Octametallic 4f-phosphonate horseshoes.
Zangana, Karzan H.; Pineda, Eufemio Moreno; Schnack, Jürgen; Winpenny, Richard E. P.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 14045–14048; doi:10.1039/c3dt52086b

data_7021985
_publ_section_title
;
 Octametallic 4f-phosphonate horseshoes.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14045
_journal_page_last               14048
_journal_paper_doi               10.1039/c3dt52086b
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C88 H175 O47 P6 Tb8, 2(C3 H10 N)'
_chemical_formula_sum            'C94 H195 N2 O47 P6 Tb8'
_chemical_formula_weight         3562.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-08-14
_audit_creation_method
;
  Olex2 1.2
  (compiled 2013.04.25 svn.r2679, GUI svn.r4466)
;
_audit_update_record
;
2013-08-14 # Formatted by publCIF
;
_cell_angle_alpha                76.727(4)
_cell_angle_beta                 75.084(4)
_cell_angle_gamma                82.955(4)
_cell_formula_units_Z            2
_cell_length_a                   14.0342(7)
_cell_length_b                   24.0928(11)
_cell_length_c                   26.4594(12)
_cell_measurement_reflns_used    6325
_cell_measurement_temperature    150.05(16)
_cell_measurement_theta_max      27.4570
_cell_measurement_theta_min      3.2760
_cell_volume                     8394.9(7)
_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
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      150.05(16)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.9846
_diffrn_measured_fraction_theta_max 0.8210
_diffrn_measurement_details
;
  1 omega  -49.00   54.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8673  -77.0000 -180.0000 103

  2 omega  -94.00   10.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  -77.0000   60.0000 104

  3 omega  -94.00   11.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  -77.0000  -60.0000 105
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0432452000
_diffrn_orient_matrix_UB_12      0.0014182000
_diffrn_orient_matrix_UB_13      0.0086994000
_diffrn_orient_matrix_UB_21      -0.0257447000
_diffrn_orient_matrix_UB_22      0.0196744000
_diffrn_orient_matrix_UB_23      0.0158818000
_diffrn_orient_matrix_UB_31      -0.0146709000
_diffrn_orient_matrix_UB_32      -0.0230232000
_diffrn_orient_matrix_UB_33      0.0218168000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0900
_diffrn_reflns_av_unetI/netI     0.2421
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            46157
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.035
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.441
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40051
_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            'clear ? colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       plate
_exptl_crystal_F_000             3516
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.395
_refine_diff_density_min         -1.855
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1206
_refine_ls_number_reflns         33802
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      2.761
_refine_ls_R_factor_all          0.1687
_refine_ls_R_factor_gt           0.0782
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0407P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1568
_refine_ls_wR_factor_ref         0.2034
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15334
_reflns_number_total             33802
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt52086b.txt
_cod_data_source_block           Tb8P6
_cod_database_code               7021985