Straightening Out Halogen Bonds
Setter, Caitlin J.; Whittaker, Jacob J.; Brock, Aidan J.; Arachchige, Kasun; McMurtrie, John; Clegg, Jack Kay; Pfrunder, Michael Craig; CrystEngComm  (2020) –; doi:10.1039/D0CE00176G

data_7239920
_publ_section_title
;
 Straightening Out Halogen Bonds
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00176G
_journal_year                    2020
_chemical_formula_moiety         '2(C17 H10 N2 O2), 0.25(C4 H8 O)'
_chemical_formula_sum            'C35 H22 N4 O4.25'
_chemical_formula_weight         566.56
_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   mixed
_audit_creation_date             2020-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
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2020-01-11 deposited with the CCDC.	2020-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                93.98(3)
_cell_angle_beta                 91.69(3)
_cell_angle_gamma                92.08(3)
_cell_formula_units_Z            2
_cell_length_a                   3.8500(8)
_cell_length_b                   14.124(3)
_cell_length_c                   26.384(5)
_cell_measurement_reflns_used    4229
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.708
_cell_measurement_theta_min      1.548
_cell_volume                     1429.6(5)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.862
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_device_type  'MX1 Beamline Australian Synchrotron'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.862
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            4229
_diffrn_reflns_point_group_measured_fraction_full 0.862
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        24.708
_diffrn_reflns_theta_max         24.708
_diffrn_reflns_theta_min         1.548
_diffrn_source                   Synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  24.708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_description       plate
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   24.708
_exptl_transmission_factor_min   1.548
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         4229
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.1383
_refine_ls_R_factor_gt           0.1192
_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^)+(0.0965P)^2^+11.0815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3540
_refine_ls_wR_factor_ref         0.3645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3266
_reflns_number_total             4229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00176g2.cif
_cod_data_source_block           pbnpdhTHF
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        1429.5(5)
_cod_database_code               7239920
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.991
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.742(6)
 0.258(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 O1-H1
 0.97 with sigma of 0.02
 O2-H1
 1.67 with sigma of 0.02
 H3-O3
 0.87 with sigma of 0.02
 C37-C36 \\sim C36-C35 \\sim C35-C34
 with sigma of 0.02
 O5-C37 \\sim O5-C34
 with sigma of 0.02
 O5-C36 \\sim O5-C35
 with sigma of 0.04
 C36-C34 \\sim C37-C35
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
O5 \\sim C37 \\sim C36 \\sim C35 \\sim C34: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(C35) = Uanis(C34) = Uanis(O5) = Uanis(C37) = Uanis(C36)
5. Rigid body (RIGU) restrains
 O5, C37, C36, C35, C34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O5(0.25) C37(0.25) H37A(0.25) H37B(0.25) C36(0.25) H36A(0.25)
 H36B(0.25) C35(0.25) H35A(0.25) H35B(0.25) C34(0.25) H34A(0.25) H34B(0.25)
7.a Free rotating group:
 O5(C37,C36,C35,C34)
7.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C36(H36A,H36B), C35(H35A,H35B), C34(H34A,H34B)
7.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C22(H22), C32(H32), C9(H9), C20(H20), C19(H19), C29(H29), C31(H31),
 C3(H3A), C6(H6), C28(H28), C25(H25), C23(H23), C16(H16), C7(H7), C15(H15),
 C13(H13), C12(H12)
;
_shelx_res_checksum              80385
_olex2_submission_special_instructions 'No special instructions were received'