High-Nuclearity Metal-Organic Nanospheres: A Cd66 Ball
Stephen P. Argent; Alex Greenaway; Maria del Carmen Gimenez-Lopez; William Lewis; Harriott Nowell; Andrei N. Khlobystov; Alexander J. Blake; Neil R. Champness; Martin Schröder; Journal of the American Chemical Society 134 (2012) 55–58; doi:10.1021/ja207845u

data_4117231
_publ_section_title
;
 High-Nuclearity Metal-Organic Nanospheres: A Cd66 Ball
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              55
_journal_page_last               58
_journal_paper_doi               10.1021/ja207845u
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C954 H624 Cd66 N20 O220, 96(C3 H7 N O)'
_chemical_formula_sum            'C1242 H1296 Cd66 N116 O316'
_chemical_formula_weight         30322.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           48
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2bc'
_symmetry_space_group_name_H-M   'P n n n :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   35.4763(2)
_cell_length_b                   43.6363(3)
_cell_length_c                   48.9095(3)
_cell_measurement_reflns_used    44383
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      24.8426
_cell_measurement_theta_min      1.4901
_cell_volume                     75714.6(8)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -61.00  116.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000    0.0000  120.0000 354

;
_diffrn_measurement_device_type  'Rigaku Saturn 724+'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  'silicon double crystal'
_diffrn_radiation_source         'Diamond Light Source Beamline I19'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            202795
_diffrn_reflns_theta_full        24.21
_diffrn_reflns_theta_max         24.21
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       column
_exptl_crystal_F_000             30512
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
;
_refine_diff_density_max         1.843
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2682
_refine_ls_number_reflns         66838
_refine_ls_number_restraints     5469
_refine_ls_restrained_S_all      1.339
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0694P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1405
_refine_ls_wR_factor_ref         0.1497
_reflns_number_gt                44626
_reflns_number_total             66838
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja207845u_si_001_2.cif
_cod_data_source_block           spa76
_cod_original_cell_volume        75714.5(9)
_cod_original_sg_symbol_H-M      'P n n n'
_cod_database_code               4117231
_nottingham_internal_coll_name   SPA76
_nottingham_internal_coll_number 9751
_nottingham_internal_coll_client SPA/MS/NRC
_nottingham_internal_coll_type   Diamond
_nottingham_internal_coll_frame_time 1s
_nottingham_internal_coll_frame_width 0.5
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_user   AG/AJB
_nottingham_internal_coll_date   25/10/2011
_nottingham_internal_process_date 25/10/2011
_nottingham_internal_solution_user SPA
_nottingham_internal_solution_date 26/10/2011
_nottingham_internal_refinement_user SPA
_nottingham_internal_refinement_date 25/05/2011