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_1566582
_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 Cl6 N12 Zn3, C11.098 H12.197 O2, C10.332 H10.664 O2, 1.733(C6 H12), 0.157(C6 H10)'
_chemical_formula_sum            'C68.62 H68.92 Cl6 N12 O4 Zn3'
_chemical_formula_weight         1534.51
_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                 102.247(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.3060(13)
_cell_length_b                   14.4880(4)
_cell_length_c                   31.8026(11)
_cell_measurement_reflns_used    10445
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.6130
_cell_measurement_theta_min      2.3870
_cell_volume                     14996.7(9)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.972
_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    -22.00  28.00   1.00   30.00    --  -43.64  38.00-150.00   50
  2  \w    -44.00  26.00   1.00   30.00    --  -43.64  57.00 120.00   70
  3  \w    -22.00  28.00   1.00   30.00    --  -43.64  38.00   0.00   50
  4  \w     -5.00  34.00   1.00   30.00    --  -43.64  19.00 -90.00   39
  5  \w    -44.00  26.00   1.00   30.00    --  -43.64  57.00-120.00   70
  6  \w     -5.00  34.00   1.00   30.00    --  -43.64  19.00-120.00   39
  7  \w     -5.00  34.00   1.00   30.00    --  -43.64  19.00 -60.00   39
  8  \w     30.00 127.00   1.00   90.00    --  104.50 -77.00-180.00   97
  9  \w     35.00  93.00   1.00   90.00    --  104.50 -61.00-150.00   58
 10  \w     35.00  93.00   1.00   90.00    --  104.50 -61.00 120.00   58
 11  \w     80.00 175.00   1.00   90.00    --  104.50  45.00 120.00   95
 12  \w     34.00  72.00   1.00   90.00    --  104.50 -45.00 150.00   38
 13  \w     31.00 112.00   1.00   90.00    --  104.50-125.00 -30.00   81
 14  \w     34.00  72.00   1.00   90.00    --  104.50 -45.00   0.00   38
 15  \w     65.00 178.00   1.00   90.00    --  104.50  15.00  60.00  113
 16  \w     34.00  72.00   1.00   90.00    --  104.50 -45.00 -30.00   38
 17  \w     34.00  72.00   1.00   90.00    --  104.50 -45.00-120.00   38
 18  \w     80.00 175.00   1.00   90.00    --  104.50  45.00 -30.00   95
 19  \w     34.00  72.00   1.00   90.00    --  104.50 -45.00  30.00   38
 20  \w     30.00 127.00   1.00   90.00    --  104.50 -77.00   0.00   97
 21  \w   -113.00 -18.00   1.00   30.00    --  -43.64 -57.00 -30.00   95
 22  \w   -113.00 -18.00   1.00   30.00    --  -43.64 -57.00  60.00   95
 23  \w   -113.00 -18.00   1.00   30.00    --  -43.64 -57.00-150.00   95
 24  \w   -113.00 -18.00   1.00   30.00    --  -43.64 -57.00 -90.00   95
 25  \w   -113.00 -18.00   1.00   30.00    --  -43.64 -57.00 120.00   95
 26  \w     31.00  57.00   1.00   90.00    --  104.50 -30.00  60.00   26
 27  \w     78.00 178.00   1.00   90.00    --  104.50  30.00-120.00  100
 28  \w     78.00 103.00   1.00   90.00    --  104.50  61.00 -90.00   25
 29  \w     78.00 165.00   1.00   90.00    --  104.50  61.00 150.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction SuperNova, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\b'
_diffrn_radiation_wavelength     1.39222
_diffrn_reflns_av_R_equivalents  0.1070
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            125662
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        56.650
_diffrn_reflns_theta_max         75.676
_diffrn_reflns_theta_min         2.452
_exptl_absorpt_coefficient_mu    2.497
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.934
_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    1.359
_exptl_crystal_description       block
_exptl_crystal_F_000             6309
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.650
_refine_diff_density_min         -1.120
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1285
_refine_ls_number_reflns         20597
_refine_ls_number_restraints     390
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.0738
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1195P)^2^+15.0864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1901
_refine_ls_wR_factor_ref         0.2540
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11668
_reflns_number_total             20597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5046.cif
_cod_data_source_block           beta_me-daid_zncl2
_cod_database_code               1566582
_shelx_shelxl_version_number     2016/6
_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
2. Restrained distances
 Zn-Cl \\sim Zn03-Cl09 \\sim Zn03-Cl2 \\sim Zn-Cl2A
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Zn \\sim Zn03: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.001 within 2A
Cl \\sim Cl09 \\sim Cl2A \\sim Cl2: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 2A
C02L \\sim C026 \\sim C02A \\sim C025 \\sim C02T \\sim C02W: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.02 within 2A
