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_7044177
_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 Fe9 N16.67 Ni0 O26.8'
_chemical_formula_weight         2180.00
_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                   25.6264(5)
_cell_length_b                   25.6264(5)
_cell_length_c                   25.3002(5)
_cell_measurement_reflns_used    22572
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      72.03
_cell_measurement_theta_min      6.51
_cell_volume                     16615.0(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 0.564
_diffrn_measured_fraction_theta_max 0.994
_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  0.3563
_diffrn_reflns_av_unetI/netI     0.2693
_diffrn_reflns_Laue_measured_fraction_full 0.564
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38901
_diffrn_reflns_point_group_measured_fraction_full 0.564
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         49.980
_diffrn_reflns_theta_min         6.517
_exptl_absorpt_coefficient_mu    9.752
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.201
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             6688
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
TITL shelxl    P 4/n n c    R = 0.25
CELL   25.6264   25.6264   25.3002     90.00     90.00     90.00
SPGR P4/nnc
C101 0.160 0.250 0.750 !       3.47 eA-3
C102 0.724 0.728 0.309 !       2.49 eA-3
C103 0.750 0.754 0.023 !       1.98 eA-3
C104 0.871 0.665 0.151 !       1.67 eA-3
Q105 0.750 0.753 0.609 !       1.64 eA-3
C106 0.742 0.822 0.373 !       1.49 eA-3
C107 0.885 0.791 0.269 !       1.46 eA-3
C108 0.788 0.750 0.250 !       1.42 eA-3
C109 0.685 0.858 0.414 !       1.41 eA-3
C110 0.444 0.464 0.138 !       1.40 eA-3
C111 0.772 0.682 0.196 !       1.38 eA-3
C112 0.966 0.904 0.191 !       1.35 eA-3
C113 0.473 0.623 0.029 !       1.35 eA-3
C114 0.118 0.506 0.556 !       1.34 eA-3
Q115 0.843 0.955 0.197 !       1.30 eA-3
Q116 0.228 0.623 0.207 !       1.29 eA-3
C117 0.654 0.586 0.209 !       1.29 eA-3
C118 0.917 0.886 0.171 !       1.27 eA-3
C119 0.610 0.591 0.326 !       1.27 eA-3
C120 0.595 0.773 0.153 !       1.27 eA-3
C121 0.382 0.177 0.680 !       1.25 eA-3
C122 0.421 0.501 0.397 !       1.25 eA-3
Q123 0.636 0.799 0.638 !       1.25 eA-3
Q124 0.642 0.015 0.105 !       1.24 eA-3
C125 0.975 0.376 0.409 !       1.24 eA-3
Q126 0.033 0.017 0.302 !       1.24 eA-3
Q127 0.664 0.187 0.659 !       1.23 eA-3
C128 0.499 0.914 0.342 !       1.23 eA-3
Q129 0.979 0.085 0.215 !       1.21 eA-3
Q130 0.305 0.404 0.435 !       1.20 eA-3
C131 0.353 0.491 0.944 !       1.20 eA-3
Q132 0.663 0.996 0.066 !       1.19 eA-3
Q133 0.493 0.690 0.276 !       1.19 eA-3
C134 0.750 0.755 0.102 !       1.17 eA-3
C135 0.678 0.898 0.089 !       1.17 eA-3
Q136 0.166 0.433 0.194 !       1.16 eA-3
C137 0.089 0.453 0.636 !       1.16 eA-3
Q138 0.265 0.628 0.189 !       1.16 eA-3
C139 0.730 0.563 0.477 !       1.15 eA-3
C140 0.638 0.827 0.340 !       1.15 eA-3
C141 0.859 0.859 0.195 !       1.15 eA-3
C142 0.730 0.633 0.115 !       1.14 eA-3
Q143 0.867 0.994 0.118 !       1.13 eA-3
Q144 0.740 0.959 0.096 !       1.11 eA-3
Q145 0.289 0.859 0.247 !       1.10 eA-3
