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_7126231
_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                   17.559(5)
_cell_length_b                   26.315(16)
_cell_length_c                   7.259(8)
_cell_measurement_reflns_used    673
_cell_measurement_temperature    297.90(10)
_cell_measurement_theta_max      25.9820
_cell_measurement_theta_min      4.0740
_cell_volume                     3354(4)
_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_environment      air
_diffrn_ambient_temperature      297.90(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.599
_diffrn_measured_fraction_theta_max 0.599
_diffrn_measurement_details
;
 Data were collected at room temperature and pressure of 1.09(2) GPa (1090000 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      0.0044928000
_diffrn_orient_matrix_UB_12      0.0137172000
_diffrn_orient_matrix_UB_13      0.0824927000
_diffrn_orient_matrix_UB_21      -0.0371764000
_diffrn_orient_matrix_UB_22      -0.0074666000
_diffrn_orient_matrix_UB_23      0.0280727000
_diffrn_orient_matrix_UB_31      0.0154043000
_diffrn_orient_matrix_UB_32      -0.0221925000
_diffrn_orient_matrix_UB_33      0.0421293000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2726
_diffrn_reflns_av_unetI/netI     0.4784
_diffrn_reflns_Laue_measured_fraction_full 0.599
_diffrn_reflns_Laue_measured_fraction_max 0.599
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            15625
_diffrn_reflns_point_group_measured_fraction_full 0.580
_diffrn_reflns_point_group_measured_fraction_max 0.580
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         4.186
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.080
_exptl_absorpt_correction_T_max  0.441
_exptl_absorpt_correction_T_min  0.378
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model (Absorb Angel (2004) J. Appl. Cryst. 37:486-492)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details
;
 Flack x determined using 154 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.22(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         3321
_refine_ls_number_restraints     694
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.4167
_refine_ls_R_factor_gt           0.1781
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_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          0.3875
_refine_ls_wR_factor_ref         0.5136
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_full    0.557
_reflns_Friedel_fraction_max     0.557
_reflns_number_gt                797
_reflns_number_total             3321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00461h2.cif
_cod_data_source_block           1_09_GPa
_cod_depositor_comments
'Adding full bibliography for 7126224--7126231.cif.'
_cod_database_code               7126231
_chemical_oxdiff_formula         'c34 h22 n2 o f10 s2 i2'
_reflns_odcompleteness_completeness 56.03
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 H5_$1-H24B
 2.5 with sigma of 0.02
 C8-C10
 1.45 with sigma of 0.02
 C9-C24
 1.45 with sigma of 0.02
 C19-C17
 1.45 with sigma of 0.02
 C24-C25
 4.1 with sigma of 0.02
 C26-F10 \\sim F10-C30
 with sigma of 0.02
 F5-F1 \\sim F2-F6
 with sigma of 0.02
 F4-F1 \\sim F2-F3 \\sim F4-F5 \\sim F3-F6
 with sigma of 0.02
 F2-F1 \\sim F3-F4 \\sim F5-F6
 with sigma of 0.02
 C2-C6 \\sim C6-C4
 with sigma of 0.02
 F1-C11 \\sim C11-F2
 with sigma of 0.02
 F6-C13 \\sim F5-C13 \\sim F4-C12 \\sim F3-C12 \\sim F1-C11 \\sim F2-C11
 with sigma of 0.02
 F4-F2 \\sim F6-F4 \\sim F5-F3 \\sim F3-F1
 with sigma of 0.02
 C23-C17 \\sim C17-C20
 with sigma of 0.02
 C27-F8 \\sim F8-C29
 with sigma of 0.02
3. Restrained planarity
 C26, I1, C27, C31, C28, F7, F10, C30, F8, C29, F9, I2
 with sigma of 0.1
 C2, C1, N1, C5, C4, C3, C6, C7, C8, C9, S1
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
F7 \\sim I1 \\sim C26 \\sim C27 \\sim C31 \\sim C28 \\sim F10 \\sim C30 \\sim
F8 \\sim C29 \\sim F9 \\sim I2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
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
C20 \\sim C19 \\sim C23 \\sim C22 \\sim N2 \\sim C21: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
F8 \\sim F7: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C11 \\sim C10 \\sim C14 \\sim C13 \\sim C12 \\sim F6 \\sim F5 \\sim F3 \\sim F4
\\sim F1 \\sim F2: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C6 \\sim C3: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C9 \\sim S1 \\sim C6 \\sim C7 \\sim C8 \\sim C24: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
F5 \\sim C13 \\sim F6: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C13 \\sim C12 \\sim C11: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C18 \\sim C16 \\sim C17 \\sim S2 \\sim C15 \\sim C25: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C18 \\sim S2 \\sim C17 \\sim C16 \\sim C15 \\sim C25: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
S2 \\sim C18 \\sim C15 \\sim C16 \\sim C17 \\sim C25: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(F8) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F9) \\sim
Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(N2) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C17) \\sim Ueq,
Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C11) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(C7)
\\sim Ueq, Uanis(S1) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(F1) \\sim Ueq,
Uanis(F2) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C5)
\\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(I1) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(C30) \\sim Ueq,
Uanis(C29) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(I2) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 C28, I1, C26, C27, C31, F7, F10, C30, F8, C29, F9, I2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed U11: C12(0.11162) F4(0.09316)
 Fixed U12: C12(0.02413) F4(0.01639)
 Fixed U13: C12(-0.02635) F4(-0.06091)
 Fixed U22: C12(0.17909) F4(0.05414)
 Fixed U23: C12(0.00476) F4(0.01173)
 Fixed U33: C12(0.1868) F4(0.24166)
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), C13(C12,C11,C10,C14)
7.c Fitted hexagon refined as free rotating group:
 N2(C22,C23,C19,C20,C21), C2(C1,N1,C5,C4,C3), C27(C26,C31,C30,C29,C28)
7.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              89928
_shelx_hkl_checksum              87767
_shelx_fab_checksum              31742
_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 2.151
_oxdiff_exptl_absorpt_empirical_full_min 0.625