Exploring the Programmable Assembly of a Polyoxometalate-Organic Hybrid via Metal Ion Coordination
Panchao Yin; Tao Li; Ross S. Forgan; Claire Lydon; Xiaobing Zuo; Zhaoxiong Norm Zheng; Byeongdu Lee; Deliang Long; Leroy Cronin; Tianbo Liu; Journal of the American Chemical Society 135 (2013) 13425–13432; doi:10.1021/ja404777g

data_4120759
_publ_section_title
;
 Exploring the Programmable Assembly of a Polyoxometalate-Organic Hybrid
 via Metal Ion Coordination
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13425
_journal_page_last               13432
_journal_paper_doi               10.1021/ja404777g
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C180 H382 N14 O126 P4 V6 W30'
_chemical_formula_weight         10704.02
_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                 93.178(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.4135(5)
_cell_length_b                   28.3495(10)
_cell_length_c                   34.4392(12)
_cell_measurement_reflns_used    8438
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.1
_cell_measurement_theta_min      2.29
_cell_volume                     15025.6(9)
_computing_cell_refinement       Apex2
_computing_data_collection       Apex2
_computing_data_reduction        Apex2
_computing_molecular_graphics    Diamond3
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker ApexII Quasar CCD'
_diffrn_measurement_method       '\w & \p 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  0.1054
_diffrn_reflns_av_sigmaI/netI    0.1864
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            84776
_diffrn_reflns_theta_full        24.22
_diffrn_reflns_theta_max         24.22
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    11.707
_exptl_absorpt_correction_T_max  0.7202
_exptl_absorpt_correction_T_min  0.3340
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.366
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             9972
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
Summary and Remarks : N = NOTE, W = WARNING, E = ERROR
================================================================================

W: Coordinates do not form a Connected Set
N: DISORDERED structure - ATOMS with Pop. .LT. 1.0 are not moved or as a group.
--------------------------------------------------------------------------------
N: Number of Isotropic Non-H Atoms .......................................   54
N: Number of moved primary input atoms: ..................................  228
W: Number of unusual anisotropic displacement parameters .................    8
N: Total Potential Solvent Accessible Void Vol ..................  5680.3 Ang^3
N: Electron Count / Cell =   4396 - To be included in D(calc), F000 & Mol.Wght.

================================================================================
;
_refine_diff_density_max         3.48
_refine_diff_density_min         -1.81
_refine_diff_density_rms         0.35
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         23950
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.1610
_refine_ls_R_factor_gt           0.0822
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1107P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2163
_refine_ls_wR_factor_ref         0.2384
_reflns_number_gt                10217
_reflns_number_total             23950
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja404777g_si_001.cif
_cod_data_source_block           cl578
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 
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_cod_database_code               4120759