Assembly of Six Polyoxometalate-Based Hybrid Compounds from a Simple Supramolecule to a Complicated Pseudorotaxane Framework via Tuning the pH of the Reaction Systems
Li, Shaobin; Ma, Huiyuan; Pang, Haijun; Zhang, Li; Crystal Growth & Design 14 (2014) 4450–; doi:10.1021/cg5005352

data_4511747
_publ_section_title
;
 Assembly of Six Polyoxometalate-Based Hybrid Compounds from a Simple
 Supramolecule to a Complicated Pseudorotaxane Framework via Tuning the pH
 of the Reaction Systems
;
_journal_issue                   9
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4450
_journal_paper_doi               10.1021/cg5005352
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety
'C28 H30 Cu2 K0.53 N8 O62 P2 W18, C14 H14 Cu N4, 0.47(K)'
_chemical_formula_sum            'C42 H44 Cu3 K N12 O62 P2 W18'
_chemical_formula_weight         5309.67
_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                90.000(5)
_cell_angle_beta                 98.430(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   13.152(5)
_cell_length_b                   25.208(5)
_cell_length_c                   34.395(5)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.27
_cell_measurement_theta_min      2.20
_cell_volume                     11280(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SMART'
_computing_publication_material  'Bruker SMART'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_sigmaI/netI    0.0774
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            56805
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    18.971
_exptl_absorpt_correction_T_max  0.005
_exptl_absorpt_correction_T_min  0.002
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_density_diffrn    3.125
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             9368.0
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         3.591
_refine_diff_density_min         -2.999
_refine_diff_density_rms         0.463
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1267
_refine_ls_number_reflns         19831
_refine_ls_number_restraints     545
_refine_ls_restrained_S_all      0.916
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0718
_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^)+(0.1000P)^2^+1316.6508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1864
_refine_ls_wR_factor_ref         0.1975
_reflns_number_gt                15005
_reflns_number_total             19871
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5005352_si_002.cif
_cod_data_source_block           compound6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/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 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4511742--4511747.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C42 H44 Cu3 K N12 O62 P2 W18 '
_cod_database_code               4511747