Modulation of FeII spin crossover effect in the pentadecanuclear {Fe9[M(CN)8]6} (M = Re, W) clusters by facial coordination of tridentate polyamine ligand
Chorazy, Szymon; Jan Stanek, Jan; Kobylarczyk, Jedrzej; Ohkoshi, Shin-ichi; Sieklucka, Barbara; Podgajny, Robert; Dalton Trans.  (2017) –; doi:10.1039/C7DT01416C

data_7042933
_publ_section_title
;
 Modulation of FeII spin crossover effect in the pentadecanuclear
 {Fe9[M(CN)8]6} (M = Re, W) clusters by facial coordination of tridentate
 polyamine ligand
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01416C
_journal_year                    2017
_chemical_formula_moiety         'C134 H168 Fe9 N72 O14 Re6'
_chemical_formula_sum            'C134 H168 Fe9 N72 O14 Re6'
_chemical_formula_weight         4631.24
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2017-05-04T18:50:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2017-05-05 deposited with the CCDC.
2017-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                86.341(6)
_cell_angle_beta                 83.480(6)
_cell_angle_gamma                86.361(6)
_cell_formula_units_Z            2
_cell_length_a                   17.5772(9)
_cell_length_b                   17.6464(8)
_cell_length_c                   28.8773(13)
_cell_measurement_reflns_used    72887
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.986
_cell_measurement_wavelength     0.71075
_cell_volume                     8866.6(7)
_computing_data_collection       'RAPID-AUTO (Rigaku, 2009)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1474
_diffrn_reflns_av_unetI/netI     0.1819
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            72887
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25.028
_diffrn_reflns_theta_min         2.986
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.861
_exptl_absorpt_correction_T_max  0.727
_exptl_absorpt_correction_T_min  0.529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4544
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.113
_refine_diff_density_min         -1.584
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.27
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     2071
_refine_ls_number_reflns         30077
_refine_ls_number_restraints     743
_refine_ls_restrained_S_all      1.273
_refine_ls_R_factor_all          0.2841
_refine_ls_R_factor_gt           0.207
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+461.3475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3348
_refine_ls_wR_factor_ref         0.3702
_reflns_Friedel_coverage         0
_reflns_number_gt                18593
_reflns_number_total             30077
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01416c2.cif
_cod_data_source_block           shelx
_cod_database_code               7042933
_shelx_res_checksum              59635