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_4511745
_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         'C49 H48 Cu2 N14 O40 P W12, 0.5(C14 H14 N4)'
_chemical_formula_sum            'C56 H55 Cu2 N16 O40 P W12'
_chemical_formula_weight         3956.31
_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                 99.291(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   15.117(5)
_cell_length_b                   24.346(5)
_cell_length_c                   24.353(5)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.17
_cell_volume                     8845(4)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0606
_diffrn_reflns_av_sigmaI/netI    0.0701
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            44158
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    16.111
_exptl_absorpt_correction_T_max  0.015
_exptl_absorpt_correction_T_min  0.008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_density_diffrn    2.971
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7136.0
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         14.159
_refine_diff_density_min         -3.467
_refine_diff_density_rms         0.611
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1144
_refine_ls_number_reflns         15446
_refine_ls_number_restraints     411
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0835
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0776P)^2^+1541.6389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2230
_refine_ls_wR_factor_ref         0.2372
_reflns_number_gt                11654
_reflns_number_total             15568
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5005352_si_002.cif
_cod_data_source_block           compound4
_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        'C56 H55 Cu2 N16 O40 P W12 '
_cod_database_code               4511745