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_4122978
_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
'(Cu4 C84 H52 O26 N12) (Cu1.6 Mo6.4 C168 H104 O52 N24)'
_chemical_formula_sum            'C252 H156 Cu5.6 Mo6.4 N36 O78'
_chemical_formula_weight         5905.97
_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                   31.22(3)
_cell_length_b                   31.22(3)
_cell_length_c                   25.05(3)
_cell_measurement_reflns_used    1388
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      20.3178
_cell_measurement_theta_min      2.4595
_cell_volume                     24416(4)
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.1836
_diffrn_reflns_av_sigmaI/netI    0.3706
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25881
_diffrn_reflns_theta_full        24.82
_diffrn_reflns_theta_max         24.82
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.446
_exptl_absorpt_correction_T_max  0.9568
_exptl_absorpt_correction_T_min  0.9568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    0.803
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             5950
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         1.136
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         10619
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.3304
_refine_ls_R_factor_gt           0.1434
_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^+120.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2659
_refine_ls_wR_factor_ref         0.3150
_reflns_number_gt                1787
_reflns_number_total             10619
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja508822r_si_006.cif
_cod_data_source_block           mo3_3020
_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        24416(44)
_cod_original_sg_symbol_H-M      I4/m
_cod_original_formula_sum        'C252 H156 Cu5.60 Mo6.40 N36 O78'
_cod_database_code               4122978