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_7707346
_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'
_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             2021-04-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-04-30 deposited with the CCDC.	2021-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                78.877(2)
_cell_angle_beta                 83.742(2)
_cell_angle_gamma                78.844(2)
_cell_formula_units_Z            6
_cell_length_a                   13.6232(3)
_cell_length_b                   17.8150(3)
_cell_length_c                   26.3257(4)
_cell_measurement_reflns_used    23498
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.19
_cell_measurement_theta_min      3.80
_cell_volume                     6133.6(2)
_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_temperature      120.15
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            52042
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.555
_diffrn_reflns_theta_min         3.432
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.914
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.966
_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_colour_primary    red
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_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         1.121
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1814
_refine_ls_number_reflns         23091
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0665P)^2^+11.6813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20222
_reflns_number_total             23091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01076j2.cif
_cod_data_source_block           conea-fe
_cod_depositor_comments
'Adding full bibliography for 7707339--7707346.cif.'
_cod_database_code               7707346
_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 C(H,H,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
 C5B-C18B
 1.51 with sigma of 0.02
 C21B-C22B
 1.51 with sigma of 0.02
 C22B-C23B
 1.51 with sigma of 0.02
 C18B-O19B
 1.22 with sigma of 0.02
 C23B-O24B
 1.22 with sigma of 0.02
 C23B-O25B
 1.28 with sigma of 0.02
 C18B-N20B
 1.3 with sigma of 0.02
 N20B-C21B
 1.46 with sigma of 0.02
 O24B-O25B
 2.2 with sigma of 0.02
 O19B-N20B
 2.26 with sigma of 0.02
 C5B-C18D
 1.51 with sigma of 0.02
 C21D-C22D
 1.51 with sigma of 0.02
 C22D-C23D
 1.51 with sigma of 0.02
 C18D-O19D
 1.22 with sigma of 0.02
 C23D-O24D
 1.22 with sigma of 0.02
 C23D-O25D
 1.28 with sigma of 0.02
 C18D-N20D
 1.3 with sigma of 0.02
 N20D-C21D
 1.46 with sigma of 0.02
 O24D-O25D
 2.2 with sigma of 0.02
 O19D-N20D
 2.26 with sigma of 0.02
 C29B-C42B
 1.51 with sigma of 0.02
 C45B-C46B
 1.51 with sigma of 0.02
 C42B-O43B
 1.22 with sigma of 0.02
 C47B-O48B
 1.22 with sigma of 0.02
 C47B-O49B
 1.28 with sigma of 0.02
 C42B-N44B
 1.3 with sigma of 0.02
 N44B-C45B
 1.46 with sigma of 0.02
 O48B-O49B
 2.2 with sigma of 0.02
 O43B-N44B
 2.26 with sigma of 0.02
 C29B-C42D
 1.51 with sigma of 0.02
 C45D-C46B
 1.51 with sigma of 0.02
 C42D-O43D
 1.22 with sigma of 0.02
 C47B-O48D
 1.22 with sigma of 0.02
 C47B-O49D
 1.28 with sigma of 0.02
 C42D-N44D
 1.3 with sigma of 0.02
 N44D-C45D
 1.46 with sigma of 0.02
 O48D-O49D
 2.2 with sigma of 0.02
 O43D-N44D
 2.26 with sigma of 0.02
 Cl5A-O56A
