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_7245765
_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 H32 Cd2 N4 O22), C2 H7 N, C2 H6.5 N0.5'
_chemical_formula_sum            'C28 H29.5 Cd N3.5 O11'
_chemical_formula_weight         703.45
_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                   15.7981(13)
_cell_length_b                   16.2656(14)
_cell_length_c                   22.388(2)
_cell_measurement_reflns_used    3112
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.118
_cell_measurement_theta_min      2.558
_cell_volume                     5752.9(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17933
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.341
_diffrn_reflns_theta_min         1.797
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6805
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0672 before and 0.0453 after correction.
The Ratio of minimum to maximum transmission is 0.9126.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_description       block
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.686
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.134
_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     216
_refine_ls_number_reflns         3670
_refine_ls_number_restraints     200
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1462
_refine_ls_R_factor_gt           0.0867
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1387P)^2^+47.5455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2523
_refine_ls_wR_factor_ref         0.2929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2143
_reflns_number_total             3670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01192a2.cif
_cod_data_source_block           20210618
_cod_original_cell_volume        5753.0(9)
_cod_original_formula_sum        'C28 H29.50 Cd N3.50 O11'
_cod_database_code               7245765
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.664
_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, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
O1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C2) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Others
 Fixed Sof: N2(0.25) H2a(0.25) H1a(0.5) H1b(0.5)
5.a Riding coordinates:
 N1(H1), C16(H16a,H16b,H16c), N2(H2a)
5.b Rotating group:
 O1(H1a,H1b)
5.c Ternary CH refined with riding coordinates:
 C2(H2)
5.d Aromatic/amide H refined with riding coordinates:
 C14(H14), C7(H7), C13(H13), C8(H8)
5.e Idealised Me refined as rotating group:
 C3(H3a,H3b,H3c), C15(H15a,H15b,H15c)
;
_shelx_res_checksum              76769
_shelx_hkl_checksum              95576
_olex2_submission_special_instructions 'No special instructions were received'