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_7044176
_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 Fe1.19 N16.67 Ni7.81 O26.8'
_chemical_formula_weight         2202.34
_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                   25.4102(5)
_cell_length_b                   25.4102(5)
_cell_length_c                   25.5493(5)
_cell_measurement_reflns_used    39142
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      72.00
_cell_measurement_theta_min      6.51
_cell_volume                     16496.6(6)
_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      200(2)
_diffrn_measured_fraction_theta_full 0.862
_diffrn_measured_fraction_theta_max 0.918
_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  0.0617
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.862
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            51269
_diffrn_reflns_point_group_measured_fraction_full 0.862
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         64.987
_diffrn_reflns_theta_min         6.508
_exptl_absorpt_coefficient_mu    3.220
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             6782
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.31
_platon_squeeze_details
;
TITL shelxl    P 4/n n c    R = 0.13
CELL   25.4102   25.4102   25.5493     90.00     90.00     90.00
SPGR P4/nnc
C101 0.131 0.979 0.417 !       2.72 eA-3
C102 0.538 0.133 0.471 !       2.43 eA-3
C103 0.500 0.051 0.142 !       2.34 eA-3
C104 0.448 0.460 0.148 !       2.09 eA-3
C105 0.938 0.446 0.627 !       1.96 eA-3
C106 0.137 0.548 0.990 !       1.68 eA-3
C107 0.617 0.766 0.486 !       1.60 eA-3
C108 0.734 0.917 0.006 !       1.50 eA-3
C109 0.508 0.603 0.444 !       1.35 eA-3
C110 0.584 0.964 0.429 !       1.13 eA-3
C111 0.561 0.982 0.463 !       1.04 eA-3
C112 0.250 0.248 0.016 !       0.97 eA-3
Q113 0.330 0.876 0.178 !       0.96 eA-3
C114 0.778 0.916 0.067 !       0.95 eA-3
C115 0.924 0.835 0.204 !       0.94 eA-3
C116 0.751 0.952 0.030 !       0.93 eA-3
Q117 0.291 0.137 0.153 !       0.88 eA-3
Q118 0.272 0.679 0.320 !       0.87 eA-3
C119 0.250 0.252 0.641 !       0.87 eA-3
C120 0.910 0.920 0.087 !       0.83 eA-3
Q121 0.635 0.734 0.656 !       0.81 eA-3
Q122 0.171 0.683 0.183 !       0.80 eA-3
C123 0.891 0.625 0.316 !       0.80 eA-3
C124 0.874 0.907 0.364 !       0.78 eA-3
C125 0.640 0.914 0.228 !       0.77 eA-3
C126 0.595 0.842 0.345 !       0.72 eA-3
Q127 0.197 0.265 0.159 !       0.69 eA-3
Q128 0.276 0.781 0.247 !       0.69 eA-3
C129 0.097 0.094 0.891 !       0.69 eA-3
Q130 0.371 0.855 0.794 !       0.68 eA-3
C131 0.886 0.927 0.424 !       0.67 eA-3
C132 0.892 0.673 0.285 !       0.67 eA-3
C133 0.594 0.939 0.108 !       0.67 eA-3
C134 0.791 0.580 0.229 !       0.65 eA-3
Q135 0.233 0.627 0.181 !       0.65 eA-3
Q136 0.795 0.802 0.655 !       0.65 eA-3
C137 0.048 0.146 0.789 !       0.65 eA-3
Q138 0.627 0.293 0.297 !       0.64 eA-3
Q139 0.778 0.719 0.753 !       0.63 eA-3
Q140 0.685 0.151 0.199 !       0.63 eA-3
Q141 0.687 0.294 0.302 !       0.61 eA-3
C142 0.584 0.923 0.346 !       0.57 eA-3
C143 0.593 0.906 0.251 !       0.54 eA-3
C144 0.963 0.954 0.089 !       0.54 eA-3
C145 0.750 0.922 0.248 !       0.54 eA-3
C146 0.094 0.108 0.702 !       0.53 eA-3
C147 0.628 0.861 0.340 !       0.52 eA-3
Q148 0.208 0.945 0.092 !       0.52 eA-3
C149 0.702 0.625 0.105 !       0.52 eA-3
C150 0.791 0.607 0.243 !       0.52 eA-3
Q151 0.158 0.020 0.228 !       0.51 eA-3
;
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         6459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1211P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1852
_refine_ls_wR_factor_ref         0.1969
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4570
_reflns_number_total             6459
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02930f2.cif
_cod_data_source_block           shelxl_CCDC2
_cod_original_cell_volume        16496.6(7)
_cod_original_formula_sum        'C77.33 H85.60 Fe1.19 N16.67 Ni7.81 O26.80'
_cod_database_code               7044176
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014/6
_shelx_res_checksum              78176
_shelx_fab_checksum              60902