Large negative linear compressibility of a porous molecular co-crystal.
Sobczak, Szymon; Półrolniczak, Aleksandra; Ratajczyk, Paulina; Cai, Weizhao; Gładysiak, Andrzej; Nikolayenko, Varvara I.; Castell, Dominic C.; Barbour, Leonard J.; Katrusiak, Andrzej; Chemical communications (Cambridge, England) 56 (2020) 4324–4327; doi:10.1039/d0cc00461h

data_7126226
_publ_section_title
;
 Large negative linear compressibility of a porous molecular co-crystal.
;
_journal_issue                   31
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4324
_journal_page_last               4327
_journal_paper_doi               10.1039/d0cc00461h
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C6 F4 I2, C25 H16 F6 N2 S2'
_chemical_formula_sum            'C31 H16 F10 I2 N2 S2'
_chemical_formula_weight         924.38
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-12-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-20 deposited with the CCDC.	2020-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.723(8)
_cell_length_b                   26.15(6)
_cell_length_c                   7.00(3)
_cell_measurement_reflns_used    119
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.4310
_cell_measurement_theta_min      4.1170
_cell_volume                     3244(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.445
_diffrn_measured_fraction_theta_max 0.445
_diffrn_measurement_details
;
 Data were collected at room temperature and pressure of 1.59(2) GPa (1590000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0016143000
_diffrn_orient_matrix_UB_12      -0.0134424000
_diffrn_orient_matrix_UB_13      -0.0857232000
_diffrn_orient_matrix_UB_21      -0.0371361000
_diffrn_orient_matrix_UB_22      0.0087498000
_diffrn_orient_matrix_UB_23      -0.0240140000
_diffrn_orient_matrix_UB_31      0.0158169000
_diffrn_orient_matrix_UB_32      0.0221588000
_diffrn_orient_matrix_UB_33      -0.0444601000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3185
_diffrn_reflns_av_unetI/netI     0.6373
_diffrn_reflns_Laue_measured_fraction_full 0.445
_diffrn_reflns_Laue_measured_fraction_max 0.445
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            14627
_diffrn_reflns_point_group_measured_fraction_full 0.442
_diffrn_reflns_point_group_measured_fraction_max 0.442
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         4.167
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.152
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.894
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.323
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.60(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         2530
_refine_ls_number_restraints     848
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.4345
_refine_ls_R_factor_gt           0.1738
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3915
_refine_ls_wR_factor_ref         0.5193
_reflns_Friedel_coverage         0.823
_reflns_Friedel_fraction_full    0.438
_reflns_Friedel_fraction_max     0.438
_reflns_number_gt                537
_reflns_number_total             2530
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00461h2.cif
_cod_data_source_block           1_59_GPa
_cod_depositor_comments
'Adding full bibliography for 7126224--7126231.cif.'
