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_1544161
_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         'C29 H28 F4 I N3 O'
_chemical_formula_sum            'C29 H28 F4 I N3 O'
_chemical_formula_weight         637.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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 4.2'
_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                 112.879(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            12
_cell_length_a                   25.213(7)
_cell_length_b                   13.978(3)
_cell_length_c                   27.637(7)
_cell_measurement_reflns_used    19353
_cell_measurement_temperature    125
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.90
_cell_volume                     8974(4)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b31'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b31 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b31'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      125
_diffrn_detector_area_resol_mean 14.222
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.2103
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            109125
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.380
_diffrn_reflns_theta_min         1.753
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.121
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3840.00
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_refine_diff_density_max         3.73
_refine_diff_density_min         -1.27
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1027
_refine_ls_number_reflns         16446
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1938
_refine_ls_R_factor_gt           0.1077
_refine_ls_shift/su_max          0.038
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1362P)^2^+110.0794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2707
_refine_ls_wR_factor_ref         0.3145
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8588
_reflns_number_total             16446
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c6sc03696a2.cif
_cod_data_source_block           S3
_cod_depositor_comments
'Adding full bibliography for 1544158--1544161.cif.'
_cod_database_code               1544161
_shelx_res_checksum              10955
_shelx_hkl_checksum              47088
_solvent_exptl_crystal_recrystallization_method Acetonitrile