pH controlled assembly of a self-complementary halogen-bonded dimer
Maugeri, Leonardo; Jamieson, Ellen M. G.; Cordes, David B.; Slawin, Alexandra M. Z.; Philp, Douglas; Chem. Sci. 8 (2017) 938–; doi:10.1039/C6SC03696A

data_1544160
_publ_section_title
;
 pH controlled assembly of a self-complementary halogen-bonded dimer
;
_journal_issue                   2
_journal_name_full               'Chem. Sci.'
_journal_page_first              938
_journal_paper_doi               10.1039/C6SC03696A
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         'C28 H25 F4 I N3 O, C9 H17 N2'
_chemical_formula_sum            'C37 H42 F4 I N5 O'
_chemical_formula_weight         775.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-06-27
_audit_creation_method           'by CrystalStructure 4.1'
_audit_update_record
;
2016-06-28 deposited with the CCDC.
2016-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 103.187(10)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   20.258(3)
_cell_length_b                   13.9884(13)
_cell_length_c                   26.734(4)
_cell_measurement_reflns_used    7313
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      1.60
_cell_volume                     7376.0(17)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b32'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b32'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            44203
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.382
_diffrn_reflns_theta_min         1.565
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3168.00
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.80
_refine_diff_density_min         -0.43
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     473
_refine_ls_number_reflns         6762
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0297P)^2^+21.2857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0882
_reflns_number_gt                4925
_reflns_number_total             6762
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c6sc03696a2.cif
_cod_data_source_block           2-2-DBUH2
_cod_depositor_comments
'Adding full bibliography for 1544158--1544161.cif.'
_cod_original_cell_volume        7376.1(17)
_cod_database_code               1544160
_shelx_res_checksum              47021
_shelx_hkl_checksum              96127
_solvent_exptl_crystal_recrystallization_method Acetonitrile