Construction of naphthalenediimide-based cadmium complexes and application in iodine adsorption, photochromism and photocatalysis
Sun, Mingyang; Bai, Fengying; Guan, QingLin; Xing, Yongheng; Xu, Fen; CrystEngComm  (2022) –; doi:10.1039/D2CE01192A

data_7245766
_publ_section_title
;
 Construction of naphthalenediimide-based cadmium complexes and
 application in iodine adsorption, photochromism and photocatalysis
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01192A
_journal_year                    2022
_chemical_formula_moiety         '0.5(C48 H28 Cd2 N5 O22), C2 H8 N'
_chemical_formula_sum            'C26 H22 Cd N3.5 O11'
_chemical_formula_weight         671.87
_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_Hall           '-I 2 2c'
_space_group_name_H-M_alt        'I b a m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-06-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-06-27 deposited with the CCDC.	2022-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.6608(14)
_cell_length_b                   16.6690(15)
_cell_length_c                   22.238(2)
_cell_measurement_reflns_used    3234
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      53.864
_cell_measurement_theta_min      3.568
_cell_volume                     5805.2(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS SMART APEX II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16623
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.932
_diffrn_reflns_theta_min         1.784
_exptl_absorpt_coefficient_mu    0.816
_exptl_absorpt_correction_T_max  0.9838
_exptl_absorpt_correction_T_min  0.7501
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       block
_exptl_crystal_F_000             2708
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.618
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         3234
_refine_ls_number_restraints     537
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0678
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1404P)^2^+11.7416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2119
_refine_ls_wR_factor_ref         0.2448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2120
_reflns_number_total             3234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01192a2.cif
_cod_data_source_block           20200416
_cod_original_cell_volume        5805.3(9)
_cod_original_formula_sum        'C26 H22 Cd N3.50 O11'
_cod_database_code               7245766
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.908
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H5a,H5b} of N5, {H4a,H4b} of N4
 At 1.5 times of:
  All C(H,H,H) groups, {H3d,H3e} of N3, All O(H,H) groups
2. Restrained distances
 O0AA-C19 = O2AA-C19 = O4-C1 = O5-C1
 1.25 with sigma of 0.01
 C25-N3 = N3-C25_$1
 1.47 with sigma of 0.005
 C5-C4 = C15-C11 = C17-C14 = C8-C16
 1.47 with sigma of 0.01
 N2-C18 = N1-C2
 1.45 with sigma of 0.01
 O6-C15 = O7-C4 = O8-C16 = O9-C17
 1.21 with sigma of 0.01
 C3-C2 = C20-C18
 1.54 with sigma of 0.01
 N1-C15 = N1-C4 = N2-C16 = N2-C17
 1.4 with sigma of 0.01
 C23-N4
 1.34 with sigma of 0.02
 N5-C24
 1.34 with sigma of 0.02
 N4-C23 = N5-C24
 1.34 with sigma of 0.02
 C25-C25_$1
 2.401 with sigma of 0.02
 O4-O5 = O2AA-O0AA
 2.165 with sigma of 0.02
 O6-C11 = O7-C5 = O8-C8 = O9-C14
 2.351 with sigma of 0.02
 C2-C4 \\sim C2-C15
 with sigma of 0.02
 C18-C16 \\sim C18-C17
 with sigma of 0.02
 C16-C9 \\sim C16-C7
 with sigma of 0.02
 C17-C9 \\sim C17-C13
 with sigma of 0.02
 C4-C10 \\sim C4-C6
 with sigma of 0.02
 C15-C10 \\sim C15-C12
 with sigma of 0.02
 N4-C23 \\sim N5-C24
 with sigma of 0.02
3. Restrained planarity
 O7, N1, C4, C5
 with sigma of 0.1
 N2, C16, C17, C18
 with sigma of 0.1
 O2AA, C19, O0AA, C18
 with sigma of 0.1
 O8, N2, C8, C16
 with sigma of 0.1
 O5, O4, C1, C2
 with sigma of 0.1
 C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C17, C16, C4, C15
 with sigma of 0.1
 O6, N1, C11, C15
 with sigma of 0.1
 O9, N2, C14, C17
 with sigma of 0.1
 N1, C2, C4, C15
 with sigma of 0.1
4. Rigid bond restraints
 Cd1, O1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
O5 \\sim O4 \\sim O7 \\sim O6 \\sim O8 \\sim O9 \\sim O2AA \\sim O0AA \\sim N1
\\sim N2 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim
C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim
C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
N4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(N3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N4) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
6. Rigid body (RIGU) restrains
 Cd1, O5, O4, O7, O6, O8, O9, O2AA, O0AA, N1, N2, C1, C2, C3, C4, C5, C6, C7,
 C8, C9, C10, C11, C12, C13, C14, C15, C16, C17, C18, C19, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N4, C23
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N5, C24
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
7. Others
 Fixed Sof: O5(0.5) O4(0.5) O7(0.5) O6(0.5) O8(0.5) O9(0.5) O2AA(0.5)
 O0AA(0.5) O1(0.5) H1a(0.5) H1b(0.5) N1(0.5) N2(0.5) C1(0.5) C2(0.5) C3(0.5)
 H3a(0.5) H3b(0.5) H3c(0.5) C4(0.5) C5(0.5) C6(0.5) H6(0.5) C7(0.5) H7(0.5)
 C8(0.5) C9(0.5) C10(0.5) C11(0.5) C12(0.5) H12(0.5) C13(0.5) H13(0.5) C14(0.5)
 C15(0.5) C16(0.5) C17(0.5) C18(0.5) H18(0.5) C19(0.5) C20(0.5) H20a(0.5)
 H20b(0.5) H20c(0.5) N4(0.125) H4a(0.125) H4b(0.125) N5(0.125) H5a(0.125)
 H5b(0.125)
8.a Riding coordinates:
 O1(H1a,H1b), N3(H3d,H3e), C25(H25a,H25b,H25c)
8.b Ternary CH refined with riding coordinates:
 C18(H18)
8.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C12(H12), C13(H13)
8.d X=CH2 refined with riding coordinates:
 N4(H4a,H4b), N5(H5a,H5b)
8.e Naphthalene refined as free rotating group:
 C5(C6,C7,C8,C9,C10,C11,C12,C13,C14)
8.f Idealised Me refined as rotating group:
 C3(H3a,H3b,H3c), C20(H20a,H20b,H20c)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 156 electrons were 
found in a volume of 612\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[H2O] per Asymmetric Unit 
which account for 160 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              24854
_shelx_hkl_checksum              72823
_shelx_fab_checksum              26295
_olex2_submission_special_instructions 'No special instructions were received'