Copper Lanthanide Phosphonate Cages: Highly Symmetric {Cu3Ln9P6} and {Cu6Ln6P6} Clusters with C3v and D3h Symmetry.
Moreno Pineda, Eufemio; Heesing, Christian; Tuna, Floriana; Zheng, Yan-Zhen; McInnes, Eric J. L.; Schnack, Jürgen; Winpenny, Richard E. P.; Inorganic chemistry  (2015) 150610150327001–; doi:10.1021/acs.inorgchem.5b00649

data_4343293
_publ_section_title
;
 Copper Lanthanide Phosphonate Cages: Highly Symmetric {Cu3Ln9P6} and
 {Cu6Ln6P6} Clusters with C3v and D3h Symmetry.
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              150610150327001
_journal_paper_doi               10.1021/acs.inorgchem.5b00649
_journal_year                    2015
_chemical_formula_moiety         'C99 H189 Cu3 Dy9 O55 P6, C8 H12 Cu1 N4'
_chemical_formula_sum            'C107 H201 Cu4 Dy9 N4 O55 P6'
_chemical_formula_weight         4326.18
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3'
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   20.5394(4)
_cell_length_b                   20.5394(4)
_cell_length_c                   32.7197(7)
_cell_measurement_reflns_used    25876
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.3515
_cell_measurement_theta_min      1.6878
_cell_volume                     11954.1(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega    2.20  182.15   0.2999   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000   73.8966  -25.8022 600

  2 omega    2.20  182.15   0.2999   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000   73.8966   94.1986 600

  3 omega    2.20  182.15   0.2999   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000   73.8966  214.1966 600
;
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0197929000
_diffrn_orient_matrix_UB_12      -0.0233668000
_diffrn_orient_matrix_UB_13      -0.0168175000
_diffrn_orient_matrix_UB_21      -0.0255294000
_diffrn_orient_matrix_UB_22      0.0137681000
_diffrn_orient_matrix_UB_23      0.0005143000
_diffrn_orient_matrix_UB_31      0.0234008000
_diffrn_orient_matrix_UB_32      0.0292241000
_diffrn_orient_matrix_UB_33      -0.0136617000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            31896
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.409
_diffrn_reflns_theta_min         1.691
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.818
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             6333
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.326
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details
;
 Flack x determined using 4161 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.494(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         10816
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0260P)^2^+143.5550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0903
_reflns_Friedel_coverage         0.981
_reflns_friedel_fraction_full    0.987
_reflns_friedel_fraction_max     0.977
_reflns_number_gt                9517
_reflns_number_total             10816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00649_si_008.cif
_cod_data_source_block           Cu3Dy9P6
_cod_original_cell_volume        11954.1(6)
_cod_database_code               4343293
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         Cu4Dy9P6N4O55C107H201
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: H4NA(0.33333) H4NB(0.33333) H4NC(0.33333)
4.a Idealised Me refined as rotating group:
 C2P(H2PA,H2PB,H2PC), C3(H3A,H3B,H3C), C3P(H3PA,H3PB,H3PC), C4(H4A,H4B,H4C),
 C4P(H4PA,H4PB,H4PC), C5(H5A,H5B,H5C), C6P(H6PA,H6PB,H6PC), C7P(H7PA,H7PB,H7PC),
  C8(H8A,H8B,H8C), C8P(H8PA,H8PB,H8PC), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C2N(H2NA,H2NB,H2NC), C4N(H4NA,H4NB,H4NC)
;
_olex2_submission_special_instructions 'No special instructions were received'