C38 \\sim C23 \\sim C41 \\sim C40 \\sim C39 \\sim C37: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 2A
C26 \\sim C27 \\sim C28 \\sim C20 \\sim C29 \\sim C42: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 2A
C36 \\sim C33 \\sim C34 \\sim C32 \\sim C31 \\sim C30: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 2A
C43 \\sim C44: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.04 within 2A
C00M \\sim C01I \\sim C01A \\sim C00N \\sim C016 \\sim C00O \\sim C01E \\sim
C00P \\sim C014 \\sim C00Q \\sim C018 \\sim C00R \\sim C01C \\sim C00S \\sim
C01G \\sim C00T \\sim C01L \\sim C00U \\sim C015 \\sim C00V \\sim C017 \\sim
C00W \\sim C019 \\sim C00X \\sim C01B \\sim C00Y \\sim C01D \\sim C00Z \\sim
C01F \\sim C010 \\sim C01H \\sim C011 \\sim C01J \\sim C012 \\sim C01M \\sim
C013: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
Uanis(C43) \\sim Ueq, Uanis(O02D) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C01M) \\sim Ueq, Uanis(C01L) \\sim Ueq, Uanis(C01D) \\sim Ueq,
Uanis(C01F) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Sof(Cl2A)=Sof(Cl)=Sof(Zn)=1-FVAR(1)
 Sof(Zn03)=Sof(Cl09)=Sof(Cl2)=FVAR(1)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=
 Sof(H22B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C35)=
 Sof(H35A)=Sof(H35B)=FVAR(2)
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C19)=Sof(H19A)=
 Sof(H19B)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(C11)=
 Sof(H11A)=Sof(H11B)=FVAR(3)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2C)=Sof(H2D)=Sof(C4)=Sof(H4A)=Sof(H4B)=
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C9)=Sof(H9A)=Sof(H9B)=
 FVAR(4)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C8)=Sof(H8A)=Sof(H8B)=
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C17)=Sof(H17A)=
 Sof(H17B)=FVAR(5)
 Sof(C33)=Sof(H01P)=Sof(H33)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C34)=Sof(H34A)=
 Sof(H34B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C31)=
 Sof(H31A)=Sof(H31B)=FVAR(6)
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C20)=Sof(H20A)=
 Sof(H20B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C29)=Sof(H2A)=Sof(H2B)=Sof(C42)=
 Sof(H42A)=Sof(H42B)=FVAR(7)
 Sof(C23)=Sof(H23)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(C41)=Sof(H41)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C39)=Sof(H39A)=Sof(H39B)=
 FVAR(8)
 Fixed Sof: O01K(0.5) O01N(0.5) O(0.5) O01P(0.5) C01Q(0.5) C01T(0.5) H01T(0.5)
 C02P(0.5) C02K(0.5) C02R(0.5) H02R(0.5) C028(0.5) H028(0.5) O01R(0.5)
 C01S(0.5) O1(0.5) C01V(0.5) H01V(0.5) C01W(0.5) O2(0.5) C01Y(0.5) C01Z(0.5)
 H01Z(0.5) C020(0.5) C021(0.5) H021(0.5) C022(0.5) C023(0.5) H023(0.5)
 C024(0.5) H024(0.5) C029(0.5) H029(0.5) C02B(0.5) H02B(0.5) C02C(0.5)
 O02D(0.5) C02E(0.5) H02A(0.5) H02C(0.5) H02D(0.5) C02F(0.5) H02E(0.5)
 H02F(0.5) H02G(0.5) C02G(0.5) C02H(0.5) C02I(0.5) H02I(0.5) C02L(0.5)
 C026(0.5) H026(0.5) C02W(0.5) H02W(0.5) C02T(0.5) C025(0.5) H025(0.5)
 C02A(0.5) H02H(0.5) C02U(0.5) H02U(0.5) C02V(0.5) C44(0.5) H44A(0.5) H44B(0.5)
 H44C(0.5) C43(0.5) H43A(0.5) H43B(0.5) H43C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C21(H21A,H21B), C22(H22A,H22B), C24(H24A,H24B), C25(H25A,
 H25B), C35(H35A,H35B), C1(H1A,H1B), C2(H2C,H2D), C3(H3A,H3B), C4(H4A,H4B),
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C13(H13A,H13B), C17(H17A,H17B), C14(H14A,H14B), C12(H12A,H12B),
 C19(H19A,H19B), C15(H15A,H15B), C16(H16A,H16B), C11(H11A,H11B), C27(H27A,H27B),
  C28(H28A,H28B), C20(H20A,H20B), C26(H26A,H26B), C29(H2A,H2B), C33(H01P,H33),
 C36(H36A,H36B), C34(H34A,H34B), C30(H30A,H30B), C32(H32A,H32B), C31(H31A,H31B),
  C37(H37A,H37B), C38(H38A,H38B), C40(H40A,H40B), C39(H39A,H39B), C42(H42A,H42B)
5.b Aromatic/amide H refined with riding coordinates:
 C00M(H00M), C00Q(H00Q), C00V(H00V), C00Z(H00Z), C010(H010), C011(H011),
 C012(H012), C013(H013), C014(H014), C015(H015), C016(H016), C017(H017),
 C019(H019), C01A(H01A), C01C(H01C), C01D(H01D), C01E(H01E), C01F(H01F),
 C01G(H01G), C01H(H01H), C01I(H01I), C01J(H01J), C01L(H01L), C01M(H01M),
 C01T(H01T), C02R(H02R), C028(H028), C01V(H01V), C01Z(H01Z), C021(H021),
 C023(H023), C024(H024), C029(H029), C02B(H02B), C02I(H02I), C026(H026),
 C02W(H02W), C025(H025), C02A(H02H), C02U(H02U), C23(H23), C41(H41)
5.c Fitted hexagon refined as free rotating group:
 C01Q(C01T,C02P,C02K,C02R,C028), C02L(C026,C02W,C02T,C025,C02A)
5.d Idealised Me refined as rotating group:
 C02E(H02A,H02C,H02D), C02F(H02E,H02F,H02G), C44(H44A,H44B,H44C), C43(H43A,
 H43B,H43C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              53071
_shelx_hkl_checksum              5176
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_original_sample_id beta_me-daid_zncl2
_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
- B-factor correction
;