Preparation of Core-Shell Coordination Molecular Assemblies via the Enrichment of Structure-Directing "Codes" of Bridging Ligands and Metathesis of Metal Units.
Park, Jinhee; Chen, Ying-Pin; Perry, Zachary; Li, Jian-Rong; Zhou, Hong-Cai; Journal of the American Chemical Society  (2014) 141120112955009–; doi:10.1021/ja508822r

data_4122977
_publ_section_title
;
 Preparation of Core-Shell Coordination Molecular Assemblies via the
 Enrichment of Structure-Directing &quot;Codes&quot; of Bridging Ligands
 and Metathesis of Metal Units.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              141120112955009
_journal_paper_doi               10.1021/ja508822r
_journal_year                    2014
_chemical_formula_moiety         'C252 H156 Mo12 N36 O80'
_chemical_formula_sum            'C252 H156 Mo12 N36 O80'
_chemical_formula_weight         6119.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_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                   31.220(10)
_cell_length_b                   31.220(10)
_cell_length_c                   24.656(8)
_cell_measurement_reflns_used    3977
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      18.48
_cell_measurement_theta_min      2.48
_cell_volume                     24032(13)
_computing_cell_refinement       'SAINT+ ver. (Bruker, 2001)'
_computing_data_collection       'APEX2  (Bruker, 2008)'
_computing_data_reduction        'SAINT+ ver. (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1934
_diffrn_reflns_av_sigmaI/netI    0.1880
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            86231
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.352
_exptl_absorpt_correction_T_max  0.9329
_exptl_absorpt_correction_T_min  0.8720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    0.846
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             6128
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         1.319
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.106
_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     237
_refine_ls_number_reflns         9669
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.2542
_refine_ls_R_factor_gt           0.1353
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+390.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2555
_refine_ls_wR_factor_ref         0.2847
_reflns_number_gt                3281
_reflns_number_total             9669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja508822r_si_005.cif
_cod_data_source_block           i4m_nodma_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        24032(14)
_cod_original_sg_symbol_H-M      I4/m
_cod_database_code               4122977