Bipyridine-functionalized Cd(ii) coordination frameworks based on robust cyclophosphazenes: structural engineering toward enhanced photocatalytic activity
Özcan, Elif; Zorlu, Yunus; CrystEngComm 27 (2025) 6913–6925; doi:10.1039/D5CE00433K

data_1575749
_publ_section_title
;
 Bipyridine-functionalized Cd(ii) coordination frameworks based on robust
 cyclophosphazenes: structural engineering toward enhanced photocatalytic
 activity
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              6913
_journal_page_last               6925
_journal_paper_doi               10.1039/D5CE00433K
_journal_volume                  27
_journal_year                    2025
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C60 H44 Cd2 N7 O16 P3, 2[C3H7NO]'
_chemical_formula_sum            'C66 H58 Cd2 N9 O18 P3'
_chemical_formula_weight         1582.92
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-08-31
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-09-09 deposited with the CCDC.	2025-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.06(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.873(9)
_cell_length_b                   9.425(7)
_cell_length_c                   34.44(3)
_cell_measurement_reflns_used    1102
_cell_measurement_temperature    298
_cell_measurement_theta_max      16.18
_cell_measurement_theta_min      2.24
_cell_volume                     3529(5)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX2 v2019.1-0 (Bruker AXS, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1401
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8615
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        22.000
_diffrn_reflns_theta_max         22.000
_diffrn_reflns_theta_min         1.873
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  0.6752
_exptl_absorpt_correction_T_min  0.4724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1370 before and 0.0813 after correction.
The Ratio of minimum to maximum transmission is 0.6996.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       block
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details
;
 Flack x determined using 2180 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.13(4)
_refine_ls_extinction_coef       0.0072(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     983
_refine_ls_number_reflns         8615
_refine_ls_number_restraints     1047
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0681
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+3.5603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1489
_refine_ls_wR_factor_ref         0.1639
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                6930
_reflns_number_total             8615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00433k2.cif
_cod_data_source_block           23gtu209_h4l1_cd_22bpy_dmf
_cod_depositor_comments
'Adding full bibliography for 1575749--1575751.cif.'
_cod_database_code               1575749
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.929
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.75706
 0.24294
2. Restrained distances
 C96-C28 = C49-C43
 1.4 with sigma of 0.02
 C53-C52 = C54-C53
 1.4 with sigma of 0.02
 C32-C31 = C33-C32 = C34-C33 = C35-C34 = C36-C35 = C36-C31 = C42-C37 = C38-C37
 = C39-C38 = C40-C39 = C41-C40 = C42-C41
 1.4 with sigma of 0.01
 C24-C21
 1.45 with sigma of 0.01
 N11-C61 = N11-C60
 1.41 with sigma of 0.02
 N11-C62
 1.32 with sigma of 0.03
 O19-C62
 1.25 with sigma of 0.02
