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_7126228
_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, C24.85 H16 F6 N2 S2, C3 H6 O, H2 O'
_chemical_formula_sum            'C33.85 H24 F10 I2 N2 O2 S2'
_chemical_formula_weight         998.70
_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                   17.2451(6)
_cell_length_b                   27.2415(16)
_cell_length_c                   7.9554(3)
_cell_measurement_reflns_used    5224
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4780
_cell_measurement_theta_min      3.2280
_cell_volume                     3737.3(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      293.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -53.00  45.00   1.00  100.00    --   16.55 -77.00 -30.00   98
  2  \w    -52.00  35.00   1.00  100.00    --   16.55 -57.00-150.00   87
  3  \w     34.00  91.00   1.00  100.00    --   16.55 179.00-120.00   57
  4  \w    -21.00  89.00   1.00  100.00    --   16.55  19.00  30.00  110
  5  \w    -25.00  57.00   1.00  100.00    --   16.55 -99.00  90.00   82
  6  \w    -25.00  23.00   1.00  100.00    --  -17.41 -99.00 -90.00   48
  7  \w    -25.00  10.00   1.00  100.00    --  -17.41 -99.00  60.00   35
  8  \w    -86.00   1.00   1.00  100.00    --  -17.41 -57.00-180.00   87
;
_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      0.0144051000
_diffrn_orient_matrix_UB_12      0.0224496000
_diffrn_orient_matrix_UB_13      0.0325746000
_diffrn_orient_matrix_UB_21      0.0383299000
_diffrn_orient_matrix_UB_22      -0.0073525000
_diffrn_orient_matrix_UB_23      -0.0203512000
_diffrn_orient_matrix_UB_31      -0.0038315000
_diffrn_orient_matrix_UB_32      0.0109540000
_diffrn_orient_matrix_UB_33      -0.0804648000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0942
_diffrn_reflns_av_unetI/netI     0.0953
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            44072
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.917
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.878
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.843
_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_density_diffrn    1.775
_exptl_crystal_description       block
_exptl_crystal_F_000             1940
_exptl_crystal_size_max          0.327
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.046
_refine_diff_density_max         1.375
_refine_diff_density_min         -1.220
_refine_diff_density_rms         0.164
_refine_ls_abs_structure_details
;
 Flack x determined using 1412 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.024(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7610
_refine_ls_number_restraints     588
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1592
_refine_ls_R_factor_gt           0.1190
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.042
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1004P)^2^+47.3128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2469
_refine_ls_wR_factor_ref         0.2726
_reflns_Friedel_coverage         0.861
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                5292
_reflns_number_total             7610
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00461h2.cif
_cod_data_source_block           0_0001_GPa_H2O
_cod_depositor_comments
'Adding full bibliography for 7126224--7126231.cif.'
_cod_database_code               7126228
_chemical_oxdiff_formula         'C31 H24 F10 O1 S2 N2 I2'
_reflns_odcompleteness_completeness 98.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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
 C33A-O1A
 1.2 with sigma of 0.02
 C32A-C34A
 2.1 with sigma of 0.02
 C33B-C34B
 1.4 with sigma of 0.02
 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
 O1B-C33B \\sim O1A-C33A
 with sigma of 0.02
 C32B-C34B \\sim C34A-C32A
 with sigma of 0.02
 O1A-C32A \\sim O1A-C34A \\sim O1B-C34B \\sim O1B-C32B
 with sigma of 0.02
 C33B-C34B \\sim C32B-C33B \\sim C33A-C32A \\sim C33A-C34A
 with sigma of 0.02
3. Restrained planarity
 C33B, O1B, C32B, C34B
 with sigma of 0.1
4. Rigid bond restraints
 O1B, C33B, C34B, C32B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C9 \\sim S2 \\sim C18 \\sim C17 \\sim C15 \\sim C25 \\sim C16 \\sim C19 \\sim
C14 \\sim C23 \\sim C20 \\sim C13 \\sim C10 \\sim C22 \\sim C21 \\sim F5 \\sim
C12 \\sim F6 \\sim C8 \\sim C11 \\sim N2 \\sim F4 \\sim F3 \\sim C7 \\sim F1
\\sim F2 \\sim S1 \\sim C24 \\sim C6 \\sim C3 \\sim C2 \\sim C4 \\sim C1 \\sim
C5 \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C32A \\sim O1A \\sim C33A \\sim C34A: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(O1B) \\sim Ueq, Uanis(O1W) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O1B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O1B) \\sim Ueq, Uanis(C33B) \\sim Ueq, Uanis(C34A) \\sim Ueq, Uanis(C34B)
\\sim Ueq, Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C33A) \\sim Ueq, Uanis(C32B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C34A) \\sim Ueq, Uanis(C32A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C34B) \\sim Ueq, Uanis(C34A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C34A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
6. Rigid body (RIGU) restrains
 C30, C29, C28, C27, C26, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14, C13, C12, C11, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, C6, S1, C9, C8, C4, C5, N1, C1, C2, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17, C16, C15, C18, S2, C19, C20, C21, N2, C22, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C34A, O1A, C33A, C32A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32A, O1A, C33A, C34A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C33B, O1B, C32B, C34B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32B, O1B, C33B, C34B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: O1B(0.5) C33B(0.5) O1A(0.5) C32A(0.5) H32D(0.5) H32E(0.5)
 H32F(0.5) C33A(0.5) C34A(0.5) H34D(0.5) H34E(0.5) H34F(0.5) C32B(0.5)
 H32A(0.5) H32B(0.5) H32C(0.5) C34B(0.5) H34A(0.5) H34B(0.5) H34C(0.5)
8.a Free rotating group:
 O1W(H1WA,H1WB)
8.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C7(H7), C21(H21), C22(H22), C23(H23), C20(H20), C1(H1), C5(H5),
 C4(H4), C2(H2)
8.c Fitted pentagon refined as free rotating group:
 C16(C17,S2,C18,C15), S1(C9,C8,C7,C6), C10(C14,C13,C12,C11)
8.d Fitted hexagon refined as free rotating group:
 C28(C27,C26,C31,C30,C29), C21(N2,C22,C23,C19,C20), C1(N1,C5,C4,C3,C2)
8.e Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C24(H24A,H24B,H24C), C32A(H32D,H32E,H32F), C34A(H34D,
 H34E,H34F), C32B(H32A,H32B,H32C), C34B(H34A,H34B,H34C)
;
_shelx_res_checksum              26201
_shelx_hkl_checksum              30765
_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 1.310
_oxdiff_exptl_absorpt_empirical_full_min 0.621