Self-assembled palladium(ii) "click" cages: synthesis, structural modification and stability.
Scott, Synøve Ø; Gavey, Emma L.; Lind, Samuel J.; Gordon, Keith C.; Crowley, James D.; Dalton transactions (Cambridge, England : 2003) 40 (2011) 12117–12124; doi:10.1039/c1dt10551e

data_7017134
_publ_section_title
;
 Self-assembled palladium(ii) "click" cages: synthesis, structural
 modification and stability.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12117
_journal_page_last               12124
_journal_paper_doi               10.1039/c1dt10551e
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C128 H120 B4 F16 N33 O16 Pd2'
_chemical_formula_sum            'C128 H120 B4 F16 N33 O16 Pd2'
_chemical_formula_weight         2936.61
_chemical_name_common            "Pd ''click'' cage"
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 122.689(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.9204(17)
_cell_length_b                   22.5838(14)
_cell_length_c                   24.610(3)
_cell_measurement_reflns_used    6819
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      21.16
_cell_measurement_theta_min      2.50
_cell_volume                     13060(2)
_computing_cell_refinement       'APEX2 and SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXTL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0687
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            43487
_diffrn_reflns_theta_full        21.29
_diffrn_reflns_theta_max         21.29
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    0.376
_exptl_absorpt_correction_T_max  0.9492
_exptl_absorpt_correction_T_min  0.8891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6012
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_platon_squeeze_details
; The unit cell contains 32 acetonitrile molecules
which have been treated as a diffuse contribution
to the overall scattering without specific atom
positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.850
_refine_diff_density_min         -1.147
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     826
_refine_ls_number_reflns         7217
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0997P)^2^+35.7097P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1566
_reflns_number_gt                5761
_reflns_number_total             7217
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c1dt10551e.txt
_cod_data_source_block           seg242
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        13060.2(20)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7017134