Intrinsic-Unsaturation-Enriched Biporous and Chemorobust Cu(II) Framework for Efficient Catalytic CO<sub>2</sub> Fixation and Pore-Fitting Actuated Size-Exclusive Hantzsch Condensation with Mechanistic Validation.
Seal, Nilanjan; Neogi, Subhadip; ACS applied materials & interfaces 13 (2021) 55123–55135; doi:10.1021/acsami.1c16984

data_4519130
_publ_section_title
;
 Intrinsic-Unsaturation-Enriched Biporous and Chemorobust Cu(II) Framework
 for Efficient Catalytic CO<sub>2</sub> Fixation and Pore-Fitting Actuated
 Size-Exclusive Hantzsch Condensation with Mechanistic Validation.
;
_journal_issue                   46
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              55123
_journal_page_last               55135
_journal_paper_doi               10.1021/acsami.1c16984
_journal_volume                  13
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C23 H25 N O4'
_chemical_formula_sum            'C23 H25 N O4'
_chemical_formula_weight         379.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-05-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.616(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.8163(6)
_cell_length_b                   9.9332(7)
_cell_length_c                   11.4002(9)
_cell_measurement_reflns_used    10784
_cell_measurement_temperature    280(2)
_cell_measurement_theta_max      27.97
_cell_measurement_theta_min      2.32
_cell_volume                     993.57(13)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      280.15
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10784
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.32
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.9888
_exptl_absorpt_correction_T_min  0.9483
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.4(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4691
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0862P)^2^+0.1399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1403
_refine_ls_wR_factor_ref         0.1581
_reflns_number_gt                3653
_reflns_number_total             4691
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            am1c16984_si_008.cif
_cod_data_source_block           10b
_cod_depositor_comments
;

2025-09-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C46 H50 N2 O8'
_cod_original_formula_weight         758.88
_cod_original_formula_moiety         '2(C23 H25 N O4)'
_cod_original_formula_units_Z            1
_cod_database_code               4519130
_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.a Secondary CH2 refined with riding coordinates:
 C00O(H00I,H00J), C00Q(H00N,H00O)
2.b Aromatic/amide H refined with riding coordinates:
 C009(H009), C00E(H00E), C00G(H00G), C00K(H00K), C00L(H00L), C00M(H00M),
 C00P(H00P)
2.c Idealised Me refined as rotating group:
 C00F(H00A,H00B,H00C), C00J(H00D,H00F,H00H), C00R(H00Q,H00R,H00S), C00S(H00T,
 H00U,H00V)
;
_olex2_submission_special_instructions 'No special instructions were received'