C146 0.862 0.748 0.201 !       1.10 eA-3
C147 0.619 0.514 0.132 !       1.09 eA-3
Q148 0.220 0.220 0.137 !       1.09 eA-3
Q149 0.248 0.650 0.703 !       1.08 eA-3
Q150 0.272 0.485 0.582 !       1.07 eA-3
C151 0.786 0.792 0.053 !       1.06 eA-3
C152 0.509 0.359 0.021 !       1.06 eA-3
Q153 0.338 0.196 0.157 !       1.06 eA-3
Q154 0.301 0.135 0.345 !       1.05 eA-3
C155 0.365 0.561 0.493 !       1.05 eA-3
C156 0.540 0.587 0.224 !       1.05 eA-3
Q157 0.612 0.464 0.916 !       1.04 eA-3
Q158 0.722 0.960 0.163 !       1.04 eA-3
Q159 0.412 0.390 0.424 !       1.03 eA-3
Q160 0.717 0.819 0.772 !       1.03 eA-3
Q161 0.054 0.141 0.000 !       1.02 eA-3
Q162 0.110 0.064 0.495 !       1.02 eA-3
Q163 0.478 0.490 0.200 !       1.02 eA-3
C164 0.940 0.058 0.365 !       1.02 eA-3
Q165 0.996 0.142 0.470 !       1.02 eA-3
C166 0.024 0.663 0.491 !       1.01 eA-3
C167 0.992 0.546 0.074 !       1.01 eA-3
Q168 0.316 0.525 0.191 !       1.01 eA-3
Q169 0.397 0.831 0.558 !       1.01 eA-3
Q170 0.499 0.578 0.285 !       0.99 eA-3
C171 0.922 0.504 0.470 !       0.99 eA-3
C172 0.588 0.955 0.135 !       0.99 eA-3
Q173 0.202 0.798 0.343 !       0.98 eA-3
Q174 0.902 0.052 0.111 !       0.98 eA-3
C175 0.770 0.963 0.250 !       0.98 eA-3
C176 0.179 0.250 0.008 !       0.98 eA-3
Q177 0.483 0.250 0.250 !       0.98 eA-3
C178 0.245 0.057 0.930 !       0.96 eA-3
Q179 0.359 0.220 0.276 !       0.96 eA-3
C180 0.259 0.388 0.546 !       0.95 eA-3
C181 0.063 0.220 0.041 !       0.95 eA-3
Q182 0.054 0.921 0.250 !       0.94 eA-3
C183 0.920 0.866 0.080 !       0.94 eA-3
C184 0.075 0.543 0.447 !       0.93 eA-3
C185 0.539 0.951 0.337 !       0.93 eA-3
Q186 0.369 0.357 0.479 !       0.93 eA-3
C187 0.543 0.654 0.189 !       0.93 eA-3
Q188 0.680 0.734 0.553 !       0.93 eA-3
C189 0.912 0.781 0.021 !       0.93 eA-3
Q190 0.343 0.537 0.010 !       0.92 eA-3
C191 0.799 0.647 0.322 !       0.92 eA-3
Q192 0.704 0.296 0.708 !       0.92 eA-3
Q193 0.666 0.674 0.526 !       0.91 eA-3
Q194 0.085 0.591 0.607 !       0.91 eA-3
Q195 0.201 0.881 0.054 !       0.91 eA-3
C196 0.907 0.575 0.393 !       0.91 eA-3
Q197 0.848 0.314 0.862 !       0.91 eA-3
Q198 0.528 0.010 0.320 !       0.91 eA-3
C199 0.670 0.600 0.109 !       0.90 eA-3
;
_refine_diff_density_max         1.157
_refine_diff_density_min         -1.742
_refine_diff_density_rms         0.265
_refine_ls_extinction_coef       0.106(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.567
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.567
_refine_ls_R_factor_all          0.2477
_refine_ls_R_factor_gt           0.2074
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_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          0.4505
_refine_ls_wR_factor_ref         0.4775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2342
_reflns_number_total             4254
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02930f2.cif
_cod_data_source_block           shelxl_CCDC3
_cod_original_cell_volume        16615.0(7)
_cod_original_formula_sum        'C77.33 H85.60 Fe9 N16.67 Ni0 O26.80'
_cod_database_code               7044177
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014/6
_shelx_res_checksum              84287
_shelx_fab_checksum              27856