(Z)-4,4′-Stilbene dicarboxylic acid, the overlooked metal–organic framework linker
Hunter, Lucy R.; Karlsson, Joshua K. G.; Sellars, Jonathan D.; Probert, Michael R.; CrystEngComm 25 (2023) 2353–2358; doi:10.1039/D3CE00138E

data_7246512
_publ_section_title
;
 (Z)-4,4&#x2032;-Stilbene dicarboxylic acid, the overlooked metal--organic
 framework linker
;
_journal_issue                   16
_journal_name_full               CrystEngComm
_journal_page_first              2353
_journal_page_last               2358
_journal_paper_doi               10.1039/D3CE00138E
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C64 H50 O20 Sm2, 5(C3 H7 N O)'
_chemical_formula_sum            'C79 H85 N5 O25 Sm2'
_chemical_formula_weight         1805.21
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-06
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-01-06 deposited with the CCDC.	2023-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                91.2650(10)
_cell_angle_beta                 93.9650(10)
_cell_angle_gamma                93.6030(10)
_cell_formula_units_Z            2
_cell_length_a                   9.65620(10)
_cell_length_b                   11.69050(10)
_cell_length_c                   35.0640(4)
_cell_measurement_reflns_used    41741
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.2430
_cell_measurement_theta_min      2.0680
_cell_volume                     3939.56(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     -2.00  48.00   0.50    3.22    --    8.74-102.00  78.00  100
  2  \w    -88.00   2.00   0.50    3.22    --   -8.04 -38.00-180.00  180
  3  \w    -89.00 -35.00   0.50    3.22    --   -8.04 -19.00 -90.00  108
  4  \w    -72.00 -35.00   0.50    3.22    --    8.74 -19.00 -30.00   74
  5  \w     -7.00  39.00   0.50    3.22    --    8.74  57.00  60.00   92
  6  \w     -7.00  39.00   0.50    3.22    --    8.74  57.00-180.00   92
  7  \w    -21.00  32.00   0.50    3.22    --    8.74 -77.00   0.00  106
  8  \w     -7.00  39.00   0.50    3.22    --    8.74  57.00 -30.00   92
  9  \w    -72.00 -35.00   0.50    3.22    --    8.74 -19.00  60.00   74
 10  \w     -7.00  39.00   0.50    3.22    --    8.74  57.00-150.00   92
 11  \w     -4.00  46.00   0.50    3.22    --    8.74 -99.00-180.00  100
 12  \w     -7.00  33.00   0.50    3.22    --    8.74  57.00-120.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0118826000
_diffrn_orient_matrix_UB_12      -0.0459880000
_diffrn_orient_matrix_UB_13      0.0124748000
_diffrn_orient_matrix_UB_21      0.0121844000
_diffrn_orient_matrix_UB_22      -0.0396685000
_diffrn_orient_matrix_UB_23      -0.0148061000
_diffrn_orient_matrix_UB_31      0.0717957000
_diffrn_orient_matrix_UB_32      0.0031542000
_diffrn_orient_matrix_UB_33      0.0060509000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            61624
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         1.855
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.557
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.517
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.63a (Rigaku Oxford Diffraction, 2022)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       plate
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1028
_refine_ls_number_reflns         14946
_refine_ls_number_restraints     808
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0229
_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^)+(0.0210P)^2^+1.9215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0503
_refine_ls_wR_factor_ref         0.0524
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13082
_reflns_number_total             14946
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00138e2.cif
_cod_data_source_block           sm_stilbene_2d_fa
_cod_depositor_comments
'Adding full bibliography for 7246512--7246521.cif.'
_cod_database_code               7246512
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Sm2 C79 O10 N5 H60'
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.716
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O02S-C65 \\sim O21-C65
 with sigma of 0.02
 Sm1-H9A \\sim Sm1-H9B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O21)=Sof(H65A)=1-FVAR(1)
 Sof(O02S)=Sof(H65)=FVAR(1)
5.a Free rotating group:
 O9(H9A,H9B)
5.b Rotating group:
 O7(H7A,H7B), O8(H8A,H8B), O10(H10A,H10B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14A), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25),
 C27(H27), C28(H28), C30(H30), C31(H31), C35(H35), C36(H36), C38(H38), C39(H39),
  C40(H40), C41(H41), C43(H43), C44(H44), C46(H46), C47(H47), C51(H51),
 C52(H52), C54(H54), C55(H55), C56(H56), C57(H57), C59(H59), C60(H60), C62(H62),
  C63(H63), C65(H65A), C65(H65), C70(H70), C71(H71), C74(H74), C79(H79)
5.d Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C69(H69A,H69B,
 H69C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C75(H75A,H75B,H75C), C76(H76A,
 H76B,H76C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C)
5.e Idealised tetrahedral OH refined as rotating group:
 O14(H14), O16(H16)
;
_shelx_res_checksum              94870
_shelx_hkl_checksum              25050
_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 1.176
_oxdiff_exptl_absorpt_empirical_full_min 0.873