 1.43598 with sigma of 0.02
 Cl5A-O57A
 1.43598 with sigma of 0.02
 Cl5A-O58A
 1.43598 with sigma of 0.02
 Cl5A-O59A
 1.43598 with sigma of 0.02
 Cl5B-O56B
 1.43598 with sigma of 0.02
 Cl5B-O57B
 1.43598 with sigma of 0.02
 Cl5B-O58B
 1.43598 with sigma of 0.02
 Cl5B-O59B
 1.43598 with sigma of 0.02
 O56A-O57A
 2.344955 with sigma of 0.02
 O56A-O58A
 2.344955 with sigma of 0.02
 O56A-O59A
 2.344955 with sigma of 0.02
 O57A-O58A
 2.344955 with sigma of 0.02
 O57A-O59A
 2.344955 with sigma of 0.02
 O58A-O59A
 2.344955 with sigma of 0.02
 O56B-O57B
 2.344955 with sigma of 0.02
 O56B-O58B
 2.344955 with sigma of 0.02
 O56B-O59B
 2.344955 with sigma of 0.02
 O57B-O58B
 2.344955 with sigma of 0.02
 O57B-O59B
 2.344955 with sigma of 0.02
 O58B-O59B
 2.344955 with sigma of 0.02
 Cl7A-O76A
 1.43598 with sigma of 0.02
 Cl7A-O77A
 1.43598 with sigma of 0.02
 Cl7A-O78A
 1.43598 with sigma of 0.02
 Cl7A-O79A
 1.43598 with sigma of 0.02
 Cl7B-O76B
 1.43598 with sigma of 0.02
 Cl7B-O77B
 1.43598 with sigma of 0.02
 Cl7B-O78B
 1.43598 with sigma of 0.02
 Cl7B-O79B
 1.43598 with sigma of 0.02
 O76A-O77A
 2.344955 with sigma of 0.02
 O76A-O78A
 2.344955 with sigma of 0.02
 O76A-O79A
 2.344955 with sigma of 0.02
 O77A-O78A
 2.344955 with sigma of 0.02
 O77A-O79A
 2.344955 with sigma of 0.02
 O78A-O79A
 2.344955 with sigma of 0.02
 O76B-O77B
 2.344955 with sigma of 0.02
 O76B-O78B
 2.344955 with sigma of 0.02
 O76B-O79B
 2.344955 with sigma of 0.02
 O77B-O78B
 2.344955 with sigma of 0.02
 O77B-O79B
 2.344955 with sigma of 0.02
 O78B-O79B
 2.344955 with sigma of 0.02
 O43D-O72
 -3 with sigma of 0.005
 O43D-N82_$10
 -3 with sigma of 0.005
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)=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(DFIX)=1(DFIX)=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: C18B(0.7) O19B(0.7) N20B(0.7) H20B(0.7) C21B(0.7) H21A(0.7)
 H21B(0.7) C22B(0.7) H22A(0.7) H22B(0.7) C23B(0.7) O24B(0.7) O25B(0.7)
 H25B(0.7) C18D(0.3) O19D(0.3) N20D(0.3) H20D(0.3) C21D(0.3) H21C(0.3)
 H21D(0.3) C22D(0.3) H22C(0.3) H22D(0.3) C23D(0.3) O24D(0.3) O25D(0.3)
 H25D(0.3) C42B(0.84) O43B(0.84) N44B(0.84) H44B(0.84) C45B(0.84) H45A(0.84)
 H45B(0.84) H46A(0.84) H46B(0.84) H46C(0.16) H46D(0.16) C42D(0.16) O43D(0.16)
 N44D(0.16) H44D(0.16) C45D(0.16) H45C(0.16) H45D(0.16) O48B(0.84) O49B(0.84)
 H49B(0.84) O48D(0.16) O49D(0.16) H49D(0.16) Cl5A(0.67) O56A(0.67) O57A(0.67)
 O58A(0.67) O59A(0.67) Cl5B(0.33) O56B(0.33) O57B(0.33) O58B(0.33) O59B(0.33)
 Cl7A(0.67) O76A(0.67) O77A(0.67) O78A(0.67) O79A(0.67) Cl7B(0.33) O76B(0.33)
 O77B(0.33) O78B(0.33) O79B(0.33)
4.a Secondary CH2 refined with riding coordinates:
 C21A(H21E,H21F), C22A(H22E,H22F), C45A(H45E,H45F), C46A(H46E,H46F), C21B(H21A,
 H21B), C22B(H22A,H22B), C21D(H21C,H21D), C22D(H22C,H22D), C45B(H45A,H45B),
 C46B(H46A,H46B), C46B(H46C,H46D), C45D(H45C,H45D), C21C(H21G,H21H), C22C(H22G,
 H22H), C45C(H45G,H45H), C46C(H46G,H46H)
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), N20D(H20D), C28B(H28B), C30B(H30B), C34B(H34B),
 C35B(H35B), C36B(H36B), C39B(H39B), C40B(H40B), C41B(H41B), N44B(H44B),
 N44D(H44D), 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), O25D(H25D), O49B(H49B), O49D(H49D),
 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              14746
_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
;