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_7126227
_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                   17.556(4)
_cell_length_b                   26.464(17)
_cell_length_c                   7.633(2)
_cell_measurement_reflns_used    774
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.2720
_cell_measurement_theta_min      3.6130
_cell_volume                     3546(3)
_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 0.659
_diffrn_measurement_details
;
 Data were collected at room temperature and pressure of 0.40(2) GPa
 (400000 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      0.0063269000
_diffrn_orient_matrix_UB_12      0.0215516000
_diffrn_orient_matrix_UB_13      0.0518712000
_diffrn_orient_matrix_UB_21      0.0250639000
_diffrn_orient_matrix_UB_22      0.0098134000
_diffrn_orient_matrix_UB_23      -0.0651040000
_diffrn_orient_matrix_UB_31      -0.0313783000
_diffrn_orient_matrix_UB_32      0.0121509000
_diffrn_orient_matrix_UB_33      -0.0417804000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2456
_diffrn_reflns_av_unetI/netI     0.6940
_diffrn_reflns_Laue_measured_fraction_full 0.659
_diffrn_reflns_Laue_measured_fraction_max 0.659
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            18081
_diffrn_reflns_point_group_measured_fraction_full 0.646
_diffrn_reflns_point_group_measured_fraction_max 0.646
_diffrn_reflns_theta_full        24.710
_diffrn_reflns_theta_max         24.710
_diffrn_reflns_theta_min         3.807
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.968
_exptl_absorpt_correction_T_max  0.427
_exptl_absorpt_correction_T_min  0.236
_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    1.731
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.046
_refine_diff_density_max         1.039
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.178
_refine_ls_abs_structure_details
;
 Flack x determined using 144 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.10(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         3900
_refine_ls_number_restraints     700
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.4824
_refine_ls_R_factor_gt           0.2025
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.025
_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          0.4301
_refine_ls_wR_factor_ref         0.5737
_reflns_Friedel_coverage         0.809
_reflns_Friedel_fraction_full    0.630
_reflns_Friedel_fraction_max     0.630
_reflns_number_gt                718
_reflns_number_total             3900
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00461h2.cif
_cod_data_source_block           0_4_GPa
_cod_depositor_comments
'Adding full bibliography for 7126224--7126231.cif.'
_cod_database_code               7126227
_chemical_oxdiff_formula         'C34 H22 N2 O1 F10 S2 I2 '
_shelx_estimated_absorpt_t_max   0.831
_shelx_estimated_absorpt_t_min   0.487
_reflns_odcompleteness_completeness 61.94
_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
 C11-F1
 1.5 with sigma of 0.02
 C13-F6
 1.5 with sigma of 0.02
 F4-C12
 1.54 with sigma of 0.02
 C13-F5
 1.54 with sigma of 0.02
 C12-F3
 1.54 with sigma of 0.02
 C19-C17
 1.45 with sigma of 0.02
 C8-C10
 1.45 with sigma of 0.02
 C15-C14
 1.45 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
 F10-C31 \\sim F7-C27 \\sim F8-C28 \\sim F9-C30
 with sigma of 0.02
 C26-F10 \\sim F10-C30
 with sigma of 0.02
 C28-F7 \\sim F7-C26
 with sigma of 0.02
 C28-I2 \\sim I2-C30
 with sigma of 0.02
 S2-C19 \\sim C19-C16
 with sigma of 0.02
 F2-F1 \\sim F4-F3 \\sim F6-F5
 with sigma of 0.02
 F4-F1 \\sim F3-F2 \\sim F5-F4 \\sim F6-F3
 with sigma of 0.02
 F3-C13 \\sim F5-C12 \\sim F2-C12 \\sim F3-C11 \\sim F1-C12 \\sim F4-C11 \\sim
F6-C12 \\sim F4-C13
 with sigma of 0.02
 F2-C11 \\sim F1-C11 \\sim F3-C12 \\sim F4-C12 \\sim F5-C13 \\sim F6-C13
 with sigma of 0.02
3. Restrained planarity
 I1, I2, F8, F9, F10, C27, C26, C31, C30, C29, C28, F7
 with sigma of 0.1
 C3, C2, C1, N1, C5, C4, C9, C8, C7, C6, S1, C24
 with sigma of 0.1
 C25, C18, S2, C15, C16, C17, C19, C23, C22, N2, C21, C20
 with sigma of 0.1
 C7, C6, S1, C9, C8, C4, C5, N1, C1, C2, C3, C24
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C19 \\sim C23 \\sim C22 \\sim N2 \\sim C21 \\sim C20: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C26 \\sim C31 \\sim C30 \\sim C29 \\sim C28 \\sim C27: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C4 \\sim C5 \\sim N1 \\sim C1 \\sim C2 \\sim C3: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C14 \\sim C10: within 2A with sigma of 0.1 and sigma for terminal atoms of 0.2
C9 \\sim S1 \\sim C6 \\sim C7 \\sim C8: 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
0.04 and sigma for terminal atoms of 0.08
Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F5) \\sim Ueq, Uanis(F1) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C10) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
5. Rigid body (RIGU) restrains
 F7, I1, C26, C27, C31, C28, F10, C30, F8, C29, F9, I2, C16, F3, C12, F4, C13,
 C11, F5, F6, C14, F1, F2, C10, C15, C8, C18, C9, C7, C25, S2, H16, C17, C24,
 S1, H7, C6, H25A, H25B, H25C, C19, H24A, H24B, H24C, C3, C20, C23, C2, C4, H20,
  C21, C22, H23, H2, C1, C5, H4, H21, N2, H22, H1, N1, H5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a 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.b Fitted pentagon refined as free rotating group:
 S2(C18,C15,C16,C17), C9(C8,C7,C6,S1), C14(C13,C12,C11,C10)
6.c Fitted hexagon refined as free rotating group:
 C3(C2,C1,N1,C5,C4), C27(C26,C31,C30,C29,C28), C19(C20,C21,N2,C22,C23)
6.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              81155
_shelx_hkl_checksum              59676
_shelx_fab_checksum              79077
_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 6.699
_oxdiff_exptl_absorpt_empirical_full_min 0.575