Facile fabrication in coordination networks: an in situ sequential replacement of linkers by successive SC–SC transformations via core@shell crystals
Ebrahimi, Bahare; Notash, Behrouz; CrystEngComm 26 (2024) 4720–4731; doi:10.1039/D4CE00632A

data_7249086
_publ_section_title
;
 Facile fabrication in coordination networks: an in situ sequential
 replacement of linkers by successive SC--SC transformations via
 core@shell crystals
;
_journal_issue                   34
_journal_name_full               CrystEngComm
_journal_page_first              4720
_journal_page_last               4731
_journal_paper_doi               10.1039/D4CE00632A
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety
'C24.60 H21.20 Cd N12 O2, C12 H8 N6, 2(Cl O4), 1.4(C H4 O)'
_chemical_formula_sum            'C38 H34.8 Cd Cl2 N18 O11.4'
_chemical_formula_weight         1109.331
_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             2024-07-02
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2024.05.30 svn.r93eb12d9 for OlexSys, GUI svn.r6697)
;
_audit_update_record
;
2024-07-14 deposited with the CCDC.	2024-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                105.06(3)
_cell_angle_beta                 109.51(3)
_cell_angle_gamma                90.79(3)
_cell_formula_units_Z            1
_cell_length_a                   9.1632(18)
_cell_length_b                   9.795(2)
_cell_length_c                   13.509(3)
_cell_measurement_reflns_used    3837
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      1.666
_cell_volume                     1096.9(5)
_computing_cell_refinement       'X-Area (Stoe & Cie GmbH, 2005)'
_computing_data_collection       'X-Area (Stoe & Cie GmbH, 2005)'
_computing_data_reduction        'X-Area (Stoe & Cie GmbH, 2005)'
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.15
_diffrn_detector_area_resol_mean '0.15 mm'
_diffrn_measured_fraction_theta_full 0.9953
_diffrn_measured_fraction_theta_max 0.9953
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1790
_diffrn_reflns_av_unetI/netI     0.1662
_diffrn_reflns_Laue_measured_fraction_full 0.9953
_diffrn_reflns_Laue_measured_fraction_max 0.9953
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12281
_diffrn_reflns_point_group_measured_fraction_full 0.9953
_diffrn_reflns_point_group_measured_fraction_max 0.9953
_diffrn_reflns_theta_full        24.9998
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.704
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'shape of crystal determined optically'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       plate
_exptl_crystal_F_000             561.890
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   0.991
_exptl_transmission_factor_min   0.774
_refine_diff_density_max         1.5164
_refine_diff_density_min         -1.8834
_refine_diff_density_rms         0.1652
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             12.2219
_refine_ls_goodness_of_fit_ref   0.9668
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    37
_refine_ls_number_parameters     386
_refine_ls_number_reflns         3837
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      0.9528
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0895P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1519
_refine_ls_wR_factor_ref         0.1626
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                3025
_reflns_number_total             3837
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4ce00632a2.cif
_cod_data_source_block           shelx_2346038
_cod_depositor_comments
'Adding full bibliography for 7249084--7249086.cif.'
_cod_original_formula_sum        'C38 H34.80 Cd Cl2 N18 O11.40'
_cod_database_code               7249086
_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) groups, All O(H,H,H) groups
2. Restrained distances
 O6-C19 \\sim O6a-C19a
 with sigma of 0.02
 C19-H19d \\sim C19a-H19a
 with sigma of 0.02
 C19-H19e \\sim C19a-H19b
 with sigma of 0.02
 C19-H19f \\sim C19a-H19c
 with sigma of 0.02
 O6-H19d \\sim O6a-H19a
 with sigma of 0.04
 O6-H19e \\sim O6a-H19b
 with sigma of 0.04
 O6-H19f \\sim O6a-H19c
 with sigma of 0.04
 H19d-H19e \\sim H19a-H19b
 with sigma of 0.04
 H19d-H19f \\sim H19a-H19c
 with sigma of 0.04
 H19e-H19f \\sim H19b-H19c
 with sigma of 0.04
 Cd1-H6aa \\sim Cd1-H6ab
 with sigma of 0.02
 Cl1-O2 \\sim Cl1a-O2a
 with sigma of 0.02
 Cl1-O3 \\sim Cl1a-O3a
 with sigma of 0.02
 Cl1-O4 \\sim Cl1a-O4a
 with sigma of 0.02
 Cl1-O5 \\sim Cl1a-O5a
 with sigma of 0.02
 O2-O3 \\sim O2a-O3a
 with sigma of 0.04
 O2-O4 \\sim O2a-O4a
 with sigma of 0.04
 O2-O5 \\sim O2a-O5a
 with sigma of 0.04
 O3-O4 \\sim O3a-O4a
 with sigma of 0.04
 O3-O5 \\sim O3a-O5a
 with sigma of 0.04
 O4-O5 \\sim O4a-O5a
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 Cl1, O2, O3, O4, O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3a, Cl1a, O2a, O4a, O5a
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(Cl1a)=Sof(O2a)=Sof(O3a)=Sof(O4a)=Sof(O5a)=1-FVAR(1)
 Sof(Cl1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(O5)=FVAR(1)
 Fixed Sof: C20(0.3) O6(0.7) H6(0.7) H19e(0.7) C19(0.7) H19d(0.7) H19f(0.7)
 O1(0.7) C19a(0.3) H19a(0.3) H19b(0.3) H19c(0.3) H6aa(0.7) H6ab(0.7) H6a(0.3)
5.a Riding coordinates:
 O6a(H6a)
5.b Free rotating group:
 O6a(H6aa,H6ab)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16)
5.d Idealised Me refined as rotating group:
 C19(H19d,H19e,H19f), C19a(H19a,H19b,H19c)
5.e Idealised tetrahedral OH refined as rotating group:
 O6(H6)
;
_olex2_submission_special_instructions 'No special instructions were received'