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_7044174
_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 Fe2.98 N16.67 Ni6.02 O26.8'
_chemical_formula_weight         2197.22
_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                   25.3484(5)
_cell_length_b                   25.3484(5)
_cell_length_c                   25.3324(5)
_cell_measurement_reflns_used    34419
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      72.05
_cell_measurement_theta_min      6.54
_cell_volume                     16277.1(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      160(2)
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.967
_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  0.0661
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.910
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            45088
_diffrn_reflns_point_group_measured_fraction_full 0.910
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         64.994
_diffrn_reflns_theta_min         6.534
_exptl_absorpt_coefficient_mu    4.797
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.393
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             6760
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
TITL shelxl    P 4/n n c    R = 0.12
CELL   25.3484   25.3484   25.3324     90.00     90.00     90.00
SPGR P4/nnc
C101 0.981 0.137 0.078 !       3.31 eA-3
C102 0.502 0.058 0.133 !       3.26 eA-3
C103 0.478 0.633 0.971 !       3.10 eA-3
C104 0.460 0.058 0.141 !       2.80 eA-3
C105 0.441 0.556 0.126 !       2.56 eA-3
C106 0.898 0.773 0.015 !       2.05 eA-3
C107 0.470 0.643 0.008 !       1.88 eA-3
C108 0.899 0.993 0.055 !       1.87 eA-3
C109 0.750 0.753 0.266 !       1.49 eA-3
C110 0.753 0.603 0.449 !       1.43 eA-3
C111 0.601 0.540 0.085 !       1.30 eA-3
C112 0.822 0.577 0.232 !       1.20 eA-3
Q113 0.250 0.245 0.031 !       1.08 eA-3
C114 0.750 0.755 0.148 !       1.07 eA-3
C115 0.244 0.228 0.496 !       1.06 eA-3
C116 0.785 0.600 0.414 !       0.94 eA-3
C117 0.515 0.557 0.469 !       0.93 eA-3
C118 0.750 0.752 0.008 !       0.88 eA-3
C119 0.678 0.899 0.186 !       0.87 eA-3
C120 0.649 0.944 0.209 !       0.84 eA-3
C121 0.249 0.262 0.695 !       0.82 eA-3
Q122 0.265 0.132 0.026 !       0.78 eA-3
C123 0.031 0.487 0.501 !       0.76 eA-3
C124 0.703 0.595 0.297 !       0.75 eA-3
C125 0.094 0.353 0.727 !       0.75 eA-3
Q126 0.318 0.856 0.568 !       0.75 eA-3
Q127 0.531 0.833 0.772 !       0.74 eA-3
C128 0.820 0.693 0.162 !       0.73 eA-3
C129 0.750 0.751 0.117 !       0.73 eA-3
C130 0.750 0.748 0.414 !       0.72 eA-3
Q131 0.247 0.798 0.185 !       0.72 eA-3
C132 0.512 0.568 0.164 !       0.69 eA-3
C133 0.507 0.426 0.568 !       0.66 eA-3
C134 0.651 0.580 0.217 !       0.64 eA-3
C135 0.542 0.555 0.068 !       0.64 eA-3
C136 0.898 0.644 0.313 !       0.63 eA-3
Q137 0.126 0.161 0.407 !       0.60 eA-3
C138 0.795 0.836 0.132 !       0.59 eA-3
Q139 0.467 0.594 0.093 !       0.59 eA-3
Q140 0.048 0.919 0.275 !       0.59 eA-3
C141 0.939 0.750 0.250 !       0.59 eA-3
C142 0.400 0.154 0.896 !       0.58 eA-3
C143 0.727 0.574 0.268 !       0.57 eA-3
Q144 0.409 0.797 0.639 !       0.56 eA-3
C145 0.602 0.902 0.282 !       0.55 eA-3
Q146 0.135 0.398 0.422 !       0.55 eA-3
C147 0.409 0.586 0.015 !       0.55 eA-3
C148 0.386 0.132 0.902 !       0.55 eA-3
C149 0.109 0.095 0.756 !       0.54 eA-3
Q150 0.109 0.779 0.188 !       0.54 eA-3
Q151 0.094 0.474 0.325 !       0.54 eA-3
Q152 0.242 0.163 0.401 !       0.54 eA-3
C153 0.868 0.853 0.199 !       0.53 eA-3
C154 0.883 0.625 0.228 !       0.53 eA-3
Q155 0.384 0.554 0.134 !       0.52 eA-3
C156 0.672 0.935 0.290 !       0.52 eA-3
Q157 0.159 0.069 0.210 !       0.52 eA-3
Q158 0.578 0.282 0.360 !       0.52 eA-3
C159 0.904 0.650 0.155 !       0.52 eA-3
Q160 0.031 0.012 0.672 !       0.51 eA-3
Q161 0.281 0.157 0.100 !       0.51 eA-3
Q162 0.376 0.418 0.084 !       0.51 eA-3
Q163 0.250 0.752 0.297 !       0.50 eA-3
;
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         6716
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0767P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1307
_refine_ls_wR_factor_ref         0.1421
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4762
_reflns_number_total             6716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02930f2.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        16277.1(7)
_cod_original_formula_sum        'C77.33 H85.60 Fe2.98 N16.67 Ni6.02 O26.80'
_cod_database_code               7044174
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014/6
_shelx_res_checksum              2076
_shelx_fab_checksum              32926