Self-assembly of tin(iv) cyanophenyl porphyrins into hydrogen-bonded frameworks reinforced by halogen bonding: synthesis, structure and computational perspectives
Bandaru, Rohith Phaneendra; Jami, Ananda Kumar; Tripuramallu, Bharat Kumar; CrystEngComm 27 (2025) 7081–7093; doi:10.1039/D5CE00731C

data_7250897
_publ_section_title
;
 Self-assembly of tin(iv) cyanophenyl porphyrins into hydrogen-bonded
 frameworks reinforced by halogen bonding: synthesis, structure and
 computational perspectives
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              7081
_journal_page_last               7093
_journal_paper_doi               10.1039/D5CE00731C
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C60 H32 I2 N8 O2 Sn, C3 H7 N O'
_chemical_formula_sum            'C63 H39 I2 N9 O3 Sn'
_chemical_formula_weight         1342.52
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2025-07-14 deposited with the CCDC.	2025-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                68.874(3)
_cell_angle_beta                 70.185(3)
_cell_angle_gamma                62.069(3)
_cell_formula_units_Z            2
_cell_length_a                   14.5583(9)
_cell_length_b                   14.6841(11)
_cell_length_c                   16.1918(13)
_cell_measurement_reflns_used    14027
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.465
_cell_measurement_theta_min      1.618
_cell_volume                     2791.2(4)
_computing_cell_refinement       'SAINT V8.32B (?, 2016)'
_computing_data_reduction        'SAINT V8.32B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49974
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.465
_diffrn_reflns_theta_min         1.618
_exptl_absorpt_coefficient_mu    1.619
_exptl_absorpt_correction_T_max  0.615
_exptl_absorpt_correction_T_min  0.464
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2, Bruker-AXS'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         3.517
_refine_diff_density_min         -2.773
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         14027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0593P)^2^+14.9217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1379
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11268
_reflns_number_total             14027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00731c2.cif
_cod_data_source_block           bkt11
_cod_depositor_comments
'Adding full bibliography for 7250896--7250898.cif.'
_cod_database_code               7250897
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.642
_shelx_estimated_absorpt_t_min   0.498
_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
2.a Aromatic/amide H refined with riding coordinates:
 C43(H43), C18(H18), C3(H3), C22(H22), C8(H8), C19(H19), C25(H25), C13(H13),
 C26(H26), C44(H44), C9(H9), C56(H56), C4(H4), C51(H51), C14(H14), C50(H50),
 C40(H40), C47(H47), C53(H53), C36(H36), C33(H33), C23(H23), C54(H54), C39(H39),
  C37(H37), C60(H60), C57(H57), C32(H32), C46(H46), C29(H29), C59(H59),
 C30(H30), C63(H63)
2.b Idealised Me refined as rotating group:
 C61(H61A,H61B,H61C), C62(H62A,H62B,H62C)
;
_shelx_res_checksum              81931
_olex2_submission_special_instructions 'No special instructions were received'