Carboxamide functionality grafted entangled Co(II) framework as unique hydrogen-bond-donor catalyst in solvent-free tandem deacetalization-Knoevenagel condensation with pore-fitting-mediated size-selectivity
Mondal, Partha Pratim Pratim; Seal, Nilanjan; Singh, Manpreet; Neogi, Subhadip; Dalton Transactions  (2023) –; doi:10.1039/D3DT01053H

data_7713190
_publ_section_title
;
 Carboxamide functionality grafted entangled Co(II) framework as unique
 hydrogen-bond-donor catalyst in solvent-free tandem
 deacetalization-Knoevenagel condensation with pore-fitting-mediated
 size-selectivity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01053H
_journal_year                    2023
_chemical_formula_moiety         'C25 H18 Co N4 O5, C3 H7 N O'
_chemical_formula_sum            'C28 H25 Co N5 O6'
_chemical_formula_weight         586.474
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2023-05-03
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2023.03.24 svn.rc9df729e for OlexSys, GUI svn.r6758)
;
_audit_update_record
;
2023-05-25 deposited with the CCDC.	2023-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.579(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7124(4)
_cell_length_b                   21.0705(9)
_cell_length_c                   12.0672(4)
_cell_measurement_reflns_used    5198
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.2420
_cell_measurement_theta_min      2.8470
_cell_volume                     2685.78(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.9975
_diffrn_measured_fraction_theta_max 0.9975
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     18.00 113.10   0.30   15.00    --   29.89  54.00-150.00  317
  2  \w    -67.00  52.10   0.30   15.00    --   29.89  54.00 -30.00  397
  3  \w     93.00 118.20   0.30   15.00    --   29.89  54.00 -30.00   84
  4  \w    -69.00  -6.00   0.30   15.00    --   29.89  54.00-150.00  210
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.9975
_diffrn_reflns_Laue_measured_fraction_max 0.9975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20283
_diffrn_reflns_point_group_measured_fraction_full 0.9975
_diffrn_reflns_point_group_measured_fraction_max 0.9975
_diffrn_reflns_theta_full        24.9991
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       needle
_exptl_crystal_F_000             1214.289
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.2005
_refine_diff_density_min         -0.5783
_refine_diff_density_rms         0.0857
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             7.9988
_refine_ls_goodness_of_fit_ref   1.0528
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    56
_refine_ls_number_parameters     410
_refine_ls_number_reflns         4720
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.0429
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0811P)^2^+2.2767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1382
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                4119
_reflns_number_total             4720
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt01053h2.cif
_cod_data_source_block           CSMCRI-MOF-25
_cod_original_cell_volume        2685.78(17)
_cod_database_code               7713190
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N00Z-C011 \\sim N0-C1
 with sigma of 0.02
 N00Z-C012 \\sim N0-C2
 with sigma of 0.02
 N00Z-C014 \\sim N0-C0
 with sigma of 0.02
 O013-C014 \\sim O0-C0
 with sigma of 0.02
 N00Z-O013 \\sim N0-O0
 with sigma of 0.04
 C011-C012 \\sim C1-C2
 with sigma of 0.04
 C011-C014 \\sim C1-C0
 with sigma of 0.04
 C012-C014 \\sim C2-C0
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C2 \\sim C014: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C1 \\sim C011: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C012 \\sim C0: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
4. Rigid body (RIGU) restrains
 O0, C0, N0, C1, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O013, N00Z, C011, C012, C014
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N00Z(0.6) C011(0.6) H01a(0.6) H01b(0.6) H01c(0.6) C012(0.6)
 H01d(0.6) H01e(0.6) H01f(0.6) O013(0.6) C014(0.6) H014(0.6) C0(0.4) H0(0.4)
 N0(0.4) C1(0.4) H1a(0.4) H1b(0.4) H1c(0.4) C2(0.4) H2a(0.4) H2b(0.4) H2c(0.4)
 O0(0.4)
6.a Aromatic/amide H refined with riding coordinates:
 N009(H009), N00A(H00A), C00D(H00D), C00E(H00E), C00H(H00H), C00I(H00I),
 C00J(H00J), C00K(H00K), C00M(H00M), C00N(H00N), C00P(H00P), C00R(H00R),
 C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y), C010(H010),
 C014(H014), C0(H0)
6.b Idealised Me refined as rotating group:
 C011(H01a,H01b,H01c), C012(H01d,H01e,H01f), C1(H1a,H1b,H1c), C2(H2a,H2b,H2c)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;