Calix[4]arene-based polyoxometalate organic‒inorganic hybrid and coordination polymer as heterogeneous catalysts for azide‒alkyne cycloaddition and Knoevenagel condensation reaction
Yue, Liu-Juan; Liu, Ying-Ying; Xu, Guo-Hai; Ma, Jian-Fang; New Journal of Chemistry 43 (2019) 15871–; doi:10.1039/C9NJ03930A

data_7058889
_publ_section_title
;
 Calix[4]arene-based polyoxometalate organic--inorganic hybrid and
 coordination polymer as heterogeneous catalysts for azide--alkyne
 cycloaddition and Knoevenagel condensation reaction
;
_journal_issue                   40
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15871
_journal_paper_doi               10.1039/C9NJ03930A
_journal_volume                  43
_journal_year                    2019
_chemical_formula_sum            'C140 H166 Cu4 N10 O52 Si W12'
_chemical_formula_weight         5309.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-09-09 deposited with the CCDC.    2019-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                85.192(5)
_cell_angle_beta                 88.211(4)
_cell_angle_gamma                72.490(5)
_cell_formula_units_Z            1
_cell_length_a                   11.9741(6)
_cell_length_b                   12.1625(8)
_cell_length_c                   28.3572(14)
_cell_measurement_reflns_used    6101
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.2643
_cell_measurement_theta_min      2.9721
_cell_volume                     3924.5(4)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0965
_diffrn_reflns_av_unetI/netI     0.1522
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            24870
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.978
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    9.373
_exptl_absorpt_correction_T_max  0.2558
_exptl_absorpt_correction_T_min  0.1174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.246
_exptl_crystal_description       block
_exptl_crystal_F_000             2510
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         3.849
_refine_diff_density_min         -4.215
_refine_diff_density_rms         0.366
_refine_ls_extinction_coef       0.00152(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     999
_refine_ls_number_reflns         13779
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.0951
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1267P)^2^+14.2173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2397
_refine_ls_wR_factor_ref         0.2706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8451
_reflns_number_total             13779
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj03930a2.cif
_cod_data_source_block           compound-1
_cod_database_code               7058889
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.117
_shelx_estimated_absorpt_t_max   0.256
_plat242
;
PROBLEM: Low 'MainMol' Ueq as Compared to Neighbors of   C39 Check
RESPONSE: The alert comes from the vibration of tertbutyl groups. 
;
_plat342
;
PROBLEM: Low Bond Precison on C-C Bonds      0.0311 Ang.
RESPONSE: The alert is generated because of the moderate data
quality and the vibration of tertbutyl groups. 
;
_shelx_res_checksum              7310
_shelx_fab_checksum              12266