41B), N44B(H44B), C4C(H4C), C6C(H6C),
  C10C(H10C), C11C(H11C), C12C(H12C), C15C(H15C), C16C(H16C), C17C(H17C),
 N20C(H20C), C28C(H28C), C30C(H30C), C34C(H34C), C35C(H35C), C36C(H36C),
 C39C(H39C), C40C(H40C), C41C(H41C), N44C(H44C)
4.c Tetrahedral OH refined with riding coordinates:
 O25A(H25A), O49A(H49A), O25B(H25B), O49B(H49B), O25C(H25C), O49C(H49C)
4.d Idealised Me refined as rotating group:
 C80(H80A,H80B,H80C), C83(H83A,H83B,H83C), C86(H86A,H86B,H86C), C89(H89A,H89B,
 H89C), C92(H92A,H92B,H92C), C95(H95A,H95B,H95C)
;
_shelx_res_checksum              1286
_olex2_submission_special_instructions 'No special instructions were received'