Thermal hysteresis induced by external pressure in a 3D Hofmann-type SCO-MOF.
Li, Yue; Kong, Qing-Rong; Guo, Ying; Tang, Zheng; Dalton transactions (Cambridge, England : 2003) 50 (2021) 1384–1389; doi:10.1039/d0dt03796f

data_7706197
_publ_section_title
;
 Thermal hysteresis induced by external pressure in a 3D Hofmann-type
 SCO-MOF.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1384
_journal_page_last               1389
_journal_paper_doi               10.1039/d0dt03796f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C16 H10 Br2 Fe N6 Pt, 2(H4 O2)'
_chemical_formula_sum            'C16 H18 Br2 Fe N6 O4 Pt'
_chemical_formula_weight         769.12
_space_group_crystal_system      tetragonal
_space_group_IT_number           83
_space_group_name_Hall           '-P 4'
_space_group_name_H-M_alt        'P 4/m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-13 deposited with the CCDC.	2020-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   7.4386(2)
_cell_length_b                   7.4386(2)
_cell_length_c                   13.733(2)
_cell_measurement_reflns_used    1657
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6890
_cell_measurement_theta_min      4.1260
_cell_volume                     759.88(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.909
_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  10.00   0.50   30.00    --    0.10  47.00 137.00   50
  2  \w    -60.00  28.00   0.50   30.00    --    0.10 -82.00  60.00  176
  3  \w     35.00  60.00   0.50   30.00    --    0.10  38.00  30.00   50
  4  \w     11.00  36.00   0.50   30.00    --    0.10  47.00 137.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0279586000
_diffrn_orient_matrix_UB_12      0.0254012000
_diffrn_orient_matrix_UB_13      0.0474331000
_diffrn_orient_matrix_UB_21      -0.0807963000
_diffrn_orient_matrix_UB_22      0.0492827000
_diffrn_orient_matrix_UB_23      0.0061914000
_diffrn_orient_matrix_UB_31      -0.0421856000
_diffrn_orient_matrix_UB_32      -0.0776083000
_diffrn_orient_matrix_UB_33      0.0194678000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4726
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.818
_diffrn_reflns_theta_min         3.874
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.729
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_description       plate
_exptl_crystal_F_000             362
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         6.245
_refine_diff_density_min         -1.630
_refine_diff_density_rms         0.286
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1043
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.244
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0757
_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^)+(0.1258P)^2^+0.3917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1881
_refine_ls_wR_factor_ref         0.1936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                910
_reflns_number_total             1043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03796f2.cif
_cod_data_source_block           1_293K
_cod_depositor_comments
'Adding full bibliography for 7706197--7706200.cif.'
_cod_original_cell_volume        759.88(13)
_cod_database_code               7706197
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.24
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C6-C3
 1.5 with sigma of 0.02
 Br1-C6
 1.8 with sigma of 0.02
 C4-C6
 2.6 with sigma of 0.02
3. Restrained planarity
 Br1, C6, C3, C2, C4, C5, N1, C1
 with sigma of 0.1
4. Rigid bond restraints
 N1, C5, C4, C3, C2, C1, C6, Br1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(Br1)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Pt1) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(Fe1)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O2) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
6. Others
 Fixed Sof: N1(0.25) C5(0.25) H5(0.25) C4(0.25) H4(0.25) C3(0.25) C2(0.25)
 H2(0.25) C1(0.25) H1(0.25) C6(0.25) H6(0.25) Br1(0.25) O1(0.25) H1A(0.25)
 H1B(0.25) O2(0.25) H2A(0.25) H2B(0.25)
7.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B)
7.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C2(H2), C1(H1), C6(H6)
7.c Fitted hexagon refined as free rotating group:
 N1(C5,C4,C3,C2,C1)
;
_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 2.113
_oxdiff_exptl_absorpt_empirical_full_min 0.568