2D/3D spin crossover porous coordination polymers based on isomeric tetrapyridyl benzene ligands
Wu, Wei-Wei; Ruan, Ze-Yu; Shi, Chen-Guang; Mai, Jin-Tao; Cui, Wen; Ni, Zhao-Ping; Wu, Si-Guo; Tong, Ming-Liang; CrystEngComm  (2022) –; doi:10.1039/D2CE00445C

data_7244779
_publ_section_title
;
 2D/3D spin crossover porous coordination polymers based on isomeric
 tetrapyridyl benzene ligands
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00445C
_journal_year                    2022
_chemical_formula_moiety         'C28 H24 B20 Fe N6'
_chemical_formula_sum            'C39 H34 B30 Fe N6 S'
_chemical_formula_weight         696.25
_space_group_crystal_system      orthorhombic
_space_group_IT_number           65
_space_group_name_Hall           '-C 2 2'
_space_group_name_H-M_alt        'C m m m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-14
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2022-04-14 deposited with the CCDC.	2022-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.4250(3)
_cell_length_b                   16.2282(4)
_cell_length_c                   9.68021(19)
_cell_measurement_reflns_used    2587
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      73.5880
_cell_measurement_theta_min      4.4530
_cell_volume                     1951.87(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_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   -114.00 -17.00   1.00    5.00    --  -41.14 -38.00  60.00   97
  2  \w    -73.00 -21.00   1.00    5.00    --  -41.14  77.00 -30.00   52
  3  \w    -13.00  27.00   1.00    5.00    --  -41.14  77.00 -30.00   40
  4  \w     65.00  95.00   1.00    5.00    --   41.14-125.00  90.00   30
  5  \w    115.00 154.00   1.00   30.00    --  107.17 125.00  90.00   39
  6  \w     34.00  85.00   1.00   30.00    --  107.17-125.00-150.00   51
  7  \w     79.00 176.00   1.00   30.00    --  107.17  61.00   0.00   97
  8  \w     25.00  97.00   1.00   30.00    --  107.17 -94.00 -90.00   72
  9  \w    102.00 155.00   1.00   30.00    --  107.17  30.00-150.00   53
 10  \w     59.00 156.00   1.00   30.00    --  107.17 -15.00   0.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0665620000
_diffrn_orient_matrix_UB_12      -0.0657386000
_diffrn_orient_matrix_UB_13      -0.0768095000
_diffrn_orient_matrix_UB_21      -0.0633506000
_diffrn_orient_matrix_UB_22      -0.0685233000
_diffrn_orient_matrix_UB_23      0.0743408000
_diffrn_orient_matrix_UB_31      -0.0832132000
_diffrn_orient_matrix_UB_32      -0.0004092000
_diffrn_orient_matrix_UB_33      -0.1178775000
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3714
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.729
_diffrn_reflns_theta_min         4.482
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.855
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
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    1.185
_exptl_crystal_description       block
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.235
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1116
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.238
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0580
_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^)+(0.1015P)^2^+1.7494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1721
_refine_ls_wR_factor_ref         0.1726
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1099
_reflns_number_total             1116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00445c2.cif
_cod_data_source_block           4_tpbs_298K
_cod_original_cell_volume        1951.87(7)
_cod_database_code               7244779
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N B Fe'
_chemical_oxdiff_usercomment     WWW
_shelx_estimated_absorpt_t_max   0.614
_shelx_estimated_absorpt_t_min   0.484
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All B(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(B1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: C6(0.5) H6(0.5) C5(0.5) H5(0.5) C3(0.5) H3(0.5) H1A(0.25)
 H1C(0.25) H1B(0.25) C2(0.5) H2(0.5)
4.a Riding coordinates:
 B1(H1A,H1C,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C6(H6), C5(H5), C3(H3), C2(H2)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              76963
_shelx_hkl_checksum              86391
_shelx_fab_checksum              96543
_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 2.024
_oxdiff_exptl_absorpt_empirical_full_min 0.683