Calixarene-supported rare-earth clusters: heteroatom bridge influences cluster composition
Robyn Fairbairn; Ross McLellan; Ruaraidh McIntosh; Stephanie Taylor; Euan Brechin; Scott Dalgarno; Chem.Commun. 48 (2012) 8493–; doi:10.1039/c2cc33166g

data_7108177
_publ_section_title
;
 Calixarene-supported rare-earth clusters: heteroatom bridge influences
 cluster composition
;
_journal_name_full               Chem.Commun.
_journal_page_first              8493
_journal_paper_doi               10.1039/c2cc33166g
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C129 H207 Gd5 N12 O34'
_chemical_formula_weight         3256.32
_chemical_name_common            MonoOxaGd5
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.8340(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.8094(8)
_cell_length_b                   29.6604(11)
_cell_length_c                   23.9915(9)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.15
_cell_measurement_theta_min      2.47
_cell_volume                     14084.4(9)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'Apex II'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8 Apex II CCD Diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_sigmaI/netI    0.0918
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            116484
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    2.398
_exptl_absorpt_correction_T_max  0.7149
_exptl_absorpt_correction_T_min  0.4471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             6628
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
The routine was applied in order to remove density associated
with a very badly disordered dmf molecule. The unit cell
contains 120 electrons that correlates approximately to one
dmf in the asymmetric unit.
;
_refine_diff_density_max         2.363
_refine_diff_density_min         -1.299
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1685
_refine_ls_number_reflns         29878
_refine_ls_number_restraints     297
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+53.8726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1353
_reflns_number_gt                19566
_reflns_number_total             29878
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc33166g.txt
_cod_data_source_block           MOXAC4GD
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7108177