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_7126230
_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                   17.606(3)
_cell_length_b                   25.580(17)
_cell_length_c                   6.944(9)
_cell_measurement_reflns_used    386
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.1040
_cell_measurement_theta_min      4.0650
_cell_volume                     3127(5)
_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    'XS (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 0.660
_diffrn_measured_fraction_theta_max 0.660
_diffrn_measurement_details
;
 Data were collected at room temperature and pressure of 2.50(2) GPa (2500000 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      0.0037928000
_diffrn_orient_matrix_UB_12      0.0155012000
_diffrn_orient_matrix_UB_13      0.0830293000
_diffrn_orient_matrix_UB_21      -0.0371635000
_diffrn_orient_matrix_UB_22      -0.0074253000
_diffrn_orient_matrix_UB_23      0.0296185000
_diffrn_orient_matrix_UB_31      0.0154252000
_diffrn_orient_matrix_UB_32      -0.0218666000
_diffrn_orient_matrix_UB_33      0.0503556000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2913
_diffrn_reflns_av_unetI/netI     0.1846
_diffrn_reflns_Laue_measured_fraction_full 0.660
_diffrn_reflns_Laue_measured_fraction_max 0.660
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            5210
_diffrn_reflns_point_group_measured_fraction_full 0.662
_diffrn_reflns_point_group_measured_fraction_max 0.662
_diffrn_reflns_theta_full        14.698
_diffrn_reflns_theta_max         14.698
_diffrn_reflns_theta_min         4.216
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.236
_exptl_absorpt_correction_T_max  0.445
_exptl_absorpt_correction_T_min  0.355
_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    2.002
_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          0.106
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details
;
 Flack x determined using 85 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.724
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         786
_refine_ls_number_restraints     916
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.2098
_refine_ls_R_factor_gt           0.1421
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.017
_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          0.3450
_refine_ls_wR_factor_ref         0.4147
_reflns_Friedel_coverage         0.739
_reflns_Friedel_fraction_full    0.664
_reflns_Friedel_fraction_max     0.664
_reflns_number_gt                446
_reflns_number_total             786
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00461h2.cif
_cod_data_source_block           2_5_GPa
_cod_depositor_comments
'Adding full bibliography for 7126224--7126231.cif.'
_cod_database_code               7126230
_chemical_oxdiff_formula         'Zn C15 F5 O5 N4 H10'
_shelx_estimated_absorpt_t_max   0.843
_shelx_estimated_absorpt_t_min   0.615
_reflns_odcompleteness_completeness 13.16
_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, All O(H,H) groups
2. Restrained distances
 F9_$1-F1_$2
 2.55 with sigma of 0.02
 F10_$1-F1_$2
 2.55 with sigma of 0.02
 C25-C24
 4.5 with sigma of 0.02
 H5_$3-H24A
 2.1 with sigma of 0.02
 C25-C18
 1.54 with sigma of 0.02
 S2-C17
 1.45 with sigma of 0.02
 C9-C24
 1.54 with sigma of 0.02
 C9-C18
 4.14 with sigma of 0.02
 C8-C10
 1.45 with sigma of 0.02
 C18-C15
 1.4 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
 F4-F2 \\sim F6-F4 \\sim F5-F3 \\sim F3-F1
 with sigma of 0.02
 C26-F10 \\sim F10-C30
 with sigma of 0.02
 C26-F7 \\sim F7-C28
 with sigma of 0.02
 C29-F8 \\sim F8-C27
 with sigma of 0.02
 C23-C17 \\sim C17-C20
 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
 C7-C6 \\sim C8-C7 \\sim C9-C8 \\sim C18-C15 \\sim C16-C15 \\sim C17-C16
 with sigma of 0.02
 S1-C6 \\sim S1-C9 \\sim S2-C18 \\sim S2-C17
 with sigma of 0.02
 F1-C12 \\sim F3-C11 \\sim F4-C11 \\sim F2-C12 \\sim F6-C12 \\sim F4-C13 \\sim
F5-C12 \\sim F3-C13
 with sigma of 0.02
 C8-C10 \\sim C14-C15
 with sigma of 0.02
 C6-C3 \\sim C8-C10 \\sim C15-C14 \\sim C19-C17
 with sigma of 0.02
3. Restrained planarity
 I2, F8, F10, C26, C31, C30, C29, C28, C27, F9, F7, I1
 with sigma of 0.1
 S2, C18, C15, C16, C17, C19, C20, C21, N2, C22, C23, C25
 with sigma of 0.1
 C2, C4, C7, C6, C3
 with sigma of 0.1
 C4, C3, C1, N1, C5, S1, C9, C6, C2, C8, C7, C24
 with sigma of 0.1
 C15, C14, C10, C11, C12, C13
 with sigma of 0.1
 C14, C10, C13, C15
 with sigma of 0.1
 C8, C7, C9, C10
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
I1 \\sim C26 \\sim C31 \\sim C27 \\sim F10 \\sim C30 \\sim C28 \\sim F7 \\sim
C29 \\sim F9 \\sim F8 \\sim I2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C23 \\sim C22 \\sim N2 \\sim C21 \\sim C20 \\sim C19: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
N1 \\sim C5 \\sim C4 \\sim C3 \\sim C2 \\sim C1: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C16 \\sim C17 \\sim S2 \\sim C18 \\sim C15 \\sim C25: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C7 \\sim C8 \\sim C9 \\sim S1 \\sim C6 \\sim C24: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C10 \\sim C14 \\sim C13 \\sim C12 \\sim C11 \\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
Uanis(C26) \\sim Ueq, Uanis(I1) \\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(F8) \\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
Uanis(N2) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(O1) \\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(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(S2) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
5. Rigid body (RIGU) restrains
 N2, N1, S1, C1, C6, F10, C18, C15, C5, F9, S2, C31, F4, C13, F1, C25, F7, O1,
 C28, F3, C21, C3, C4, C9, C17, C26, C16, C8, C2, C10, C12, C22, C7, C29, C14,
 F6, F5, F2, C30, C27, C24, C11, F8, I1, I2, C23, C19, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Free rotating group:
 O1(H1A,H1B)
6.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C20(H20), C21(H21), C22(H22), C4(H4), C2(H2), C1(H1), C5(H5),
 C7(H7), C16(H16)
6.c Fitted pentagon refined as free rotating group:
 C10(C14,C13,C12,C11)
6.d Fitted hexagon refined as free rotating group:
 C23(C19,C20,C21,N2,C22), C4(C3,C2,C1,N1,C5), C27(C26,C31,C30,C29,C28)
6.e Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              13004
_shelx_hkl_checksum              31962
_shelx_fab_checksum              23905
_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 1.950
_oxdiff_exptl_absorpt_empirical_full_min 0.531