Iron(ii) complexes of 4-sulfanyl-, 4-sulfinyl- and 4-sulfonyl-2,6-dipyrazolylpyridine ligands. A subtle interplay between spin-crossover and crystallographic phase changes
Kershaw Cook, Laurence J.; Kulmaczewski, Rafal; Barrett, Simon A.; Halcrow, Malcolm A.; Inorganic Chemistry Frontiers 2 (2015) 662–; doi:10.1039/C5QI00083A

data_4348919
_publ_section_title
;
 Iron(ii) complexes of 4-sulfanyl-, 4-sulfinyl- and
 4-sulfonyl-2,6-dipyrazolylpyridine ligands. A subtle interplay between
 spin-crossover and crystallographic phase changes
;
_journal_issue                   7
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              662
_journal_paper_doi               10.1039/C5QI00083A
_journal_volume                  2
_journal_year                    2015
_chemical_formula_moiety         'C24 H22 Fe N10 S2, 2[Cl O4]'
_chemical_formula_sum            'C24 H22 Cl2 Fe N10 O8 S2'
_chemical_formula_weight         769.39
_chemical_name_systematic
Bis[2,6-di(pyrazol-1-yl)4-methylsulfanylpyridine]iron(II)diperchlorate
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-04-21 deposited with the CCDC.
2015-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   54.8011(19)
_cell_length_b                   10.6074(3)
_cell_length_c                   16.3787(5)
_cell_measurement_reflns_used    3879
_cell_measurement_temperature    280(2)
_cell_measurement_theta_max      73.64
_cell_measurement_theta_min      4.18
_cell_volume                     9520.9(5)
_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  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      280(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       66
_diffrn_reflns_limit_h_min       -61
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22818
_diffrn_reflns_theta_full        73.73
_diffrn_reflns_theta_max         73.73
_diffrn_reflns_theta_min         4.25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.153
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             4704
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: nitromethane/diethyl ether'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.827
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         9301
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0780
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0979P)^2^+26.5933P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2019
_refine_ls_wR_factor_ref         0.2215
_reflns_number_gt                6320
_reflns_number_total             9301
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5qi00083a2.cif
_cod_data_source_block           lkc266rt
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Orthorhombic' was changed
to 'orthorhombic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4348919