Step-by-step synthesis of one Fe6 wheel and two Fe10 clusters derived from a multidentate triethanolamine ligand
Liu, Sui-Jun; Han, Song-De; Jia, Ji-Min; Xue, Li; Cui, Yu; Zhang, Shu-Ming; Chang, Ze; CrystEngComm 16 (2014) 5212–; doi:10.1039/c3ce42381f

data_7216218
_publ_section_title
;
 Step-by-step synthesis of one Fe6 wheel and two Fe10 clusters derived
 from a multidentate triethanolamine ligand
;
_journal_issue                   24
_journal_name_full               CrystEngComm
_journal_page_first              5212
_journal_paper_doi               10.1039/c3ce42381f
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C42 H80 Fe10 N6 O34'
_chemical_formula_weight         1771.62
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-03-11 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.0100(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   37.09(2)
_cell_length_b                   11.390(7)
_cell_length_c                   29.307(16)
_cell_measurement_reflns_used    21152
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      1.4
_cell_volume                     12381(12)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      386(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  RAXIS-RAPID
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1679
_diffrn_reflns_av_sigmaI/netI    0.1714
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            45224
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.30
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.369
_exptl_absorpt_correction_T_max  0.7031
_exptl_absorpt_correction_T_min  0.6487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            reddish-brown
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       strip
_exptl_crystal_F_000             7248
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.329
_refine_diff_density_min         -1.432
_refine_diff_density_rms         0.221
_refine_ls_extinction_coef       0.000163(16)
_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   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     878
_refine_ls_number_reflns         10909
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1286
_refine_ls_R_factor_gt           0.0991
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+298.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1801
_refine_ls_wR_factor_ref         0.2036
_reflns_number_gt                7413
_reflns_number_total             10909
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce42381f2.cif
_cod_data_source_block           1
_cod_original_cell_volume        12379(13)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7216218