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_7707343
_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_absolute_configuration syn
_chemical_formula_moiety         'C20 H23 N5 O2 S2'
_chemical_formula_sum            'C20 H23 N5 O2 S2'
_chemical_formula_weight         429.55
_chemical_name_systematic
;
[2,6-di(pyrazol-1-yl)pyrid-4-yl]methyl (R)-lipoate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-04-28
_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                90
_cell_angle_beta                 105.394(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.6148(7)
_cell_length_b                   5.2928(1)
_cell_length_c                   20.9507(3)
_cell_measurement_reflns_used    5437
_cell_measurement_temperature    120.00(16)
_cell_measurement_theta_max      73.2120
_cell_measurement_theta_min      4.3580
_cell_volume                     4128.29(13)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_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, 2015)'
_diffrn_ambient_temperature      120.15
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.973
_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  0.0229
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8327
_diffrn_reflns_point_group_measured_fraction_full 0.727
_diffrn_reflns_point_group_measured_fraction_max 0.716
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.521
_diffrn_reflns_theta_min         3.631
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.563
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1808
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 1302 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.022(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         5960
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0403P)^2^+1.2116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0822
_reflns_Friedel_coverage         0.322
_reflns_Friedel_fraction_full    0.403
_reflns_Friedel_fraction_max     0.393
_reflns_number_gt                5564
_reflns_number_total             5960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01076j2.cif
_cod_data_source_block           bppcola
_cod_depositor_comments
'Adding full bibliography for 7707339--7707346.cif.'
_cod_database_code               7707343
_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
2. Restrained distances
 C29-C28A
 1.51 with sigma of 0.01
 C29-C28B
 1.51 with sigma of 0.01
 S27A-C28A
 1.82 with sigma of 0.01
 S27B-C28B
 1.82 with sigma of 0.01
 S26-S27A
 2.08 with sigma of 0.01
 S26-S27B
 2.08 with sigma of 0.01
 C54-C58A
 1.51 with sigma of 0.005
 C57A-C58A
 1.51 with sigma of 0.005
 C54-C58B
 1.51 with sigma of 0.005
 C57B-C58B
 1.51 with sigma of 0.005
 C54-C57A
 2.47 with sigma of 0.01
 C54-C57B
 2.47 with sigma of 0.01
 C53-C58A
 2.47 with sigma of 0.01
 C53-C58B
 2.47 with sigma of 0.01
 S56A-C57A
 1.82 with sigma of 0.01
 S56B-C57B
 1.82 with sigma of 0.01
 S55-S56A
 2.08 with sigma of 0.01
 S55-S56B
 2.08 with sigma of 0.01
3. Others
 Fixed Sof: S27A(0.75) C28A(0.75) H28A(0.75) H28B(0.75) H29A(0.75) H29B(0.75)
 H29C(0.25) H29D(0.25) H54(0.6) H54A(0.4) S56A(0.6) C57A(0.6) H57A(0.6)
 H57B(0.6) C58A(0.6) H58A(0.6) H58B(0.6) S56B(0.4) C57B(0.4) H57C(0.4)
 H57D(0.4) C58B(0.4) H58C(0.4) H58D(0.4) C28B(0.25) H28C(0.25) H28D(0.25)
 S27B(0.25)
4.a Ternary CH refined with riding coordinates:
 C25(H25), C54(H54), C54(H54A)
4.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,
 H24B), C28A(H28A,H28B), C29(H29A,H29B), C29(H29C,H29D), C46(H46A,H46B),
 C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C57A(H57A,
 H57B), C58A(H58A,H58B), C57B(H57C,H57D), C58B(H58C,H58D), C28B(H28C,H28D)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C14(H14), C15(H15), C16(H16),
 C32(H32), C34(H34), C38(H38), C39(H39), C40(H40), C43(H43), C44(H44), C45(H45)
;
_shelx_res_checksum              38238
_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
;