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_7126224
_publ_section_title
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 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, C3 H6 O'
_chemical_formula_sum            'C34 H22 F10 I2 N2 O S2'
_chemical_formula_weight         982.45
_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                   17.2715(8)
_cell_length_b                   27.171(3)
_cell_length_c                   7.9406(7)
_cell_measurement_reflns_used    3266
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.4680
_cell_measurement_theta_min      2.8930
_cell_volume                     3726.4(6)
_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      293.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -12.00  88.00   1.00   37.50    --   17.79  77.00  60.00  100
  2  \w     -8.00  90.00   1.00   37.50    --   17.79  37.00  30.00   98
  3  \w    -51.00  39.00   1.00   37.50    --   17.79 -57.00 -90.00   90
  4  \w    -78.00   1.00   1.00   37.50    --  -18.72 128.00-122.00   79
  5  \w    -88.00   3.00   1.00   37.50    --  -18.72 -57.00 120.00   91
  6  \w    -86.00  -7.00   1.00   37.50    --  -18.72 140.00  50.00   79
  7  \w    -40.00  50.00   1.00   37.50    --  -18.72  57.00  30.00   90
  8  \w    -49.00  51.00   1.00   37.50    --  -18.72  77.00-180.00  100
  9  \w    -88.00   3.00   1.00   37.50    --  -18.72 -57.00-120.00   91
 10  \w    -25.00   6.00   1.00   37.50    --  -18.72 -99.00-180.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0011650000
_diffrn_orient_matrix_UB_12      0.0242640000
_diffrn_orient_matrix_UB_13      0.0328873000
_diffrn_orient_matrix_UB_21      0.0019829000
_diffrn_orient_matrix_UB_22      0.0095815000
_diffrn_orient_matrix_UB_23      -0.0829225000
_diffrn_orient_matrix_UB_31      -0.0410212000
_diffrn_orient_matrix_UB_32      0.0011664000
_diffrn_orient_matrix_UB_33      -0.0030188000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1674
_diffrn_reflns_av_unetI/netI     0.1597
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            57440
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.366
_diffrn_reflns_theta_min         2.921
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.880
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.911
_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
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.046
_refine_diff_density_max         2.031
_refine_diff_density_min         -2.146
_refine_diff_density_rms         0.246
_refine_ls_abs_structure_details
;
 Flack x determined using 970 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         7588
_refine_ls_number_restraints     885
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.2522
_refine_ls_R_factor_gt           0.1685
_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^)+(0.1739P)^2^+92.8088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3775
_refine_ls_wR_factor_ref         0.4266
_reflns_Friedel_coverage         0.861
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4081
_reflns_number_total             7588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00461h2.cif
_cod_data_source_block           0_0001_GPa
_cod_depositor_comments
'Adding full bibliography for 7126224--7126231.cif.'
_cod_database_code               7126224
_chemical_oxdiff_formula         C34H22N2F10S2I2O1
_reflns_odcompleteness_completeness 99.75
_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
 C3-C6
 1.34 with sigma of 0.02
 C8-C10
 1.34 with sigma of 0.02
 C14-C15
 1.34 with sigma of 0.02
 S1-C3 \\sim C3-C7
 with sigma of 0.02
 C23-C17 \\sim C17-C20
 with sigma of 0.02
3. Rigid bond restraints
 C32A, H, HA, HB, C33A, O1A, C34A, HC, HD, HE, C32B, HF, HG, HH, O1B, C33B,
 C34B, HI, HJ, HK
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim N1 \\sim C5 \\sim C4 \\sim C3 \\sim C2: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04
C28 \\sim C27 \\sim C26 \\sim C31 \\sim C30 \\sim C29 \\sim F7 \\sim I1 \\sim
F10 \\sim F8 \\sim F9 \\sim I2: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
S1 \\sim C16 \\sim H16 \\sim C17 \\sim C15 \\sim S2 \\sim C19 \\sim C18 \\sim
C14 \\sim C23 \\sim C20 \\sim C25 \\sim C10 \\sim C13 \\sim C22 \\sim H23 \\sim
C21 \\sim H20 \\sim H25A \\sim H25B \\sim H25C \\sim C8 \\sim C11 \\sim F5
\\sim C12 \\sim F6 \\sim N2 \\sim H22 \\sim H21 \\sim C9 \\sim C7 \\sim F1
\\sim F2 \\sim F4 \\sim F3 \\sim C24 \\sim H7 \\sim C6 \\sim H24A \\sim H24B
\\sim H24C \\sim C3 \\sim C4 \\sim C2 \\sim C5 \\sim H4 \\sim H2 \\sim C1 \\sim
H5 \\sim N1 \\sim H1: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08
C9 \\sim S1 \\sim C6: within 2A with sigma of 0.02 and sigma for terminal atoms
of 0.04
S1 \\sim C6 \\sim C7 \\sim C8 \\sim C9: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04
C6 \\sim C7 \\sim C8 \\sim C9 \\sim S1: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C33B) \\sim Ueq, Uanis(C32B) \\sim Ueq, Uanis(O1B) \\sim Ueq, Uanis(C34B)
\\sim Ueq, : with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C34A) \\sim Ueq, Uanis(C32A) \\sim Ueq, Uanis(C33A) \\sim Ueq, Uanis(O1A)
\\sim Ueq, : with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O1A) \\sim Ueq, Uanis(O1B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O1B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 F7, I1, C26, C27, C31, C28, C30, F10, F8, C29, F9, I2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32A, H, HA, HB, C33A, O1A, C34A, HC, HD, C32B, HF, HG, HH, O1B, C33B, C34B,
 HI, HJ, HK, HE
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32A, H, HA, HB, C33A, O1A, C34A, HC, HD, HE, C32B, HF, HG, HH, O1B, C33B,
 C34B, HI, HJ, HK
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C9, I1, C26, C27, C31, F7, C28, C30, F10, F8, C29, F9, C24, I2, H24A, H24B,
 H24C, S1, C8, C6, C7, C10, C3, H7, C14, C11, C4, C2, C15, C13, C12, F1, F2, C5,
  H4, H2, C1, C16, C18, F5, F6, F4, F3, H5, N1, H1, H16, C17, S2, C25, C19,
 H25A, H25B, H25C, C23, C20, C22, H23, C21, H20, N2, H22, H21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C32A(0.5) H(0.5) HA(0.5) HB(0.5) C33A(0.5) O1A(0.5) C34A(0.5)
 HC(0.5) HD(0.5) HE(0.5) C32B(0.5) HF(0.5) HG(0.5) HH(0.5) O1B(0.5) C33B(0.5)
 C34B(0.5) HI(0.5) HJ(0.5) HK(0.5)
7.a Free rotating group:
 C32A(C33A,O1A,C34A,C32B,O1B,C33B,C34B)
7.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C7(H7), C21(H21), C22(H22), C23(H23), C20(H20), C5(H5), C4(H4),
 C2(H2), C1(H1)
7.c Fitted pentagon refined as free rotating group:
 C16(C17,S2,C18,C15), S1(C9,C8,C7,C6), C10(C14,C13,C12,C11)
7.d Fitted hexagon refined as free rotating group:
 C29(C28,C27,C26,C31,C30), C21(N2,C22,C23,C19,C20), C5(C4,C3,C2,C1,N1)
7.e Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C24(H24A,H24B,H24C), C32A(H,HA,HB), C34A(HC,HD,HE),
 C32B(HF,HG,HH), C34B(HI,HJ,HK)
;
_shelx_res_checksum              25491
_shelx_hkl_checksum              16271
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.250
_oxdiff_exptl_absorpt_empirical_full_min 0.829