 C61-C60
 2.38 with sigma of 0.02
 N10-C63 = N10-C64
 1.41 with sigma of 0.02
 N10-C65
 1.322 with sigma of 0.02
 O20-C65
 1.25 with sigma of 0.02
 N10-C63 = N10-C64 = N11-C60 = N11-C61
 1.4 with sigma of 0.02
 N11-C62 = N10-C65
 1.32 with sigma of 0.02
 O20-C65 = O19-C62
 1.2 with sigma of 0.02
 C61-C62 = C65-C64
 2.32 with sigma of 0.02
 C60-C61
 2.38 with sigma of 0.04
 C61-C62
 2.327 with sigma of 0.04
 C62-C60
 2.424 with sigma of 0.04
 O19-N11
 2.528 with sigma of 0.04
 C63-C64
 2.387 with sigma of 0.04
 C63-C65
 2.412 with sigma of 0.04
 C65-C64
 2.327 with sigma of 0.04
 N10-O20 = N11-O19
 2.25 with sigma of 0.04
 C60-C62 = C65-C63
 2.41 with sigma of 0.04
 C63-N10 \\sim C63A-N10A
 with sigma of 0.02
 C64-N10 \\sim C64A-N10A
 with sigma of 0.02
 N10-C65 \\sim N10A-C65A
 with sigma of 0.02
 O20-C65 \\sim O20A-C65A
 with sigma of 0.02
 C63-C64 \\sim C63A-C64A
 with sigma of 0.02
 C63-C65 \\sim C63A-C65A
 with sigma of 0.02
 C64-C65 \\sim C64A-C65A
 with sigma of 0.02
 N10-O20 \\sim N10A-O20A
 with sigma of 0.02
 C61-N11 \\sim C61A-N11A
 with sigma of 0.02
 C62-N11 \\sim C62A-N11A
 with sigma of 0.02
 C62-O19 \\sim C62A-O19A
 with sigma of 0.02
 N11-C60 \\sim N11A-C60A
 with sigma of 0.02
 C61-C62 \\sim C61A-C62A
 with sigma of 0.02
 C61-C60 \\sim C61A-C60A
 with sigma of 0.02
 C62-C60 \\sim C62A-C60A
 with sigma of 0.02
 N11-O19 \\sim N11A-O19A
 with sigma of 0.02
3. Restrained planarity
 C32, C33, C34, C35, C36, C31
 with sigma of 0.1
 C37, C38, C39, C40, C41, C42
 with sigma of 0.1
 N11, C61, C62, C60, O19, N11A, C61A, C62A, C60A, O19A
 with sigma of 0.01
 N10A, C63A, C64A, C65A, O20A, C63, N10, C64, C65, O20
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
O20 \\sim C65 \\sim C65 \\sim N10 \\sim N10 \\sim C63 \\sim N10 \\sim C64 \\sim
O19 \\sim C62: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 1.7A
C62 \\sim N11 \\sim N11 \\sim C61 \\sim N11 \\sim C60 \\sim O20A \\sim C65A
\\sim C65A \\sim N10A: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.01 within 1.7A
N10A \\sim C64A \\sim N10A \\sim C63A \\sim O19A \\sim C62A \\sim C62A \\sim
N11A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01
within 1.7A
N11A \\sim C60A \\sim N11A \\sim C61A: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
C5 \\sim C4 \\sim C30 \\sim C25: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 1.7A
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Sof(N10A)=Sof(C63A)=Sof(C64A)=Sof(C65A)=Sof(O20A)=1-FVAR(1)
 Sof(C63)=Sof(C64)=Sof(N10)=Sof(O20)=Sof(C65)=FVAR(1)
 Sof(N11A)=Sof(C61A)=Sof(H61D)=Sof(H61E)=Sof(H61F)=Sof(C62A)=Sof(H62A)=
 Sof(C60A)=Sof(H60D)=Sof(H60E)=Sof(H60F)=Sof(O19A)=1-FVAR(2)
 Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=Sof(C62)=Sof(H62)=Sof(N11)=Sof(C60)=
 Sof(H60A)=Sof(H60B)=Sof(H60C)=Sof(O19)=FVAR(2)
7.a Rotating group:
 O11(H11A,H11B), O15(H15A,H15B)
7.b 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), C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C26(H26),
  C27(H27), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35),
 C38(H38), C39(H39), C40(H40), C41(H41), C44(H44), C45(H45), C47(H47), C48(H48),
  C50(H50), C51(H51), C52(H52), C53(H53), C56(H56), C57(H57), C58(H58),
 C59(H59), C62(H62), C62A(H62A)
7.c Idealised Me refined as rotating group:
 C61(H61A,H61B,H61C), C60(H60A,H60B,H60C), C61A(H61D,H61E,H61F), C60A(H60D,
 H60E,H60F)
;
_shelx_res_checksum              40582
_olex2_submission_special_instructions 'No special instructions were received'