Solvent-Free Synthesis of ZIFs: A Route toward the Elusive Fe(II) Analogue of ZIF-8.
López-Cabrelles, Javier; Romero, Jorge; Abellán, Gonzalo; Giménez-Marqués, Mónica; Palomino, Miguel; Valencia, Susana; Rey, Fernando; Mínguez Espallargas, Guillermo; Journal of the American Chemical Society 141 (2019) 7173–7180; doi:10.1021/jacs.9b02686

data_4128139
_publ_section_title
;
 Solvent-Free Synthesis of ZIFs: A Route toward the Elusive Fe(II)
 Analogue of ZIF-8.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7173
_journal_page_last               7180
_journal_paper_doi               10.1021/jacs.9b02686
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '0.33(C30 H42 Fe3 N12)'
_chemical_formula_sum            'C10 H14 Fe N4'
_chemical_formula_weight         246.10
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   8.4206(2)
_cell_length_b                   8.4206(2)
_cell_length_c                   13.1696(3)
_cell_measurement_reflns_used    2004
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.6380
_cell_measurement_theta_min      4.1610
_cell_volume                     808.70(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.922
_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    -34.00  45.00   1.00   20.00    --  -15.04  77.00-150.00   79
  2  \w     -5.00  28.00   1.00   20.00    --   15.83  77.00-150.00   33
  3  \w    -11.00  86.00   1.00   20.00    --   15.83  77.00  90.00   97
;
_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      -0.0304430000
_diffrn_orient_matrix_UB_12      0.0016664000
_diffrn_orient_matrix_UB_13      0.0499971000
_diffrn_orient_matrix_UB_21      0.0017777000
_diffrn_orient_matrix_UB_22      0.0833512000
_diffrn_orient_matrix_UB_23      -0.0111172000
_diffrn_orient_matrix_UB_31      -0.0922938000
_diffrn_orient_matrix_UB_32      -0.0502800000
_diffrn_orient_matrix_UB_33      -0.0166876000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3392
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.872
_diffrn_reflns_theta_min         4.170
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.370
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_description       block
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 385 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         1123
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0266
_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^)+(0.0130P)^2^+0.2258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0513
_reflns_Friedel_coverage         0.584
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.795
_reflns_number_gt                1062
_reflns_number_total             1123
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02686_si_003.cif
_cod_data_source_block           MUV-6
_cod_original_cell_volume        808.70(4)
_cod_database_code               4128139
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.887
_shelx_estimated_absorpt_t_min   0.842
_reflns_odcompleteness_completeness 99.15
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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.a Secondary CH2 refined with riding coordinates:
 C008(H00D,H00E)
2.b Aromatic/amide H refined with riding coordinates:
 C004(H004), C006(H006)
2.c Idealised Me refined as rotating group:
 C007(H00A,H00B,H00C)
;
_olex2_date_sample_data_collection 2018-10-29
_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 1.114
_oxdiff_exptl_absorpt_empirical_full_min 0.890