Iron Lanthanide Phosphonate Clusters: {Fe6Ln6P6} Wells-Dawson-like Structures with D3d Symmetry.
Pineda, Eufemio Moreno; Tuna, Floriana; Zheng, Yan-Zhen; Teat, Simon J.; Winpenny, Richard E. P.; Schnack, Jürgen; McInnes, Eric J. L.; Inorganic chemistry 53 (2014) 3032–3038; doi:10.1021/ic402839q

data_4337624
_publ_section_title
;
 Iron Lanthanide Phosphonate Clusters: {Fe6Ln6P6} Wells-Dawson-like
 Structures with D3d Symmetry.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3032
_journal_page_last               3038
_journal_paper_doi               10.1021/ic402839q
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C127 H192 Fe6 O59 P6 Tb6'
_chemical_formula_sum            'C127 H192 Fe6 O59 P6 Tb6'
_chemical_formula_weight         4137.23
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-10-26
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   16.8951(2)
_cell_length_b                   16.8951(2)
_cell_length_c                   103.8149(15)
_cell_measurement_reflns_used    44273
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.8510
_cell_measurement_theta_min      1.6160
_cell_volume                     25663.3(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.9659
_diffrn_measured_fraction_theta_max 0.9462
_diffrn_measurement_details
;
  1 omega    2.20  182.01   0.2997    9.9860
omega____ theta____ kappa____ phi______ frames
    -       28.0000   73.8962  -25.8019 600

  2 omega    2.20  182.01   0.2997    9.9860
omega____ theta____ kappa____ phi______ frames
    -       28.0000   73.8962   94.1981 600

  3 omega    2.20  182.01   0.2997    9.9860
omega____ theta____ kappa____ phi______ frames
    -       28.0000   73.8962 -145.8038 600
;
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0353476000
_diffrn_orient_matrix_UB_12      -0.0406257000
_diffrn_orient_matrix_UB_13      -0.0028099000
_diffrn_orient_matrix_UB_21      0.0030900000
_diffrn_orient_matrix_UB_22      0.0244064000
_diffrn_orient_matrix_UB_23      -0.0057125000
_diffrn_orient_matrix_UB_31      0.0330455000
_diffrn_orient_matrix_UB_32      -0.0101863000
_diffrn_orient_matrix_UB_33      -0.0024759000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.1040
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       140
_diffrn_reflns_limit_l_min       -135
_diffrn_reflns_number            70128
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.821
_diffrn_reflns_theta_min         1.598
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.070
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour
;
;
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             12372
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.393
_refine_diff_density_min         -1.531
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.232
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         7252
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.241
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0950
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+1499.9500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1972
_refine_ls_wR_factor_ref         0.2011
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6649
_reflns_number_total             7252
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic402839q_si_004.cif
_cod_data_source_block           Fe6Tb6P6_Phenyl
_cod_original_cell_volume        25663.2(7)
_cod_database_code               4337624
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C7-C6
 1.52 with sigma of 0.02
 C7-C4
 1.52 with sigma of 0.02
 C8-C7 = C7-C4
 1.52 with sigma of 0.02
 O16-C1C = C1C-O12
 1.23 with sigma of 0.02
 C4-C7 = C7-C9
 1.52 with sigma of 0.02
 C1C-C18 = C18-C1B
 1.52 with sigma of 0.02
 C1C-C18 = C18-C19
 1.52 with sigma of 0.02
 C1A-C18 = C18-C1C
 1.52 with sigma of 0.02
 C8-C4
 2.483 with sigma of 0.04
 O16-O12
 2.162 with sigma of 0.04
 C4-C9
 2.483 with sigma of 0.04
 C1C-C1B
 2.483 with sigma of 0.04
 C1C-C19
 2.483 with sigma of 0.04
 C1A-C1C
 2.483 with sigma of 0.04
 O7-C4 \\sim C4-O10
 with sigma of 0.02
 O3-C4 \\sim C4-O13
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O14) = Uanis(O6)
Uanis(O16) = Uanis(O12)
Uanis(C1C) = Uanis(C4)
Uanis(C1C) = Uanis(C1D)
Uanis(C9) = Uanis(C16)
Uanis(C11) = Uanis(C4)
Uanis(C1A) = Uanis(C1B) = Uanis(C19)
Uanis(O7) = Uanis(O13)
Uanis(O3) = Uanis(O3)
Uanis(O3) = Uanis(O10)
Uanis(O3) = Uanis(O7) = Uanis(O13) = Uanis(O10)
4. Others
 Sof(O6)=Sof(O7)=Sof(O8)=Sof(O10)=Sof(O11)=Sof(O17)=Sof(O18)=Sof(C1D)=Sof(C16)=
 Sof(H16A)=Sof(H16B)=Sof(H16C)=1-FVAR(1)
 Sof(O3)=Sof(O9)=Sof(O12)=Sof(O13)=Sof(O14)=Sof(O15)=Sof(O16)=Sof(C1C)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
 Fixed Sof: O5(0.5)
5.a Me refined with riding coordinates:
 C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C),
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C19(H19A,H19B,H19C)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C14(H14), C17(H17), C20(H20)
;
_shelx_hkl_checksum              11205
_shelx_res_checksum              49062
_shelxl_version_number           2013-4