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_4343288
_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 Er9 O55 P6, C8 H12 Cu1 N4'
_chemical_formula_sum            'C107 H201 Cu4 Er9 N4 O55 P6'
_chemical_formula_weight         4369.02
_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                   20.5114(3)
_cell_length_b                   20.5114(3)
_cell_length_c                   32.7097(5)
_cell_measurement_reflns_used    5765
_cell_measurement_temperature    150.1(1)
_cell_measurement_theta_max      29.1980
_cell_measurement_theta_min      3.0890
_cell_volume                     11917.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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      150.1(1)
_diffrn_detector_area_resol_mean 10.3705
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -38.00   51.00   1.0000   10.2500
omega____ theta____ kappa____ phi______ frames
    -      -11.6555   19.0000    0.0000 89
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0223375333
_diffrn_orient_matrix_UB_12      -0.0175135333
_diffrn_orient_matrix_UB_13      -0.0002690333
_diffrn_orient_matrix_UB_21      -0.0078164333
_diffrn_orient_matrix_UB_22      -0.0080015667
_diffrn_orient_matrix_UB_23      -0.0211091667
_diffrn_orient_matrix_UB_31      0.0321506000
_diffrn_orient_matrix_UB_32      0.0349776000
_diffrn_orient_matrix_UB_33      -0.0049442000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_laue_measured_fraction_full 0.993
_diffrn_reflns_laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            9342
_diffrn_reflns_point_group_measured_fraction_full 0.679
_diffrn_reflns_point_group_measured_fraction_max 0.660
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.742
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.354
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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    1.826
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             6387
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.186
_refine_ls_abs_structure_details
;
 Flack x determined using 1670 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.025(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         7154
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0324
_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^)+166.6583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0673
_reflns_Friedel_coverage         0.332
_reflns_friedel_fraction_full    0.366
_reflns_friedel_fraction_max     0.329
_reflns_number_gt                6742
_reflns_number_total             7154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00649_si_002.cif
_cod_data_source_block           Cu3Er9P6
_cod_original_cell_volume        11917.9(4)
_cod_database_code               4343288
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         Cu3Er9O32P6C100H100
_reflns_odcompleteness_completeness 99.15
_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(C15) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C13) \\sim Ueq, Uanis(C3P) \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
3. Others
 Fixed Sof: H29A(0.33333) H29B(0.33333) H29C(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), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C)
;
_olex2_date_sample_data_collection 2013-10-19
_olex2_submission_special_instructions 'No special instructions were received'