Halogen bond cocrystal polymorphs of the 1,4–di(4’–pyridyl)–1,3–diacetylene
Zhang, Pan; Bolla, Geetha; Qiu, Gege; Shu, Zhibin; Yan, Qingqing; Li, Qingyuan; Ding, Shang; Ni, Zhenjie; Zhu, Weigang; dong, huanli; Zhen, Yonggang; Hu, Wenping; CrystEngComm  (2017) –; doi:10.1039/C7CE00892A

data_7228551
_publ_section_title
;
 Halogen bond cocrystal polymorphs of the
 1,4--di(4&#x2019;--pyridyl)--1,3--diacetylene
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00892A
_journal_year                    2017
_chemical_formula_moiety         'C6 F3 I3, C14 H8 N2'
_chemical_formula_sum            'C20 H8 F3 I3 N2'
_chemical_formula_weight         713.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-31
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-03-14 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.639(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.6699(5)
_cell_length_b                   34.308(3)
_cell_length_c                   9.1378(10)
_cell_measurement_reflns_used    6792
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4817
_cell_measurement_theta_min      1.7808
_cell_volume                     2040.3(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2014)'
_computing_structure_solution
;
'SHELXT (Sheldrick, 2014)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 45.1022
              2theta: -20.1561
scan:
    Number of images: 300
               Slice: -80.0000 - 70.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 45.1022
              2theta: -20.1561
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0146
_diffrn_orient_matrix_UB_12      -0.1511
_diffrn_orient_matrix_UB_13      -0.0239
_diffrn_orient_matrix_UB_21      -0.0004
_diffrn_orient_matrix_UB_22      -0.0046
_diffrn_orient_matrix_UB_23      0.0288
_diffrn_orient_matrix_UB_31      -0.1066
_diffrn_orient_matrix_UB_32      -0.0342
_diffrn_orient_matrix_UB_33      -0.0069
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14316
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.501
_diffrn_reflns_theta_min         2.574
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    4.630
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.324
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.103
_refine_diff_density_max         0.625
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.201
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0121P)^2^+6.3587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0630
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4335
_reflns_number_total             4623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00892a2.cif
_cod_data_source_block           sa5004
_cod_database_code               7228551
_diffrn_number_total             4712
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C10(H10), C11(H11), C17(H17), C18(H18), C19(H19), C20(H20)
;
_shelx_res_checksum              34566
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'