Organic molecular tessellations and intertwined double helices assembled by halogen bonding
Ng, Chun-Fai; Chow, Hak-Fun; Mak, Thomas C. W.; CrystEngComm 21 (2019) 1130–; doi:10.1039/C8CE02133C

data_7232153
_publ_section_title
;
 Organic molecular tessellations and intertwined double helices assembled
 by halogen bonding
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              1130
_journal_paper_doi               10.1039/C8CE02133C
_journal_volume                  21
_journal_year                    2019
_chemical_formula_sum            'C13.2 H9.8 I2 N4.6'
_chemical_formula_weight         486.66
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-01-07 deposited with the CCDC.
2019-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   17.5338(8)
_cell_length_b                   10.4983(5)
_cell_length_c                   28.7697(11)
_cell_measurement_reflns_used    449
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      15
_cell_volume                     5295.8(4)
_computing_cell_refinement       'BRUKER D8VENTURE DIFFRACTOMETER'
_computing_data_collection       'BRUKER D8VENTURE DIFFRACTOMETER'
_computing_data_reduction        'BRUKER D8VENTURE DIFFRACTOMETER'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'BRUKER D8VENTURE DIFFRACTOMETER'
_diffrn_measurement_method       'PHI & OMEGA SCAN'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            108372
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_min         1.940
_exptl_absorpt_coefficient_mu    4.746
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3832
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.442
_exptl_crystal_description       block
_exptl_crystal_F_000             3635
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_platon_squeeze_details
; 
Structural refinement of Q-peaks from the residual electron density as solvent 
molecules were unsuccessful. The data was then processed with the SQUEEZE procedure: 
Spek, A. L. Acta Cryst. 2015, C71, 9-18. 915 electrons in the solvent-assesible void , which corresponded to 42 acetonitrile molecules, were found in the unit cell and has been removed by SQUEEZE procedure.
;
_refine_diff_density_max         1.041
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.36(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         9023
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+40.2012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1122
_reflns_Friedel_coverage         0.957
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                7538
_reflns_number_total             9023
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce02133c2.cif
_cod_data_source_block           L1a
_cod_depositor_comments
'Adding full bibliography for 7232153--7232157.cif.'
_cod_original_formula_sum        'C13.20 H9.80 I2 N4.60'
_cod_database_code               7232153
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.253
_shelx_estimated_absorpt_t_max   0.330
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              16671
_shelx_fab_checksum              38226