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_7126225
_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, H2 O'
_chemical_formula_sum            'C31 H18 F10 I2 N2 O S2'
_chemical_formula_weight         942.39
_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   mixed
_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                   17.564(10)
_cell_length_b                   25.64(4)
_cell_length_c                   7.07(3)
_cell_measurement_reflns_used    271
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.3440
_cell_measurement_theta_min      4.4410
_cell_volume                     3184(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_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 0.659
_diffrn_measured_fraction_theta_max 0.658
_diffrn_measurement_details
;
 Data were collected at room temperature and pressure of 1.95(2) GPa (1950000 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      0.0010846000
_diffrn_orient_matrix_UB_12      -0.0140242000
_diffrn_orient_matrix_UB_13      -0.0856610000
_diffrn_orient_matrix_UB_21      -0.0373573000
_diffrn_orient_matrix_UB_22      0.0087840000
_diffrn_orient_matrix_UB_23      -0.0215000000
_diffrn_orient_matrix_UB_31      0.0155095000
_diffrn_orient_matrix_UB_32      0.0221209000
_diffrn_orient_matrix_UB_33      -0.0468968000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2608
_diffrn_reflns_av_unetI/netI     0.1951
_diffrn_reflns_Laue_measured_fraction_full 0.659
_diffrn_reflns_Laue_measured_fraction_max 0.658
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            6062
_diffrn_reflns_point_group_measured_fraction_full 0.649
_diffrn_reflns_point_group_measured_fraction_max 0.649
_diffrn_reflns_theta_full        15.852
_diffrn_reflns_theta_max         15.852
_diffrn_reflns_theta_min         4.220
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.195
_exptl_absorpt_correction_T_max  0.419
_exptl_absorpt_correction_T_min  0.362
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43a (Rigaku Oxford Diffraction, 2018)
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    1.966
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.171
_refine_ls_abs_structure_details
;
 Flack x determined using 106 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.3(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.772
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         992
_refine_ls_number_restraints     777
_refine_ls_restrained_S_all      1.229
_refine_ls_R_factor_all          0.2562
_refine_ls_R_factor_gt           0.1726
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_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          0.4108
_refine_ls_wR_factor_ref         0.4820
_reflns_Friedel_coverage         0.737
_reflns_Friedel_fraction_full    0.637
_reflns_Friedel_fraction_max     0.638
_reflns_number_gt                530
_reflns_number_total             992
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00461h2.cif
_cod_data_source_block           1_95_GPa
_cod_depositor_comments
'Adding full bibliography for 7126224--7126231.cif.'
_cod_original_cell_volume        3185(15)
_cod_database_code               7126225
_chemical_oxdiff_formula         'c34 h22 n2 f10 s2 i2 o1 '
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.398
_reflns_odcompleteness_completeness 64.04
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     15.83
_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, All O(H,H) groups
2. Restrained distances
 F10_$1-F1_$2
 2.55 with sigma of 0.02
 C8-C10
 1.45 with sigma of 0.02
 C25-C18
 1.5 with sigma of 0.02
 F9-C30 \\sim F10-C31 \\sim F7-C27 \\sim F8-C28
 with sigma of 0.02
 F6-F5 \\sim F3-F4 \\sim F2-F1
 with sigma of 0.02
 F5-C13 \\sim F6-C13 \\sim F3-C12 \\sim F4-C12 \\sim F1-C11 \\sim F2-C11
 with sigma of 0.02
 F6-C12 \\sim F5-C12 \\sim F3-C13 \\sim F4-C13
 with sigma of 0.02
 F2-C12 \\sim F4-C11 \\sim F1-C12 \\sim F3-C11
 with sigma of 0.02
 F6-C14 \\sim F5-C14 \\sim F2-C10 \\sim F1-C10
 with sigma of 0.02
 C4-C6 \\sim C6-C2
 with sigma of 0.02
 C7-C3 \\sim C3-S1
 with sigma of 0.02
 C17-C19 \\sim C14-C15 \\sim C10-C8 \\sim C3-C6
 with sigma of 0.02
 C20-C17 \\sim C17-C23
 with sigma of 0.02
 C15-C25 \\sim C25-S2
 with sigma of 0.02
3. Restrained planarity
 I1, C26, C31, C27, F10, C30, C28, F7, F9, C29, F8, I2
 with sigma of 0.1
 C3, N1, C5, C4, C2, C1, C8, C6, S1, C9, C7, C24
 with sigma of 0.1
 C16, C17, S2, C18, C15, C25, C20, C21, N2, C22, C23, C19
 with sigma of 0.1
 C15, C18, C14, C16
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
I1 \\sim I2 \\sim F8 \\sim F9 \\sim F10 \\sim C31 \\sim C30 \\sim C29 \\sim C28
\\sim C27 \\sim C26 \\sim F7: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C25 \\sim C24: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C29 \\sim I1 \\sim C26 \\sim C31 \\sim C27 \\sim F10 \\sim C30 \\sim C28 \\sim
F7 \\sim F9 \\sim F8 \\sim I2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
I2 \\sim C29 \\sim C30 \\sim C31 \\sim F10: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
F7 \\sim F9: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
I2 \\sim F9: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C9 \\sim C8 \\sim C7 \\sim C6 \\sim S1 \\sim C24 \\sim C3 \\sim C2 \\sim C1
\\sim N1 \\sim C5 \\sim C4: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
F3 \\sim F1 \\sim F5 \\sim F6 \\sim F2 \\sim F4 \\sim C14 \\sim C13 \\sim C12
\\sim C11 \\sim C10: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08
C8 \\sim C9 \\sim C24: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
F6 \\sim C13 \\sim F5: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C12 \\sim C13 \\sim F5: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C20 \\sim C21 \\sim N2 \\sim C22 \\sim C23 \\sim C19 \\sim S2 \\sim C18 \\sim
C16 \\sim C17 \\sim C25 \\sim C15: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C15 \\sim C18 \\sim C25: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C18 \\sim S2 \\sim C17 \\sim C16 \\sim C15 \\sim F5: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(F10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C29, I1, C26, C31, C27, F10, C30, C28, F7, F9, F8, I2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F9, C30, C29, I2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 I1, I2, F8, F9, F3, C3, C2, C1, N1, C5, C4, C25, C24, F10, F1, S2, C18, C15,
 C16, C17, C31, C30, C29, C28, C27, C26, F5, F6, F2, C20, C21, N2, C22, C23,
 C19, F7, C9, C8, C7, C6, S1, F4, C14, C13, C12, C11, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Free rotating group:
 O1(H,HA)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1), C5(H5), C4(H4), C16(H16), C20(H20), C21(H21), C22(H22),
 C23(H23), C7(H7)
6.c Fitted pentagon refined as free rotating group:
 C18(C15,C16,C17,S2), C8(C7,C6,S1,C9), C10(C14,C13,C12,C11)
6.d Fitted hexagon refined as free rotating group:
 C3(C2,C1,N1,C5,C4), C31(C30,C29,C28,C27,C26), C20(C21,N2,C22,C23,C19)
6.e Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              38153
_shelx_hkl_checksum              41818
_shelx_fab_checksum              33603
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.339
_oxdiff_exptl_absorpt_empirical_full_min 0.606