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_1566581
_publ_section_title
;
 The benefits of Cu K\b radiation for the single-crystal X-ray structure
 determination of crystalline sponges
;
_journal_coeditor_code           LT5046
_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, C17 H14 O4, 2.037(C6 H12), 0.333(C6 H9), 0.189(C6 H6)'
_chemical_formula_sum            'C68.39 H67.65 Cl6 N12 O4 Zn3'
_chemical_formula_weight         1530.54
_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             2021-06-23
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.06.18 svn.r64d69d6c for OlexSys, GUI svn.r6354)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.245(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.3132(5)
_cell_length_b                   14.4948(2)
_cell_length_c                   31.7714(5)
_cell_measurement_reflns_used    15980
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.8060
_cell_measurement_theta_min      3.4790
_cell_volume                     14992.4(4)
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_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     -5.00  34.00   1.00   20.00    --  -43.14  19.00 -30.00   39
  2  \w    -44.00  27.00   1.00   20.00    --  -43.14  57.00   0.00   71
  3  \w     -5.00  34.00   1.00   20.00    --  -43.14  19.00 -90.00   39
  4  \w     -5.00  34.00   1.00   20.00    --  -43.14  19.00 120.00   39
  5  \w    -44.00  27.00   1.00   20.00    --  -43.14  57.00  60.00   71
  6  \w     -5.00  34.00   1.00   20.00    --  -43.14  19.00-150.00   39
  7  \w     31.00  57.00   1.00   80.00    --  104.50 -30.00  60.00   26
  8  \w    103.00 178.00   1.00   80.00    --  104.50  77.00  60.00   75
  9  \w     34.00  72.00   1.00   80.00    --  104.50 -45.00  30.00   38
 10  \w     31.00  57.00   1.00   80.00    --  104.50 -30.00  90.00   26
 11  \w     35.00  93.00   1.00   80.00    --  104.50 -61.00   0.00   58
 12  \w     22.00 106.00   1.00   80.00    --  104.50 -95.00 -30.00   84
 13  \w     34.00  72.00   1.00   80.00    --  104.50 -45.00-150.00   38
 14  \w     30.00 127.00   1.00   80.00    --  104.50 -77.00   0.00   97
 15  \w     80.00 175.00   1.00   80.00    --  104.50  45.00   0.00   95
 16  \w     31.00  57.00   1.00   80.00    --  104.50 -30.00   0.00   26
 17  \w     31.00  57.00   1.00   80.00    --  104.50 -30.00-180.00   26
 18  \w     31.00 105.00   1.00   80.00    --  104.50-125.00  60.00   74
 19  \w     39.00  88.00   1.00   80.00    --  104.50 -95.00-180.00   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            47323
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.744
_diffrn_reflns_theta_min         2.715
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.511
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_correction_T_min  0.673
_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_density_diffrn    1.356
_exptl_crystal_description       prism
_exptl_crystal_F_000             6288
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.211
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1278
_refine_ls_number_reflns         14931
_refine_ls_number_restraints     284
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0860
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+327.9591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2275
_refine_ls_wR_factor_ref         0.2347
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12241
_reflns_number_total             14931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5046.cif
_cod_data_source_block           alpha_me-daid_zncl2
_cod_database_code               1566581
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.743
_shelx_estimated_absorpt_t_min   0.678
_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. Uiso/Uaniso restraints and constraints
C8 \\sim C21 \\sim C24 \\sim C15 \\sim C20 \\sim C10: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01 within 2A
C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.001 within 2A
Zn \\sim Zn03: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 2A
C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 2A
C37 \\sim C38 \\sim C36 \\sim C39 \\sim C41 \\sim C40: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 2A
