Centred nine-metal rings of lanthanides
Karzan H. Zangana; Eufemio Moreno Pineda; Eric J. L. McInnes; Jurgen Schnack; Richard E. P. Winpenny; Chem.Commun. 50 (2014) 1438–; doi:10.1039/c3cc48708c

data_7111845
_publ_section_title
;
 Centred nine-metal rings of lanthanides
;
_journal_name_full               Chem.Commun.
_journal_page_first              1438
_journal_paper_doi               10.1039/c3cc48708c
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C114 H222 Dy10 O59 P6, C45 H69 Co3 N3 O13'
_chemical_formula_sum            'C159 H291 Co3 Dy10 N3 O72 P6'
_chemical_formula_weight         5384.54
_chemical_name_systematic
;
 ?
;
_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             2013-11-11
_audit_creation_method
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Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
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_cell_angle_alpha                105.194(4)
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_cell_formula_units_Z            2
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_cell_length_c                   26.0799(15)
_cell_measurement_reflns_used    10425
_cell_measurement_temperature    150.1(8)
_cell_measurement_theta_max      28.1050
_cell_measurement_theta_min      3.2880
_cell_volume                     11825.6(10)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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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
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      150.1(8)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.9872
_diffrn_measured_fraction_theta_max 0.8216
_diffrn_measurement_details
;
  1 omega  -50.00   45.00   1.0000   88.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9454  -57.0000  150.0000 95

  2 omega   -3.00   90.00   1.0000   88.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9454   57.0000  -60.0000 93

  3 omega  -94.00   10.00   1.0000   88.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  -77.0000   60.0000 104

  4 omega -103.00  -38.00   1.0000   88.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  178.0000 -120.0000 65
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0214748000
_diffrn_orient_matrix_UB_12      0.0115045000
_diffrn_orient_matrix_UB_13      -0.0144596000
_diffrn_orient_matrix_UB_21      0.0132296000
_diffrn_orient_matrix_UB_22      -0.0119005000
_diffrn_orient_matrix_UB_23      -0.0238962000
_diffrn_orient_matrix_UB_31      -0.0248479000
_diffrn_orient_matrix_UB_32      -0.0278134000
_diffrn_orient_matrix_UB_33      -0.0050672000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0905
_diffrn_reflns_av_unetI/netI     0.2053
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            65089
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.983
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.432
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24722
_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_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_description       plate
_exptl_crystal_F_000             5346
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.085
_refine_diff_density_min         -2.218
_refine_diff_density_rms         0.260
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2199
_refine_ls_number_reflns         41489
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1802
_refine_ls_R_factor_gt           0.0903
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+114.1433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1942
_refine_ls_wR_factor_ref         0.2570
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21552
_reflns_number_total             41489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc48708c.txt
_cod_data_source_block           Dy10
_cod_original_cell_volume        11825.5(9)
_cod_database_code               7111845