Tetrametallic lanthanide(III) phosphonate cages: synthetic, structural and magnetic studies.
Zangana, Karzan H.; Pineda, Eufemio Moreno; Winpenny, Richard E. P.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 17101–17107; doi:10.1039/c4dt02630f

data_7702016
_publ_section_title
;
 Tetrametallic lanthanide(III) phosphonate cages: synthetic, structural
 and magnetic studies.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17101
_journal_page_last               17107
_journal_paper_doi               10.1039/c4dt02630f
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C26 H56 Er4 N6 O35 P4, 4(C5 H6 N)'
_chemical_formula_sum            'C46 H80 Er4 N10 O35 P4'
_chemical_formula_weight         2084.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-08-27
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.3155(18)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   44.7348(10)
_cell_length_b                   19.1138(4)
_cell_length_c                   23.8851(4)
_cell_measurement_reflns_used    13812
_cell_measurement_temperature    150.03(18)
_cell_measurement_theta_max      27.7920
_cell_measurement_theta_min      3.3340
_cell_volume                     20417.6(7)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.03(18)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -64.00   54.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.3942   77.0000  -30.0000 118

  2 omega  -65.00   53.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.3942   77.0000 -150.0000 118

  3 omega  -14.00  104.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       25.8629   77.0000   90.0000 118
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0033212000
_diffrn_orient_matrix_UB_12      0.0355863000
_diffrn_orient_matrix_UB_13      0.0055632000
_diffrn_orient_matrix_UB_21      0.0154980000
_diffrn_orient_matrix_UB_22      0.0078275000
_diffrn_orient_matrix_UB_23      0.0009177000
_diffrn_orient_matrix_UB_31      -0.0005035000
_diffrn_orient_matrix_UB_32      0.0069750000
_diffrn_orient_matrix_UB_33      -0.0291761000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            54167
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.009
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.382
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55136
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) 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    1.356
_exptl_crystal_description       plate
_exptl_crystal_F_000             8116
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.194
_refine_diff_density_min         -1.749
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     872
_refine_ls_number_reflns         20804
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0437P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15116
_reflns_number_total             20804
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt02630f2.cif
_cod_data_source_block           Er4P4
_cod_database_code               7702016
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         Er4P4O20H100C50N4
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
Big solvent Voids are obtained during the first 
modelling of the data, due to non-localised solvent molecules. 
In order to get an idea of how many solvent molecules occupies the 
empty space, a SQUEZZE procedure was performed. A total of 1291 
electron counts were found, which were attributed to a total of 
31 molecules of isobutanol (42 electron counts per molecule). 
These molecules have been added to the molecular formula in the cif file
and not to the _chemical_formula_sum.

_chemical_formula_moiety          'C26 H56 Er4 N6 O35 P4, 4(C5 H6 N), 31(C5 H5 N)'
_chemical_formula_sum             'C201 H235 Er4 N41 O35 P4'
;
_shelx_res_checksum              63048
_olex2_submission_special_instructions 'No special instructions were received'