The benefits of Cu Kβ radiation for the single-crystal X-ray structure determination of crystalline sponges
Meurer, Florian; von Essen, Carolina; Kühn, Clemens; Puschmann, Horst; Bodensteiner, Michael; IUCrJ 9 (2022) –; doi:10.1107/S2052252522002147

data_1566586
_publ_section_title
;
 The benefits of Cu K\b radiation for the single-crystal X-ray structure
 determination of crystalline sponges
;
_journal_issue                   3
_journal_name_full               IUCrJ
_journal_paper_doi               10.1107/S2052252522002147
_journal_volume                  9
_journal_year                    2022
_chemical_formula_moiety         'C36 H24 I6 N12 Zn3, 9.563(C3 H6)'
_chemical_formula_sum            'C64.69 H81.39 I6 N12 Zn3'
_chemical_formula_weight         1984.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-02-17
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.12.21 svn.raa29eb21 for OlexSys, GUI svn.r6440)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.6467(15)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.5950(6)
_cell_length_b                   15.1725(3)
_cell_length_c                   29.5350(4)
_cell_measurement_reflns_used    15473
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.4770
_cell_measurement_theta_min      3.8820
_cell_volume                     15235.8(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.47a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.47a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.47a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.877
_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    -44.00  25.00   1.00   12.50    --  -44.42  57.00 -90.00   69
  2  \w   -119.00  30.00   1.00   12.50    --  -44.42   0.00 -90.00  149
  3  \w     -4.00  31.00   1.00   12.50    --  -44.42  19.00 -60.00   35
  4  \w    -44.00  25.00   1.00   12.50    --  -44.42  57.00 -60.00   69
  5  \w     81.00 177.00   1.00   50.00    --  104.50  30.00-180.00   96
  6  \w    103.00 176.00   1.00   50.00    --  104.50  77.00-180.00   73
  7  \w     33.00 127.00   1.00   50.00    --  104.50 -77.00  90.00   94
  8  \w     97.00 176.00   1.00   50.00    --  104.50 125.00-180.00   79
  9  \w     35.00  72.00   1.00   50.00    --  104.50 -61.00 -90.00   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction SuperNova, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_wavelength     1.39222
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0788
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            44970
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        56.650
_diffrn_reflns_theta_max         74.433
_diffrn_reflns_theta_min         3.830
_exptl_absorpt_coefficient_mu    15.175
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.47a (Rigaku Oxford Diffraction, 2019)
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    1.730
_exptl_crystal_description       block
_exptl_crystal_F_000             7692
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.088
_refine_diff_density_max         1.275
_refine_diff_density_min         -1.939
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     930
_refine_ls_number_reflns         18533
_refine_ls_number_restraints     387
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0869
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0153P)^2^+530.6456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1699
_refine_ls_wR_factor_ref         0.1796
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14067
_reflns_number_total             18533
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5046.cif
_cod_data_source_block           beta_cyc_zni2
_cod_database_code               1566586
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.349
_shelx_estimated_absorpt_t_min   0.206
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C1A-C1E \\sim C1C-C1E \\sim C1B-C1F \\sim C1B-C1D \\sim C1D-C1F \\sim C1A-C1C
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C1E \\sim C1A \\sim C1B \\sim C1F \\sim C1C \\sim C1D: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 2A
