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_1566585
_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, 4.5(C6 H12)'
_chemical_formula_sum            'C63 H78 I6 N12 Zn3'
_chemical_formula_weight         1960.88
_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                 100.6492(14)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.5713(5)
_cell_length_b                   15.1587(3)
_cell_length_c                   29.5198(5)
_cell_measurement_reflns_used    20764
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.5350
_cell_measurement_theta_min      4.3260
_cell_volume                     15203.6(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 2018/3 (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 0.994
_diffrn_measured_fraction_theta_max 0.978
_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  27.00   1.00    7.50    --  -44.67  19.00  90.00   32
  2  \w     -5.00  29.00   1.00    7.50    --  -44.67  19.00   0.00   34
  3  \w     -4.00  29.00   1.00    7.50    --  -44.67  19.00 120.00   33
  4  \w     -3.00  24.00   1.00    7.50    --  -44.67  19.00 150.00   27
  5  \w      4.00  31.00   1.00    7.50    --  -44.67  19.00-120.00   27
  6  \w     -4.00  27.00   1.00    7.50    --  -44.67  19.00  30.00   31
  7  \w     37.00  88.00   1.00    7.50    --   44.67-125.00 120.00   51
  8  \w    103.00 165.00   1.00   30.00    --  104.50  61.00 150.00   62
  9  \w    111.00 144.00   1.00   30.00    --  104.50  77.00   0.00   33
 10  \w    103.00 129.00   1.00   30.00    --  104.50 125.00 -90.00   26
 11  \w    140.00 165.00   1.00   30.00    --  104.50  45.00 120.00   25
 12  \w     36.00  81.00   1.00   30.00    --  104.50 -61.00-150.00   45
 13  \w     69.00 105.00   1.00   30.00    --  104.50-125.00 150.00   36
 14  \w     44.00  89.00   1.00   30.00    --  104.50 -61.00   0.00   45
 15  \w     88.00 126.00   1.00   30.00    --  104.50  45.00 120.00   38
 16  \w    108.00 176.00   1.00   30.00    --  104.50  77.00 -90.00   68
 17  \w    116.00 175.00   1.00   30.00    --  104.50  77.00-180.00   59
 18  \w    123.00 166.00   1.00   30.00    --  104.50  77.00  30.00   43
 19  \w    145.00 173.00   1.00   30.00    --  104.50 125.00 -90.00   28
 20  \w     35.00  61.00   1.00   30.00    --  104.50 -41.00-123.00   26
 21  \w     43.00 107.00   1.00   30.00    --  104.50-125.00 120.00   64
 22  \w     38.00  79.00   1.00   30.00    --  104.50 -61.00 -30.00   41
 23  \w    111.00 136.00   1.00   30.00    --  104.50 -82.00  -9.37   25
 24  \w     76.00 103.00   1.00   30.00    --  104.50 -82.00  -9.37   27
;
_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  0.0752
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            43747
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.919
_diffrn_reflns_theta_min         4.245
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    20.567
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.583
_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    1.713
_exptl_crystal_description       block
_exptl_crystal_F_000             7584
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.122
_refine_diff_density_max         3.214
_refine_diff_density_min         -2.379
_refine_diff_density_rms         0.255
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         15078
_refine_ls_number_restraints     320
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0942
_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^)+(0.1010P)^2^+756.1912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2452
_refine_ls_wR_factor_ref         0.2507
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13117
_reflns_number_total             15078
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5046.cif
_cod_data_source_block           alpha_cyc_zni2
_cod_original_cell_volume        15203.5(4)
_cod_database_code               1566585
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.188
_shelx_estimated_absorpt_t_min   0.078
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
C78 \\sim C76 \\sim C77 \\sim C75 \\sim C74 \\sim C73: 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 0.001 and sigma for terminal atoms of
0.001 within 2A
C12 \\sim C10 \\sim C14: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.02 within 2A
I5 \\sim I5A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.001 within 2A
C67 \\sim C70 \\sim C69 \\sim C71 \\sim C68 \\sim C72: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.02 within 2A
C60 \\sim C61 \\sim C62 \\sim C63 \\sim C59 \\sim C58: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.02 within 2A
C12 \\sim C14 \\sim C10 \\sim C16 \\sim C28 \\sim C22: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C81 \\sim C82 \\sim C83 \\sim C80 \\sim C84 \\sim C79: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.02 within 2A
C \\sim C1 \\sim C2 \\sim C \\sim C1 \\sim C2: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.02 within 2A
C18 \\sim C20 \\sim C21 \\sim C17 \\sim C16: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.02 within 2A
C29 \\sim C30 \\sim C32 \\sim C33 \\sim C28: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.02 within 2A
C45 \\sim C41 \\sim C42 \\sim C44: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.02 within 2A
C40 \\sim C52 \\sim C46: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.02 within 2A
C20 \\sim C21 \\sim C17 \\sim C16 \\sim C18: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C40 \\sim C34: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C77) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C78)
\\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C73) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.02
Uanis(C14) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.01
Uanis(C14) = Uanis(C10) = Uanis(C12) = Uanis(C28)
Uanis(Zn9A) = Uanis(Zn9)
Uanis(N11) = Uanis(N15) = Uanis(N13)
Uanis(N31) = Uanis(N19) = Uanis(N25)
Uanis(N13) = Uanis(N11) = Uanis(N15)
Uanis(N31) = Uanis(N25) = Uanis(N19)
Uanis(C44) = Uanis(C42) = Uanis(C41) = Uanis(C45)
Uanis(N35) = Uanis(N37) = Uanis(N39)
3. Rigid body (RIGU) restrains
 I6A, Zn9A, I5A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 I6, Zn9, I5
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Others
 Sof(I6A)=Sof(Zn9A)=Sof(I5A)=1-FVAR(1)
 Sof(I5)=Sof(I6)=Sof(Zn9)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B), C70(H70A,H70B), C69(H69A,H69B), C71(H71A,H71B), C68(H68A,
 H68B), C62(H62A,H62B), C60(H60A,H60B), C59(H59A,H59B), C76(H76A,H76B),
 C82(H82A,H82B), C67(H67A,H67B), C81(H81A,H81B), C72(H72A,H72B), C83(H83A,H83B),
  C58(H58A,H58B), C63(H63A,H63B), C74(H74A,H74B), C80(H80A,H80B), C73(H73A,
 H73B), C78(H78A,H78B), C77(H77A,H77B), C84(H84A,H84B), C75(H75A,H75B),
 C79(H79A,H79B), C(HA,HB), C1(H1A,H1B), C2(H2A,H2B)
5.b Aromatic/amide H refined with riding coordinates:
 C33(H33), C32(H32), C30(H30), C29(H29), C21(H21), C23(H23), C24(H24),
 C45(H45), C44(H44), C27(H27), C26(H26), C56(H56), C20(H20), C51(H51), C54(H54),
  C53(H53), C50(H50), C41(H41), C47(H47), C57(H57), C48(H48), C42(H42),
 C17(H17), C18(H18)
;
_shelx_res_checksum              48946
_shelx_hkl_checksum              56324
_olex2_date_sample_data_collection 2020-10-06
_olex2_date_sample_submission    2020-09-01
_olex2_submission_original_sample_id alpha_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
- B-factor correction
;