C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C32 \\sim C35 \\sim C30 \\sim C34 \\sim C31 \\sim C33: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C01U \\sim C01W \\sim C023 \\sim C01X \\sim C01T \\sim C01Z: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
C01X \\sim C01T \\sim C01Z \\sim C01W \\sim C01U \\sim C023: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
Uanis(O4) \\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Cl1) = Uanis(Cl08)
Uanis(Cl) = Uanis(Cl09)
Uanis(Zn03) = Uanis(Zn)
3. Rigid body (RIGU) restrains
 Cl, Zn, Cl1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl09, Zn03, Cl08
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Sof(Zn)=Sof(Cl)=Sof(Cl1)=1-FVAR(1)
 Sof(Zn03)=Sof(Cl08)=Sof(Cl09)=FVAR(1)
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C27)=Sof(H27A)=
 Sof(H27B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C22)=
 Sof(H22A)=Sof(H22B)=FVAR(2)
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=
 Sof(H41B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C39)=
 Sof(H39A)=Sof(H39B)=FVAR(3)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C30)=Sof(H30A)=
 Sof(H30B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C32)=
 Sof(H32A)=Sof(H32B)=FVAR(4)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C9)=Sof(H9A)=Sof(H9B)=
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C19)=Sof(H19A)=
 Sof(H19B)=FVAR(5)
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C43)=Sof(H43A)=
 Sof(H43B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C47)=
 Sof(H47A)=Sof(H47B)=FVAR(6)
 Sof(C59)=Sof(H59)=Sof(C58)=Sof(H58)=Sof(C60)=Sof(C56)=Sof(H56A)=Sof(H56B)=
 Sof(C57)=Sof(H57)=Sof(C55)=Sof(H55)=FVAR(7)
 Fixed Sof: O1(0.5) O5(0.5) O(0.5) O2(0.5) C01T(0.5) C01U(0.5) C01V(0.5)
 H01V(0.5) C01W(0.5) C01X(0.5) H01X(0.5) C01Z(0.5) H01Z(0.5) C022(0.5)
 C023(0.5) H023(0.5) C024(0.5) H024(0.5) C025(0.5) H025(0.5) C026(0.5)
 C027(0.5) C029(0.5) H029(0.5) C02B(0.5) H02B(0.5) C02E(0.5) C02G(0.5)
 H02A(0.5) H02C(0.5) H02D(0.5) C02J(0.5) H02E(0.5) H02F(0.5) H02G(0.5) O3(0.5)
 O6(0.5) C3(0.5) C4(0.5) H4(0.5) C5(0.5) C6(0.5) O4(0.5) O7(0.5) C11(0.5)
 H11(0.5) C14(0.5) C16(0.5) H16(0.5) C17(0.5) C18(0.5) H18(0.5) C20(0.5)
 C15(0.5) H15(0.5) C24(0.5) H24(0.5) C21(0.5) C8(0.5) H8(0.5) C10(0.5) H10(0.5)
 C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5) C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5)
 C53(0.33333) H53(0.33333) C54(0.33333) H54(0.33333) C52(0.33333) H52(0.33333)
 C50(0.33333) H50A(0.33333) H50B(0.33333) C49(0.33333) H49A(0.33333)
 H49B(0.33333) C51(0.33333) H51A(0.33333) H51B(0.33333)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C7(H7A,H7B), C9(H9A,H9B), C12(H12A,H12B), C13(H13A,H13B),
 C19(H19A,H19B), C23(H23A,H23B), C29(H29A,H29B), C35(H35A,H35B), C33(H33A,H33B),
  C27(H27A,H27B), C30(H30A,H30B), C34(H34A,H34B), C31(H31A,H31B), C25(H25A,
 H25B), C28(H28A,H28B), C22(H22A,H22B), C32(H32A,H32B), C37(H37A,H37B),
 C40(H40A,H40B), C41(H41A,H41B), C38(H38A,H38B), C36(H36A,H36B), C39(H39A,H39B),
  C45(H45A,H45B), C44(H44A,H44B), C43(H43A,H43B), C46(H46A,H46B), C48(H48A,
 H48B), C47(H47A,H47B), C50(H50A,H50B), C49(H49A,H49B), C51(H51A,H51B),
 C56(H56A,H56B)
5.b Aromatic/amide H refined with riding coordinates:
 C00N(H00N), C00P(H00P), C00S(H00S), C00W(H00W), C00X(H00X), C00Y(H00Y),
 C010(H010), C011(H011), C013(H013), C016(H016), C017(H017), C018(H018),
 C019(H019), C01B(H01B), C01C(H01C), C01D(H01D), C1(H1), C01F(H01F), C01G(H01G),
  C01H(H01H), C01I(H01I), C01J(H01J), C01L(H01L), C01N(H01N), C01V(H01V),
 C01X(H01X), C01Z(H01Z), C023(H023), C024(H024), C025(H025), C029(H029),
 C02B(H02B), C4(H4), C11(H11), C16(H16), C18(H18), C15(H15), C24(H24), C8(H8),
 C10(H10), C53(H53), C54(H54), C52(H52), C59(H59), C58(H58), C57(H57), C55(H55)
5.c Fitted hexagon refined as free rotating group:
 C20(C15,C24,C21,C8,C10)
5.d Idealised Me refined as rotating group:
 C02G(H02A,H02C,H02D), C02J(H02E,H02F,H02G), C26(H26A,H26B,H26C), C42(H42A,
 H42B,H42C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              95661
_shelx_hkl_checksum              94559
_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
;