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_7058890
_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_moiety         'C68 H76 Cd Cl2 N4 O4, C2 H3 N'
_chemical_formula_sum            'C70 H79 Cd Cl2 N5 O4'
_chemical_formula_weight         1237.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2ac 2b'
_space_group_name_H-M_alt        'P b n a'
_symmetry_space_group_name_Hall  '-P 2ac 2b'
_symmetry_space_group_name_H-M   'P b n a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-08-24
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2019.03.18 svn.r3573 for OlexSys, GUI svn.r5796)
;
_audit_update_record
;
2019-09-09 deposited with the CCDC.    2019-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.1543(5)
_cell_length_b                   24.6370(8)
_cell_length_c                   42.2769(16)
_cell_measurement_reflns_used    18681
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.0540
_cell_measurement_theta_min      3.6940
_cell_volume                     13701.2(9)
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            77525
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.262
_exptl_absorpt_coefficient_mu    0.445
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5184
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     814
_refine_ls_number_reflns         12050
_refine_ls_number_restraints     140
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0421P)^2^+11.1393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1039
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10158
_reflns_number_total             12050
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj03930a2.cif
_cod_data_source_block           compound-2
_cod_database_code               7058890
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C52-C57 \\sim C52-C57A
 with sigma of 0.02
 C57-C59 \\sim C57A-C59A
 with sigma of 0.02
 C52-C58 \\sim C52-C58A
 with sigma of 0.04
 C52-C59 \\sim C52-C59A
 with sigma of 0.04
 C52-C60 \\sim C52-C60A
 with sigma of 0.04
 C57-C58 \\sim C57A-C58A
 with sigma of 0.04
 C57-C60 \\sim C57A-C60A
 with sigma of 0.04
 C58-C59 \\sim C58A-C59A
 with sigma of 0.04
 C58-C60 \\sim C58A-C60A
 with sigma of 0.04
 C59-C60 \\sim C59A-C60A
 with sigma of 0.04
 C66-C68 \\sim C66-C68A
 with sigma of 0.02
 C68-C69 \\sim C68A-C69A
 with sigma of 0.02
 C68-C70 \\sim C68A-C70A
 with sigma of 0.02
 C68-C71 \\sim C68A-C71A
 with sigma of 0.02
 C66-C69 \\sim C66-C69A
 with sigma of 0.04
 C66-C70 \\sim C66-C70A
 with sigma of 0.04
 C66-C71 \\sim C66-C71A
 with sigma of 0.04
 C69-C70 \\sim C69A-C70A
 with sigma of 0.04
 C69-C71 \\sim C69A-C71A
 with sigma of 0.04
 C70-C71 \\sim C70A-C71A
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C66, C68, C69, C70, C71
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C57, C58, C59, C60, C52
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C68A, C69A, C70A, C71A, C66
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C57A, C58A, C59A, C60A, C52
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C57A)=Sof(C58A)=Sof(H58D)=Sof(H58E)=Sof(H58F)=Sof(C59A)=Sof(H59D)=
 Sof(H59E)=Sof(H59F)=Sof(C60A)=Sof(H60D)=Sof(H60E)=Sof(H60F)=1-FVAR(1)
 Sof(C57)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=Sof(C59)=Sof(H59A)=Sof(H59B)=
 Sof(H59C)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=FVAR(1)
 Sof(C68A)=Sof(C69A)=Sof(H69D)=Sof(H69E)=Sof(H69F)=Sof(C70A)=Sof(H70D)=
 Sof(H70E)=Sof(H70F)=Sof(C71A)=Sof(H71D)=Sof(H71E)=Sof(H71F)=1-FVAR(2)
 Sof(C68)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=Sof(C70)=Sof(H70A)=Sof(H70B)=
 Sof(H70C)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C19(H19A,H19B), C25(H25A,H25B), C37(H37A,H37B),
 C50(H50A,H50B), C61(H61A,H61B), C72(H72A,H72B)
5.b Me refined with riding coordinates:
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C11(H11), C7(H7), C9(H9), C10(H10), C14(H14),
 C15(H15), C16(H16), C18(H18), C20(H20), C22(H22), C23(H23), C24(H24), C29(H29),
  C31(H31), C41(H41), C43(H43), C51(H51), C56(H56), C65(H65), C67(H67)
5.d Fitted hexagon refined as free rotating group:
 C11(N1,C7,C8,C9,C10)
5.e Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C69(H69A,H69B,
 H69C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C73(H73A,H73B,H73C),
 C58A(H58D,H58E,H58F), C59A(H59D,H59E,H59F), C60A(H60D,H60E,H60F), C69A(H69D,
 H69E,H69F), C70A(H70D,H70E,H70F), C71A(H71D,H71E,H71F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              37790
_shelx_fab_checksum              1872
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'