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_4511746
_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         'C35 H41 Cu N10 O63 P2 W18, C14 H14 N4, 2H2O'
_chemical_formula_sum            'C49 H55 Cu N14 O65 P2 W18'
_chemical_formula_weight         5318.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.425(5)
_cell_angle_beta                 83.881(5)
_cell_angle_gamma                81.521(5)
_cell_formula_units_Z            2
_cell_length_a                   14.505(5)
_cell_length_b                   15.007(5)
_cell_length_c                   22.506(5)
_cell_measurement_reflns_used    7491
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.19
_cell_volume                     4818(3)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0853
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24119
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.91
_exptl_absorpt_coefficient_mu    21.743
_exptl_absorpt_correction_T_max  0.004
_exptl_absorpt_correction_T_min  0.003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_density_diffrn    3.659
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4704.0
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.26
_refine_diff_density_max         3.822
_refine_diff_density_min         -5.253
_refine_diff_density_rms         0.558
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1349
_refine_ls_number_reflns         16719
_refine_ls_number_restraints     438
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1019P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1486
_refine_ls_wR_factor_ref         0.1671
_reflns_number_gt                12258
_reflns_number_total             16974
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5005352_si_002.cif
_cod_data_source_block           compound5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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-1
_cod_original_formula_sum        'C49 H55 Cu N14 O65 P2 W18 '
_cod_database_code               4511746