Multivariate sodalite zeolitic imidazolate frameworks: a direct solvent-free synthesis
López-Cabrelles, Javier; Miguel-Casañ, Eugenia; Esteve-Rochina, María; Andres-Garcia, Eduardo; Vitórica-Yrezábal, Iñigo J.; Calbo, Joaquín; Mínguez Espallargas, Guillermo; Chemical Science 13 (2022) 842–847; doi:10.1039/D1SC04779E

data_1565835
_publ_section_title
;
 Multivariate sodalite zeolitic imidazolate frameworks: a direct
 solvent-free synthesis
;
_journal_issue                   3
_journal_name_full               'Chemical Science'
_journal_page_first              842
_journal_page_last               847
_journal_paper_doi               10.1039/D1SC04779E
_journal_volume                  13
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C10 H11 Fe N4'
_chemical_formula_sum            'C10 H11 Fe N4'
_chemical_formula_weight         243.08
_space_group_crystal_system      cubic
_space_group_IT_number           217
_space_group_name_Hall           'I -4 2 3'
_space_group_name_H-M_alt        'I -4 3 m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-08 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   17.1728(6)
_cell_length_b                   17.1728(6)
_cell_length_c                   17.1728(6)
_cell_measurement_reflns_used    1902
_cell_measurement_temperature    119.5(8)
_cell_measurement_theta_max      16.8580
_cell_measurement_theta_min      3.3440
_cell_volume                     5064.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.5(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -42.00  15.00   1.00   30.00    --  -14.89 -77.00  30.00   57
  2  \w    -41.00  15.00   1.00   30.00    --  -14.89 -77.00 -60.00   56
  3  \w    -88.00  56.00   1.00   30.00    --  -14.89   0.00-120.00  144
  4  \w    -74.00 -35.00   1.00   30.00    --  -14.89 127.00-153.39   39
  5  \w    -40.00  58.00   1.00   30.00    --  -14.89  38.00 -60.00   98
  6  \w     -6.00  85.00   1.00   30.00    --   15.83  57.00-180.00   91
  7  \w     -4.00  85.00   1.00   30.00    --   15.83  57.00 -90.00   89
  8  \w    -27.00  46.00   1.00   30.00    --   15.83 -77.00  30.00   73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0403714000
_diffrn_orient_matrix_UB_12      0.0023788000
_diffrn_orient_matrix_UB_13      0.0084555000
_diffrn_orient_matrix_UB_21      0.0067567000
_diffrn_orient_matrix_UB_22      -0.0168148000
_diffrn_orient_matrix_UB_23      0.0371694000
_diffrn_orient_matrix_UB_31      0.0055937000
_diffrn_orient_matrix_UB_32      0.0375557000
_diffrn_orient_matrix_UB_33      0.0161044000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1646
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29016
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.965
_diffrn_reflns_theta_max         24.965
_diffrn_reflns_theta_min         2.905
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.874
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.956
_exptl_crystal_description       cube
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.12(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         863
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0623P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1187
_reflns_Friedel_coverage         0.805
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                637
_reflns_number_total             863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04779e2.cif
_cod_data_source_block           sx899b
_cod_depositor_comments
'Adding full bibliography for 1565835--1565836.cif.'
_cod_original_cell_volume        5064.3(6)
_cod_database_code               1565835
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.873
_shelx_estimated_absorpt_t_min   0.866
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.88(8)
 0.12(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C3-C5 = C6-C5
 1.39 with sigma of 0.002
 C6_$2-C6_$3
 1.39 with sigma of 0.02
4. Restrained planarity
 C3, C3_$1, C5_$1, C6_$1, C6, C5
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
C5 \\sim C6: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
6. Rigid body (RIGU) restrains
 C4, C2, N1, C3, C5, C6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
7. Others
 Fixed Sof: H3(0.75) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) C6(0.25) H6(0.25)
 C5(0.25) H5(0.25)
8.a Riding coordinates:
 C6(H6)
8.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5)
8.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 474 electrons were 
found in a volume of 1804\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
4[H2O] per Asymmetric Unit 
which account for 480 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              90271
_shelx_hkl_checksum              89517
_shelx_fab_checksum              69401
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.112
_oxdiff_exptl_absorpt_empirical_full_min 0.943