_cod_original_cell_volume        3242(18)
_cod_database_code               7126226
_chemical_oxdiff_formula         'C34 H22 N2 O F10 S2 I2'
_reflns_odcompleteness_completeness 38.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.00
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H24B-H5_$1
 2.5 with sigma of 0.02
 H5_$1-H24A
 2.5 with sigma of 0.02
 C8-C10
 1.45 with sigma of 0.02
 C18-C25
 1.45 with sigma of 0.02
 C6-C3
 1.45 with sigma of 0.02
 C9-C24
 1.52 with sigma of 0.02
 I2_$2-S1
 3.6 with sigma of 0.02
 C8-C15
 3.6 with sigma of 0.02
 C17-C19
 1.45 with sigma of 0.02
 H20-H16
 2.1 with sigma of 0.02
 C25-C15
 2.5 with sigma of 0.02
 I1-C26 \\sim I2-C29
 with sigma of 0.02
 C30-I2 \\sim I2-C28
 with sigma of 0.02
 C27-I1 \\sim I1-C31
 with sigma of 0.02
 F1-C11 \\sim F2-C11 \\sim F4-C12 \\sim F3-C12 \\sim F6-C13 \\sim F5-C13 \\sim
F7-C27 \\sim F8-C28 \\sim F10-
 C31 \\sim F9-C30
 with sigma of 0.02
 C4-C6 \\sim C6-C2
 with sigma of 0.02
 C23-C17 \\sim C17-C20
 with sigma of 0.02
 F2-F1 \\sim F4-F3 \\sim F6-F5
 with sigma of 0.02
 F4-F2 \\sim F3-F1 \\sim F5-F3 \\sim F6-F4
 with sigma of 0.02
 F4-F1 \\sim F3-F2 \\sim F6-F3 \\sim F5-F4
 with sigma of 0.02
 F1-C11 \\sim F2-C11 \\sim F3-C12 \\sim F4-C12 \\sim F5-C13 \\sim F6-C13
 with sigma of 0.02
 F3-C13 \\sim F5-C12 \\sim F4-C13 \\sim F6-C12 \\sim F4-C11 \\sim F2-C12 \\sim
F1-C12 \\sim F3-C11
 with sigma of 0.02
 C19-C17 \\sim C15-C14 \\sim C8-C10 \\sim C6-C3
 with sigma of 0.02
3. Restrained planarity
 I1, I2, F8, F10, C27, C26, C31, C30, C29, C28, F9, F7
 with sigma of 0.1
 N2, C22, C23, C19, C17, C18, C15, C20, C21, C16, C25, S2
 with sigma of 0.1
 C15, C14, C18, C16
 with sigma of 0.1
 C15, C14, C10, C11, C12, C13
 with sigma of 0.1
 C2, C1, N1, C5, C4, C3, C8, C7, C6, S1, C9, C24
 with sigma of 0.1
4. Rigid bond restraints
 C13, C12, C11, F6, F5, F3, F1, F2, C10, C14, F4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S1, C9, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C8, C9, S1, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C2 \\sim C1 \\sim N1 \\sim C5 \\sim C4 \\sim C3: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
I1 \\sim I2 \\sim F8 \\sim F10 \\sim C31 \\sim C30 \\sim C29 \\sim C28 \\sim
C27 \\sim C26 \\sim F9 \\sim F7: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C13 \\sim C12 \\sim C11 \\sim F6 \\sim F5 \\sim F4 \\sim F3 \\sim F1 \\sim F2:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C23 \\sim C19 \\sim C20 \\sim C21 \\sim N2 \\sim C22: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04
C20 \\sim C21 \\sim N2 \\sim C22: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C8 \\sim C7 \\sim C6 \\sim S1 \\sim C9 \\sim C24: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C18 \\sim C15 \\sim C16 \\sim C17 \\sim S2 \\sim C25: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04
N2 \\sim C22 \\sim C23 \\sim C19 \\sim C20 \\sim C21 \\sim C8 \\sim C7 \\sim C6
\\sim S1 \\sim C9 \\sim C24: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C18) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(S2) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C19) \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C22)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
6. Rigid body (RIGU) restrains
 I1, I2, F8, F10, C31, C30, C29, C28, C27, C26, F9, F7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, C14, C13, C12, C11, F6, F5, F4, F3, F1, F2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2, C22, C23, C19, C20, C21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2, C1, N1, C5, C4, C3, C8, C7, C6, S1, C9, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C23, C19, C25, C17, S2, C18, C15, C16, N2, C22, C20, C21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C20(H20), C21(H21), C2(H2), C1(H1), C5(H5), C4(H4),
 C7(H7), C16(H16)
7.b Fitted pentagon refined as free rotating group:
 C8(C7,C6,S1,C9), C17(S2,C18,C15,C16), C10(C14,C13,C12,C11)
7.c Fitted hexagon refined as free rotating group:
 N2(C22,C23,C19,C20,C21), C2(C1,N1,C5,C4,C3), C31(C30,C29,C28,C27,C26)
7.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              23444
_shelx_hkl_checksum              3624
_shelx_fab_checksum              81218
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 25.789
_oxdiff_exptl_absorpt_empirical_full_min 0.286