A highly stable polyoxovanadate-based Cu(i)‒MOF for the carboxylative cyclization of CO2 with propargylic alcohols at room temperature
Tian, Hong-Rui; Zhang, Zhong; Liu, Shu-Mei; Dang, Tian-Yi; Li, Zhuo; Lu, Ying; Liu, Shu-Xia; Green Chemistry 22 (2020) 7513–7520; doi:10.1039/D0GC02812F

data_7241315
_publ_section_title
;
 A highly stable polyoxovanadate-based Cu(i)--MOF for the carboxylative
 cyclization of CO2 with propargylic alcohols at room temperature
;
_journal_issue                   21
_journal_name_full               'Green Chemistry'
_journal_page_first              7513
_journal_page_last               7520
_journal_paper_doi               10.1039/D0GC02812F
_journal_volume                  22
_journal_year                    2020
_chemical_formula_moiety         'C24 H20 Cu2 N8 O6 V2'
_chemical_formula_sum            'C24 H20 Cu2 N8 O6 V2'
_chemical_formula_weight         745.45
_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_Int_Tables_number      2
_audit_creation_date             2018-04-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2020-08-10 deposited with the CCDC.	2020-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                63.651(2)
_cell_angle_beta                 75.955(2)
_cell_angle_gamma                61.239(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6196(4)
_cell_length_b                   12.0604(5)
_cell_length_c                   12.2162(4)
_cell_measurement_reflns_used    8083
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.70
_cell_measurement_theta_min      2.78
_cell_volume                     1343.91(9)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293.0
_diffrn_measured_fraction_theta_full 0.9961
_diffrn_measured_fraction_theta_max 0.9961
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23387
_diffrn_reflns_theta_full        25.7386
_diffrn_reflns_theta_max         25.74
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    2.292
_exptl_absorpt_correction_T_max  0.6571
_exptl_absorpt_correction_T_min  0.6325
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.8420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             746.8784
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.5296
_refine_diff_density_min         -0.4888
_refine_diff_density_rms         0.1120
_refine_ls_d_res_high            0.8183
_refine_ls_d_res_low             7.5938
_refine_ls_goodness_of_fit_ref   1.0720
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    40
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5117
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.0713
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+0.8106P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0681
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -13
_reflns_limit_k_max              14
_reflns_limit_k_min              -12
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                4082
_reflns_number_total             5117
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0gc02812f2.cif
_cod_data_source_block           5
_cod_depositor_comments          'Adding full bibliography for 7241315.cif.'
_cod_database_code               7241315
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 Cu1, O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Cu1 \\sim O1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C1(H1), C23(H23), C11(H11), C3(H3), C2(H2), C10(H10), C14(H14),
 C20(H20), C24(H24), C18(H18), C21(H21), C5(H5), C12(H12), C6(H6), C15(H15),
 C7(H7), C17(H17), C8(H8), C9(H9)
;
_olex2_submission_special_instructions 'No special instructions were received'