Nonanuclear Spin-Crossover Complex Containing Iron(II) and Iron(III) Based on a 2,6-Bis(pyrazol-1-yl)pyridine Ligand Functionalized with a Carboxylate Group.
Abhervé, Alexandre; Recio-Carretero, María José; López-Jordà, Maurici; Clemente-Juan, Juan Modesto; Canet-Ferrer, Josep; Cantarero, Andrés; Clemente-León, Miguel; Coronado, Eugenio; Inorganic chemistry 55 (2016) 9361–9367; doi:10.1021/acs.inorgchem.6b01508

data_4348671
_publ_section_title
;
 Nonanuclear Spin-Crossover Complex Containing Iron(II) and Iron(III)
 Based on a 2,6-Bis(pyrazol-1-yl)pyridine Ligand Functionalized with a
 Carboxylate Group.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9361
_journal_page_last               9367
_journal_paper_doi               10.1021/acs.inorgchem.6b01508
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C162 H138 Cl8 Fe9 N60 O66'
_chemical_formula_weight         4767.57
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   18.1644(6)
_cell_length_b                   18.1644(6)
_cell_length_c                   48.1237(10)
_cell_measurement_reflns_used    6581
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      20.9220
_cell_measurement_theta_min      3.0750
_cell_volume                     13750.9(7)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Sapphire3'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1542
_diffrn_reflns_av_unetI/netI     0.1221
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            79824
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.394
_diffrn_reflns_theta_min         3.084
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

CrysAlisPro, Agilent Technologies,

Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)

(compiled Mar 27 2014,17:12:48)

Empirical absorption correction using spherical harmonics,

 implemented in SCALE3 ABSPACK scaling algorithm.

;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       prism
_exptl_crystal_F_000             4856
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.833
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         9361
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.833
_refine_ls_R_factor_all          0.1382
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2067
_refine_ls_wR_factor_ref         0.2664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5140
_reflns_number_total             9361
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01508_si_001.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        13750.9(10)
_cod_database_code               4348671
_shelx_estimated_absorpt_t_min   0.862
_shelx_estimated_absorpt_t_max   0.976
_shelxl_version_number           2013-4
_shelx_res_checksum              28106
_shelx_hkl_checksum              38769
_shelx_fab_checksum              73819