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_1566584
_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, C17 H14 O4, 0.333(C6 H12)'
_chemical_formula_sum            'C55 H42 I6 N12 O4 Zn3'
_chemical_formula_weight         1892.51
_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                 101.958(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.4862(8)
_cell_length_b                   15.0052(4)
_cell_length_c                   31.1250(7)
_cell_measurement_reflns_used    14653
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      74.3690
_cell_measurement_theta_min      3.7370
_cell_volume                     15756.8(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.84a (Rigaku OD, 2020)'
_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)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_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    -98.00  -6.00   1.00   30.00    --  -44.67 125.00 -60.00   92
  2  \w     -4.00  31.00   1.00   30.00    --  -44.67  19.00 -90.00   35
  3  \w     -4.00  31.00   1.00   30.00    --  -44.67  19.00 120.00   35
  4  \w    -21.00  26.00   1.00   30.00    --  -44.67  38.00  60.00   47
  5  \w     19.00 113.00   1.00   30.00    --   44.67  62.00 -37.19   94
  6  \w     36.00  68.00   1.00   90.00    --  104.50 -45.00  30.00   32
  7  \w    105.00 166.00   1.00   90.00    --  104.50  77.00 120.00   61
  8  \w    125.00 165.00   1.00   90.00    --  104.50  45.00-150.00   40
  9  \w    112.00 170.00   1.00   90.00    --  104.50  77.00  60.00   58
 10  \w     62.00 107.00   1.00   90.00    --  104.50-100.00 -16.73   45
 11  \w     39.00  76.00   1.00   90.00    --  104.50 -94.00  60.00   37
 12  \w     30.00 107.00   1.00   90.00    --  104.50-104.00 -76.41   77
 13  \w     79.00 121.00   1.00   90.00    --  104.50-136.00 134.00   42
 14  \w     77.00 173.00   1.00   90.00    --  104.50  69.00 178.28   96
 15  \w     86.00 112.00   1.00   90.00    --  104.50-125.00 -90.00   26
 16  \w     40.00  66.00   1.00   90.00    --  104.50 -61.00   0.00   26
 17  \w     37.00  85.00   1.00   90.00    --  104.50 -61.00-180.00   48
;
_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_unetI/netI     0.0833
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            35855
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        56.650
_diffrn_reflns_theta_max         75.309
_diffrn_reflns_theta_min         3.750
_exptl_absorpt_coefficient_mu    15.035
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.84a (Rigaku Oxford Diffraction, 2020)
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    1.596
_exptl_crystal_description       block
_exptl_crystal_F_000             7168
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.485
_refine_diff_density_min         -2.558
_refine_diff_density_rms         0.285
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     813
_refine_ls_number_reflns         35855
_refine_ls_number_restraints     323
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.1783
_refine_ls_R_factor_gt           0.1233
_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^)+(0.2179P)^2^+29.5800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3944
_refine_ls_wR_factor_ref         0.4217
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16702
_reflns_number_total             35855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5046.cif
_cod_data_source_block           beta_me-daid_zni2
_cod_database_code               1566584
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.419
_shelx_estimated_absorpt_t_min   0.162
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7075(16)
 0.2925(16)
2. 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
3. Restrained distances
 C2-C3 = C2-C7 = C3-C4 = C4-C5 = C5-C6 = C6-C7
 1.54 with sigma of 0.02
 C2-C4 = C2-C6 = C3-C5 = C4-C6 = C5-C7
 2.54 with sigma of 0.04
 C2-C3 \\sim C3-C4 \\sim C4-C5 \\sim C5-C6 \\sim C6-C7 \\sim C7-C2
 with sigma of 0.02
 C2-C6 \\sim C4-C6 \\sim C3-C7 \\sim C3-C5 \\sim C5-C7 \\sim C2-C4
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
C15 \\sim C016 \\sim C029 \\sim C01X: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.001 within 2A
Zn08 \\sim Zn1: within 2A with sigma of 0.0001 and sigma for terminal atoms of
0.0001 within 2A
C020 \\sim C01K \\sim C019 \\sim C01E \\sim C01O \\sim C02A: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.02 within 2A
I06A \\sim I06: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.001 within 2A
I0 \\sim I003: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.001 within 2A
Zn09 \\sim Zn: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.001 within 2A
C2 \\sim C3 \\sim C7 \\sim C4 \\sim C6 \\sim C5: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.001 within 2A
C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
I05 \\sim I05A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.001 within 2A
I004 \\sim I1: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.001 within 2A
C01T \\sim C01Y \\sim C01P \\sim C01R \\sim C01A \\sim C00Z: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C15 \\sim C029 \\sim C00X \\sim C01X \\sim C016: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
Uanis(C02B) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O00O) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(C029) \\sim Ueq, Uanis(C021) \\sim Ueq, Uanis(C023)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O00W) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 I1, Zn1, I05A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 I004, Zn08, I05
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 I06A, Zn, I0
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 I06, Zn09, I003
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2, C3, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(I06A)=Sof(Zn)=Sof(I0)=1-FVAR(1)
 Sof(I003)=Sof(I06)=Sof(Zn09)=FVAR(1)
 Sof(I1)=Sof(Zn1)=Sof(I05A)=1-FVAR(2)
 Sof(I004)=Sof(I05)=Sof(Zn08)=FVAR(2)
 Fixed Sof: C2(0.33333) H2A(0.33333) H2B(0.33333) C3(0.33333) H3A(0.33333)
 H3B(0.33333) C4(0.33333) H4A(0.33333) H4B(0.33333) C5(0.33333) H5A(0.33333)
 H5B(0.33333) C6(0.33333) H6A(0.33333) H6B(0.33333) C7(0.33333) H7A(0.33333)
 H7B(0.33333)
 Fixed X: Zn1(0.568721)
 Fixed Y: Zn1(0.888301)
 Fixed Z: Zn1(0.617041)
7.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B)
7.b Aromatic/amide H refined with riding coordinates:
 C00P(H00P), C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011), C012(H012),
 C013(H013), C014(H014), C016(H016), C017(H017), C01D(H01D), C01E(H01E),
 C01F(H01F), C01G(H01G), C01H(H01H), C01L(H01L), C01M(H01M), C01P(H01P),
 C01Q(H01Q), C01R(H01R), C01S(H01S), C01T(H01T), C01U(H01U), C01V(H01V),
 C01X(H01X), C020(H020), C021(H021), C022(H022), C023(H023), C029(H029),
 C02A(H02D), C15(H15)
7.c Idealised Me refined as rotating group:
 C028(H02A,H02B,H02C), C02B(H02E,H02F,H02G)
;
_shelx_res_checksum              67151
_shelx_hkl_checksum              77188
_shelx_fab_checksum              52749
_platon_squeeze_special_details
;
A solvent mask was calculated and 760 electrons were 
found in a volume of 3114\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1[C6H12], 1[C6H12] per Asymmetric Unit 
which account for 768 electrons 
per unit cell. C6H12 was the solvent for crystallisation.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_original_sample_id beta_me-daid_zni2
_olex2_submission_special_instructions 'No special instructions were received'