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_7042203
_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(C16H18N6O4)2](ClO4)2.CH3CN'
_chemical_formula_moiety         'C32 H36 Fe N12 O8, 2(Cl O4), C2 H3 N'
_chemical_formula_sum            'C34 H39 Cl2 Fe N13 O16'
_chemical_formula_weight         1012.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                 101.045(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0675(10)
_cell_length_b                   16.2407(11)
_cell_length_c                   18.2548(11)
_cell_measurement_reflns_used    4759
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      24.74
_cell_measurement_theta_min      2.60
_cell_volume                     4093.4(5)
_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      140(2)
_diffrn_detector_area_resol_mean 66
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker X8APEX four-circle diffractometer'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40776
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.494
_diffrn_reflns_theta_min         3.635
_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    0.590
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       prism
_exptl_crystal_F_000             2088
_exptl_crystal_preparation
;
crystallization from acetonitrile/diethylether,
crystal fixed on glass fiber with vacuum grease
;
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_refine_diff_density_max         3.946
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         8447
_refine_ls_number_restraints     179
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.1295
_refine_ls_R_factor_gt           0.0928
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1947P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2568
_refine_ls_wR_factor_ref         0.2869
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5581
_reflns_number_total             8447
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00248c2.cif
_cod_data_source_block           211014NB2_2_work7
_cod_depositor_comments
'Adding full bibliography for 7042202--7042203.cif.'
_cod_original_cell_volume        4093.3(5)
_cod_database_code               7042203
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.862
_shelx_estimated_absorpt_t_max   0.933
_shelx_res_checksum              93841