Anchoring Ag(I) into Nitro-Functionalized Metal-Organic Frameworks: Effectively Catalyzing Cycloaddition of CO<sub>2</sub> with Propargylic Alcohols under Mild Conditions.
Zhao, Jian; Jiao, Zhuo-Hao; Hou, Sheng-Li; Ma, Yue; Zhao, Bin; ACS applied materials & interfaces 13 (2021) 45558–45565; doi:10.1021/acsami.1c13438

data_4519049
_publ_section_title
;
 Anchoring Ag(I) into Nitro-Functionalized Metal-Organic Frameworks:
 Effectively Catalyzing Cycloaddition of CO<sub>2</sub> with Propargylic
 Alcohols under Mild Conditions.
;
_journal_issue                   38
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              45558
_journal_page_last               45565
_journal_paper_doi               10.1021/acsami.1c13438
_journal_volume                  13
_journal_year                    2021
_chemical_formula_moiety
'C35 H24 Co1.5 N5 O9, C5 H4 N, 0.5(C3 H7 N O), 0.5(H2 O)'
_chemical_formula_sum            'C41.5 H32.5 Co1.5 N6.5 O10'
_chemical_formula_weight         870.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-07-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                99.740(4)
_cell_angle_beta                 97.790(4)
_cell_angle_gamma                108.442(4)
_cell_formula_units_Z            2
_cell_length_a                   10.8396(5)
_cell_length_b                   11.4532(6)
_cell_length_c                   17.5160(9)
_cell_measurement_reflns_used    4476
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5810
_cell_measurement_theta_min      3.6550
_cell_volume                     1991.16(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13319
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.15
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.700
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             895
_refine_diff_density_max         1.136
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         7000
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0771P)^2^+3.2931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1637
_reflns_number_gt                5502
_reflns_number_total             7000
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            am1c13438_si_002.cif
_cod_data_source_block           p180810c1_sqd
_cod_original_cell_volume        1991.16(17)
_cod_original_formula_sum        'C41.50 H32.50 Co1.50 N6.50 O10'
_cod_database_code               4519049
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O3-N01C \\sim N01C-O2
 with sigma of 0.02
 O1B-N01C \\sim N01C-O1A
 with sigma of 0.02
 O3-N01C \\sim N01C-O1B
 with sigma of 0.02
 O3-N01C \\sim N01C-O1A
 with sigma of 0.02
 O1B-N01C \\sim N01C-O2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1B) \\sim Ueq, Uanis(O1A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
4. Others
 Sof(O3)=1-FVAR(1)
 Sof(O2)=FVAR(1)
 Sof(O1B)=1-FVAR(2)
 Sof(O1A)=FVAR(2)
 Fixed Sof: O0AA(0.5) N1(0.5) C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) C3(0.5)
 H3A(0.5) H3B(0.5) H3C(0.5) C7(0.5) H7(0.5) O1(0.5) H1A(0.5) H1B(0.5)
5.a Riding coordinates:
 O007(H00A,H00B), O1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N),
 C00O(H00O), C00Q(H00Q), C00S(H00S), C00T(H00T), C00U(H00U), C00W(H00W),
 C00X(H00X), C010(H010), C011(H011), C012(H012), C013(H013), C014(H014),
 C019(H019), C01B(H01B), C01D(H01D), C01F(H01F), C01G(H01G), C01H(H01H),
 C01I(H01I), C01J(H01J), C7(H7)
5.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
;
_olex2_submission_special_instructions 'No special instructions were received'