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_7244781
_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 H18 B2 Fe N6, 2(O)'
_chemical_formula_sum            'C28 H28 B2 Fe N6 O2'
_chemical_formula_weight         558.03
_space_group_crystal_system      orthorhombic
_space_group_IT_number           22
_space_group_name_Hall           'F 2 2'
_space_group_name_H-M_alt        'F 2 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-11
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2022-04-13 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            4
_cell_length_a                   11.012(4)
_cell_length_b                   15.769(5)
_cell_length_c                   18.997(6)
_cell_measurement_reflns_used    6056
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      28.078
_cell_measurement_theta_min      2.498
_cell_volume                     3298.8(19)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      250(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10327
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.189
_diffrn_reflns_theta_min         4.428
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.488
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6323
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0762 before and 0.0526 after correction.
The Ratio of minimum to maximum transmission is 0.8479.
The \l/2 correction factor is Not present.
;
_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    1.124
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.144
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.32(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         2001
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0765P)^2^+1.3187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1061
_reflns_Friedel_coverage         0.796
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                1920
_reflns_number_total             2001
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00445c2.cif
_cod_data_source_block           3_tpb_250K
_cod_original_cell_volume        3298.7(19)
_cod_database_code               7244781
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.906
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.68(3)
 0.32(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(B1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: O2(0.25) O1(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C2(H2), C8(H8)
;
_shelx_res_checksum              35013
_shelx_hkl_checksum              5032
_olex2_submission_special_instructions 'No special instructions were received'