N52 \\sim N22 \\sim N22A: within 2A with sigma of 0.0001 and sigma for terminal
atoms of 0.0001 within 2A
C1 \\sim C2 \\sim C3 \\sim C5 \\sim C6 \\sim C7: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.01 within 2A
C63 \\sim C64 \\sim C65 \\sim C62 \\sim C66 \\sim C61: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.02 within 2A
I5A \\sim I5: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.02
within 2A
I6 \\sim I6A: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.02
within 2A
Zn9A \\sim Zn9: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.02 within 2A
C39 \\sim C37 \\sim C35 \\sim C28 \\sim C16 \\sim C22: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.02 within 2A
C73 \\sim C76 \\sim C77 \\sim C75 \\sim C78 \\sim C74: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.02 within 2A
C4 \\sim C8 \\sim C9 \\sim C11 \\sim C13 \\sim C15: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.005 within 2A
C27 \\sim C23 \\sim C24 \\sim C26: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.002 within 2A
C25A \\sim C25: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
C27A \\sim C27: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
C26A \\sim C26: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
C24 \\sim C26 \\sim C26A: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004 within 2A
C25 \\sim C25A \\sim C55: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004 within 2A
C27 \\sim C27A \\sim C23: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004 within 2A
Uanis(N22) \\sim Ueq, Uanis(N22A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C27) \\sim Ueq, Uanis(C27A) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C26A)
\\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C25A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C1A, C1B, C1C, C1D, C1E, C1F
 with sigma for 1-2 distances of 0.04 and sigma for 1-3 distances of 0.04
 I5, Zn9, I6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 I5A, Zn9A, I6A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(N22)=Sof(C25)=Sof(C27)=Sof(H27)=Sof(C26)=Sof(H26)=Sof(Zn9A)=Sof(I5A)=
 Sof(I6A)=1-FVAR(1)
 Sof(I5)=Sof(I6)=Sof(Zn9)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(N22A)=
 Sof(C25A)=FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C1C)=Sof(H1CA)=
 Sof(H1CB)=Sof(C1D)=Sof(H1DA)=Sof(H1DB)=Sof(C1E)=Sof(H1EA)=Sof(H1EB)=Sof(C1F)=
 Sof(H1FA)=Sof(H1FB)=0.5*FVAR(3)
 Fixed Sof: C4(0.66667) H4A(0.66667) H4B(0.66667) C8(0.66667) H8A(0.66667)
 H8B(0.66667) C9(0.66667) H9A(0.66667) H9B(0.66667) C11(0.66667) H11A(0.66667)
 H11B(0.66667) C13(0.66667) H13A(0.66667) H13B(0.66667) C15(0.66667)
 H15A(0.66667) H15B(0.66667) C22(0.33333) H22A(0.33333) H22B(0.33333)
 C16(0.33333) H16A(0.33333) H16B(0.33333) C39(0.33333) H39A(0.33333)
 H39B(0.33333) C35(0.33333) H35A(0.33333) H35B(0.33333) C28(0.33333)
 H28A(0.33333) H28B(0.33333) C37(0.33333) H37A(0.33333) H37B(0.33333)
6.a Secondary CH2 refined with riding coordinates:
 C59(H59A,H59B), C58(H58A,H58B), C64(H64A,H64B), C63(H63A,H63B), C60(H60A,
 H60B), C65(H65A,H65B), C62(H62A,H62B), C66(H66A,H66B), C61(H61A,H61B),
 C76(H76A,H76B), C77(H77A,H77B), C74(H74A,H74B), C78(H78A,H78B), C75(H75A,H75B),
  C73(H73A,H73B), C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,
 H6B), C7(H7A,H7B), C4(H4A,H4B), C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B),
 C13(H13A,H13B), C15(H15A,H15B), C22(H22A,H22B), C16(H16A,H16B), C39(H39A,H39B),
  C35(H35A,H35B), C28(H28A,H28B), C37(H37A,H37B), C1A(H1AA,H1AB), C1B(H1BA,
 H1BB), C1C(H1CA,H1CB), C1D(H1DA,H1DB), C1E(H1EA,H1EB), C1F(H1FA,H1FB)
6.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C20(H20), C30(H30), C21(H21), C18(H18), C48(H48), C41(H41),
 C32(H32), C47(H47), C29(H29), C45(H45), C24(H24), C44(H44), C56(H56), C42(H42),
  C53(H53), C57(H57), C33(H33), C54(H54), C23(H23), C50(H50), C51(H51),
 C27(H27), C26(H26), C26A(H26A), C27A(H27A)
;
_shelx_res_checksum              58118
_shelx_hkl_checksum              18305
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_original_sample_id beta_cyc_zni2
_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
;