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_4337626
_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 Gd6 O59 P6'
_chemical_formula_sum            'C127 H192 Fe6 Gd6 O59 P6'
_chemical_formula_weight         4127.21
_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                   16.8883(3)
_cell_length_b                   16.8883(3)
_cell_length_c                   103.953(2)
_cell_measurement_reflns_used    23128
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.8740
_cell_measurement_theta_min      2.1170
_cell_volume                     25676.7(8)
_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 0.9994
_diffrn_measured_fraction_theta_max 0.9243
_diffrn_measurement_details
;
  1 omega    2.20  182.01   0.2997    2.9860
omega____ theta____ kappa____ phi______ frames
    -       28.0000   73.8962  -25.8019 600

  2 omega    2.20  182.01   0.2997    2.9860
omega____ theta____ kappa____ phi______ frames
    -       28.0000   73.8962   94.1981 600

  3 omega    2.20  115.48   0.2997    2.9860
omega____ theta____ kappa____ phi______ frames
    -       28.0000   73.8962 -145.8038 378
;
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0477108333
_diffrn_orient_matrix_UB_12      0.0314007667
_diffrn_orient_matrix_UB_13      -0.0000683333
_diffrn_orient_matrix_UB_21      -0.0031625000
_diffrn_orient_matrix_UB_22      0.0156910000
_diffrn_orient_matrix_UB_23      0.0062031000
_diffrn_orient_matrix_UB_31      0.0080899333
_diffrn_orient_matrix_UB_32      -0.0334877333
_diffrn_orient_matrix_UB_33      0.0028419667
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       125
_diffrn_reflns_limit_l_min       -129
_diffrn_reflns_number            56119
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_min         2.096
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.914
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64608
_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    1.601
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             12336
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.284
_refine_diff_density_min         -1.588
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.257
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         5839
_refine_ls_number_restraints     215
_refine_ls_restrained_S_all      1.255
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0717
_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^)+(0.0002P)^2^+1395.5194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1449
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5555
_reflns_number_total             5839
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic402839q_si_003.cif
_cod_data_source_block           Fe6Gd6P6_Phenyl
_cod_original_cell_volume        25676.6(11)
_cod_database_code               4337626
_olex2_refinement_description
;
1. Shared sites
{H1AA, H1LC}
2. Others
 Fixed Sof: O17(0.5)
 Fixed U13: O2(0) C7(0)
 Fixed U23: O2(0) C7(0)
 Fixed Uiso: H(0.097) H1AA(0.109) H1AB(0.109) H1AC(0.109) H1DA(0.096)
 H1DB(0.096) H1DC(0.096) H1FA(0.117) H1FB(0.117) H1FC(0.117) H1GA(0.122)
 H1GB(0.122) H1GC(0.122) H1HA(0.135) H1HB(0.135) H1HC(0.135) H1IA(0.135)
 H1IB(0.135) H1IC(0.135) H1KA(0.086) H1KB(0.086) H1KC(0.086) H1LA(0.077)
 H1LB(0.077) H1LC(0.077) H3(0.079) H4(0.09) H6A(0.064) H6B(0.064) H6C(0.064)
 H9A(0.148) H9B(0.148) H9C(0.148) H11(0.109) H12(0.105) H13A(0.122) H13B(0.122)
 H13C(0.122) H14A(0.166) H14B(0.166) H14C(0.166) H16A(0.135) H16B(0.135)
 H16C(0.135) H18A(0.135) H18B(0.135) H18C(0.135) H19A(0.135) H19B(0.135)
 H19C(0.135) H25A(0.135) H25B(0.135) H25C(0.135)
 Fixed X: O2(1) H(0.5156) H1AA(0.7697) H1AB(0.6831) H1AC(0.7678) H1DA(0.7763)
 H1DB(0.8128) H1DC(0.8579) H1FA(0.7827) H1FB(0.7231) H1FC(0.7476) H1GA(0.9388)
 H1GB(0.9183) H1GC(0.9881) H1HA(1.1567) H1HB(1.057) H1HC(1.1413) H1IA(1.0685)
 H1IB(1.1313) H1IC(1.0573) H1KA(0.9259) H1KB(0.8491) H1KC(0.8246) H1LA(0.8039)
 H1LB(0.8224) H1LC(0.7692) H3(0.6611) H4(0.7051) H6A(0.8229) H6B(0.7798)
 H6C(0.8864) C7(1) H9A(0.5861) H9B(0.5739) H9C(0.6521) H11(0.5588) H12(0.4664)
 H13A(1.0008) H13B(0.9708) H13C(1.0339) H14A(0.6801) H14B(0.5872) H14C(0.6087)
 H16A(1.2438) H16B(1.2144) H16C(1.2707) H18A(1.0168) H18B(1.0831) H18C(1.1034)
 H19A(1.2118) H19B(1.2616) H19C(1.1575) H25A(1.2335) H25B(1.2988) H25C(1.2824)
 Fixed Y: O2(1) H(0.7757) H1AA(0.4836) H1AB(0.4238) H1AC(0.5163) H1DA(0.5725)
 H1DB(0.5184) H1DC(0.6267) H1FA(0.5863) H1FB(0.5467) H1FC(0.483) H1GA(0.6318)
 H1GB(0.5308) H1GC(0.6154) H1HA(1.027) H1HB(0.9395) H1HC(0.9481) H1IA(0.8213)
 H1IB(0.8336) H1IC(0.8663) H1KA(0.5309) H1KB(0.4584) H1KC(0.5161) H1LA(0.5523)
 H1LB(0.5956) H1LC(0.487) H3(0.8765) H4(0.6672) H6A(0.4467) H6B(0.49)
 H6C(0.5223) C7(1) H9A(0.4444) H9B(0.5321) H9C(0.5359) H11(0.5655) H12(0.6209)
 H13A(0.6349) H13B(0.5345) H13C(0.622) H14A(0.529) H14B(0.5186) H14C(0.4371)
 H16A(0.8959) H16B(0.8728) H16C(0.977) H18A(0.7907) H18B(0.7687) H18C(0.7927)
 H19A(1.0044) H19B(1.0801) H19C(1.0464) H25A(0.896) H25B(1.0038) H25C(0.9356)
 Fixed Z: H(0.4561) H1AA(0.5003) H1AB(0.5093) H1AC(0.5147) H1DA(0.4484)
 H1DB(0.4399) H1DC(0.4384) H1FA(0.4411) H1FB(0.4539) H1FC(0.4454) H1GA(0.4406)
 H1GB(0.4439) H1GC(0.4526) H1HA(0.4171) H1HB(0.4153) H1HC(0.4071) H1IA(0.4294)
 H1IB(0.4172) H1IC(0.4165) H1KA(0.4697) H1KB(0.4602) H1KC(0.47) H1LA(0.5101)
 H1LB(0.496) H1LC(0.4978) H3(0.4644) H4(0.4706) H6A(0.4612) H6B(0.4706)
 H6C(0.4715) C7(0.5) H9A(0.513) H9B(0.5117) H9C(0.5208) H11(0.4622) H12(0.4551)
 H13A(0.441) H13B(0.4462) H13C(0.4549) H14A(0.4823) H14B(0.4879) H14C(0.4896)
 H16A(0.4207) H16B(0.4354) H16C(0.4308) H18A(0.4209) H18B(0.4292) H18C(0.4143)
 H19A(0.409) H19B(0.4199) H19C(0.4162) H25A(0.4374) H25B(0.4355) H25C(0.4238)
;
_shelx_hkl_checksum              87531
_shelx_res_checksum              89100
_shelxl_version_number           2013-4