Expanding the dimensionality of bis(tetrazolyl)alkane-based Fe(II) coordination polymers by the application of dinitrile coligands.
Tołoczko, Aleksandra; Kaźmierczak, Marcin; Książek, Maria; Weselski, Marek; Siczek, Miłosz; Kusz, Joachim; Bronisz, Robert; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7163–7174; doi:10.1039/d4dt00462k

data_7715499
_publ_section_title
;
 Expanding the dimensionality of bis(tetrazolyl)alkane-based Fe(II)
 coordination polymers by the application of dinitrile coligands.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7163
_journal_page_last               7174
_journal_paper_doi               10.1039/d4dt00462k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C64 H80 Fe4 N80, 4(C5 H6 N2), 8(B F4)'
_chemical_formula_sum            'C84 H104 B8 F32 Fe4 N88'
_chemical_formula_weight         3264.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-02-13 deposited with the CCDC.	2024-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.0460(10)
_cell_angle_beta                 104.760(2)
_cell_angle_gamma                103.591(2)
_cell_formula_units_Z            2
_cell_length_a                   18.9389(4)
_cell_length_b                   19.4264(3)
_cell_length_c                   19.5685(3)
_cell_measurement_reflns_used    24498
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      34.3010
_cell_measurement_theta_min      1.8560
_cell_volume                     6752.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2018)'
_diffrn_ambient_temperature      80(2)
_diffrn_detector_area_resol_mean 10.0000
_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     15.00  40.00   0.50   15.00    --    0.06  36.00 -46.54   50
  2  \w     15.00  40.00   0.50   15.00    --    0.06  35.00  61.28   50
  3  \w    -48.00  19.00   0.50   15.00    --   -8.00 -14.00 106.32  134
  4  \w    -51.00 -26.00   0.50   15.00    --  -16.00 145.00-159.19   50
  5  \w    -50.00 -25.00   0.50   15.00    --  -16.00 143.00 -27.96   50
  6  \w    -36.00  -9.00   0.50   15.00    --  -20.00 116.00  46.95   54
  7  \w    -41.00 -15.00   0.50   15.00    --  -20.00 123.00 -86.90   52
  8  \w    -40.00 -14.00   0.50   15.00    --  -20.00 121.00 -49.86   52
  9  \w    -19.00   7.00   0.50   15.00    --  -32.00  32.00 -67.73   52
 10  \w    -17.00  10.00   0.50   15.00    --  -32.00  36.00 -30.38   54
 11  \w     -4.00  23.00   0.50   15.00    --   36.00 -33.00-131.34   54
 12  \w     -6.00  22.00   0.50   15.00    --   36.00 -34.00  27.86   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            27531
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.768
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.620
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
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_density_diffrn    1.605
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.048
_refine_diff_density_max         1.318
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2173
_refine_ls_number_reflns         27531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0687
_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^)+(0.0574P)^2^+29.0637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1691
_refine_ls_wR_factor_ref         0.1815
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20692
_reflns_number_total             27531
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00462k2.cif
_cod_data_source_block           3_1_99a2mo_1_80_00
_cod_depositor_comments
'Adding full bibliography for 7715495--7715502.cif.'
_cod_database_code               7715499
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.913
_shelx_estimated_absorpt_t_max   0.974
_shelx_res_checksum              55193