Site preferences in hetero-metallic [Fe9-xNix] clusters: a combined crystallographic, spectroscopic and theoretical analysis
Georgopoulou, Anastasia N.; Al-Ameed, Karrar; Boudalis, Athanassios; Anagnostopoulos, Dimitrios F.; Psycharis, Vassilis; McGrady, John E.; Sanakis, Yiannis; Raptopoulou, Catherine P.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02930F

data_7044175
_publ_section_title
;
 Site preferences in hetero-metallic [Fe9-xNix] clusters: a combined
 crystallographic, spectroscopic and theoretical analysis
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02930F
_journal_year                    2017
_chemical_formula_sum            'C77.33 H85.6 Fe1.54 N16.67 Ni7.46 O26.8'
_chemical_formula_weight         2201.34
_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_Hall           '-P 4a 2bc'
_space_group_name_H-M_alt        'P 4/n n c'
_symmetry_space_group_name_Hall  '-P 4a 2bc'
_symmetry_space_group_name_H-M   'P 4/n n c :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-09-08 deposited with the CCDC.
2017-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   25.4547(4)
_cell_length_b                   25.4547(4)
_cell_length_c                   25.6338(4)
_cell_measurement_reflns_used    38444
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      71.97
_cell_measurement_theta_min      6.50
_cell_volume                     16609.2(5)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_molecular_graphics    'Diamond ver.3.1.'
_computing_publication_material  'publCIF J.Appl.Cryst. 2010, 43, 920'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       '\q scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.926
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            50692
_diffrn_reflns_point_group_measured_fraction_full 0.926
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         64.982
_diffrn_reflns_theta_min         6.503
_exptl_absorpt_coefficient_mu    3.492
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.576
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             6778
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
TITL shelxl    P 4/n n c    R = 0.11
CELL   25.4547   25.4547   25.6338     90.00     90.00     90.00
SPGR P4/nnc
C101 0.522 0.130 0.420 !       2.69 eA-3
C102 0.533 0.133 0.470 !       2.41 eA-3
C103 0.999 0.449 0.132 !       2.19 eA-3
C104 0.039 0.444 0.150 !       2.04 eA-3
C105 0.947 0.060 0.375 !       1.80 eA-3
C106 0.771 0.893 0.486 !       1.55 eA-3
C107 0.054 0.863 0.009 !       1.45 eA-3
C108 0.890 0.511 0.441 !       1.24 eA-3
C109 0.587 0.541 0.079 !       0.92 eA-3
Q110 0.750 0.252 0.297 !       0.86 eA-3
C111 0.250 0.251 0.016 !       0.86 eA-3
C112 0.943 0.522 0.462 !       0.83 eA-3
C113 0.834 0.561 0.234 !       0.83 eA-3
C114 0.932 0.631 0.301 !       0.81 eA-3
C115 0.930 0.665 0.289 !       0.77 eA-3
C116 0.727 0.564 0.049 !       0.74 eA-3
C117 0.942 0.623 0.329 !       0.68 eA-3
Q118 0.656 0.323 0.344 !       0.68 eA-3
Q119 0.166 0.266 0.389 !       0.66 eA-3
C120 0.899 0.566 0.074 !       0.64 eA-3
Q121 0.300 0.653 0.367 !       0.60 eA-3
C122 0.659 0.565 0.227 !       0.59 eA-3
Q123 0.750 0.751 0.695 !       0.58 eA-3
C124 0.576 0.705 0.222 !       0.54 eA-3
C125 0.092 0.152 0.823 !       0.54 eA-3
Q126 0.838 0.980 0.772 !       0.52 eA-3
Q127 0.594 0.232 0.124 !       0.52 eA-3
Q128 0.654 0.201 0.273 !       0.51 eA-3
;
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         6986
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0546
_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^)+(0.1105P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1712
_refine_ls_wR_factor_ref         0.1842
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4921
_reflns_number_total             6986
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02930f2.cif
_cod_data_source_block           shelxl_CCDC1
_cod_original_cell_volume        16609.2(6)
_cod_original_formula_sum        'C77.33 H85.60 Fe1.54 N16.67 Ni7.46 O26.80'
_cod_database_code               7044175
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014/6
_shelx_res_checksum              39614
_shelx_fab_checksum              45866