Evidence of crystal packing effects in stabilizing high or low spin states of iron(ii) complexes with functionalized 2,6-bis(pyrazol-1-yl)pyridine ligands.
Bridonneau, Nathalie; Rigamonti, Luca; Poneti, Giordano; Pinkowicz, Dawid; Forni, Alessandra; Cornia, Andrea; Dalton transactions (Cambridge, England : 2003) 46 (2017) 4075–4085; doi:10.1039/c7dt00248c

data_7042202
_publ_section_title
;
 Evidence of crystal packing effects in stabilizing high or low spin
 states of iron(ii) complexes with functionalized
 2,6-bis(pyrazol-1-yl)pyridine ligands.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4075
_journal_page_last               4085
_journal_paper_doi               10.1039/c7dt00248c
_journal_volume                  46
_journal_year                    2017
_chemical_compound_source        synthesis
_chemical_formula_iupac          '[Fe(C13H11N5O2)2](ClO4)2'
_chemical_formula_moiety         'C26 H22 Fe N10 O4, 2(Cl O4)'
_chemical_formula_sum            'C26 H22 Cl2 Fe N10 O12'
_chemical_formula_weight         793.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-12-13 deposited with the CCDC.
2017-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 127.074(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.476(3)
_cell_length_b                   10.3734(11)
_cell_length_c                   15.7959(18)
_cell_measurement_reflns_used    6873
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      32.02
_cell_measurement_theta_min      2.35
_cell_volume                     3069.1(6)
_computing_cell_refinement       'APEX2 (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'Mercury 3.8 (Macrae, 2008)'
_computing_publication_material
'WINGX publication routines v2013.3 (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_diffrn_ambient_temperature      115(2)
_diffrn_detector_area_resol_mean 66
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker X8APEX four-circle diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21845
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.020
_diffrn_reflns_theta_min         2.175
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_preparation
;
crystallization from acetonitrile/diethylether,
crystal fixed on glass fiber with vacuum grease
;
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         5317
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0494P)^2^+3.3911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4875
_reflns_number_total             5317
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00248c2.cif
_cod_data_source_block           071015LRA_work1
_cod_depositor_comments
'Adding full bibliography for 7042202--7042203.cif.'
_cod_database_code               7042202
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.759
_shelx_estimated_absorpt_t_max   0.859
_shelx_res_checksum              3246