Spin state modulation and kinetic control of thermal contraction in a [Fe<sub>2</sub>Co<sub>2</sub>] discrete Prussian blue analogue.
Yadav, Jyoti; Konar, Sanjit; Chemical science 16 (2024) 130–138; doi:10.1039/d4sc05792a

data_1573146
_publ_section_title
;
 Spin state modulation and kinetic control of thermal contraction in a
 [Fe<sub>2</sub>Co<sub>2</sub>] discrete Prussian blue analogue.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              130
_journal_page_last               138
_journal_paper_doi               10.1039/d4sc05792a
_journal_volume                  16
_journal_year                    2024
_chemical_formula_moiety         'C36 H22 B Co F10 Fe N15, Cl O4, H2 O'
_chemical_formula_sum            'C36 H24 B Cl Co F10 Fe N15 O5'
_chemical_formula_weight         1097.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-12-23 deposited with the CCDC.	2024-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.574(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5844(15)
_cell_length_b                   21.947(2)
_cell_length_c                   14.5400(15)
_cell_measurement_reflns_used    4806
_cell_measurement_temperature    140.00
_cell_measurement_theta_max      23.03
_cell_measurement_theta_min      2.36
_cell_volume                     4436.8(8)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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_temperature      140.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1152
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            56196
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.038
_diffrn_reflns_theta_max         25.038
_diffrn_reflns_theta_min         2.364
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1266 before and 0.0675 after correction.
The Ratio of minimum to maximum transmission is 0.9157.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2200
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         7835
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0656P)^2^+7.3444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1555
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5519
_reflns_number_total             7835
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05792a3.cif
_cod_data_source_block           1_2H2O_140K_1C
_cod_depositor_comments
'Adding full bibliography for 1573142--1573157.cif.'
_cod_database_code               1573146
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O5A(0.75) H5AA(0.75) H5AB(0.75) F10B(0.65) F9A(0.25) F6B(0.5)
 F8B(0.65) C30B(0.65) C29A(0.3) C28A(0.35) F6A(0.5) F7B(0.5) C26B(0.5)
 C27B(0.5) F7A(0.5) O5B(0.25) H5BA(0.25) H5BB(0.25) F8A(0.35) C27A(0.5)
 C26A(0.5) F9B(0.75) C28B(0.65) C29B(0.7) C30A(0.35) F10A(0.35)
3.a Free rotating group:
 O5A(H5AA,H5AB), O5B(H5BA,H5BB)
3.b Ternary CH refined with riding coordinates:
 B1(H1)
3.c Aromatic/amide H refined with riding coordinates:
 C34(H34), C3(H3), C8(H8), C7(H7), C24(H24), C33(H33), C36(H36), C6(H6),
 C35(H35), C11(H11), C10(H10), C9(H9), C23(H23), C4(H4), C5(H5), C21(H21),
 C22(H22)
3.d X=CH2 refined with riding coordinates:
 N14(H14A,H14B), N11(H11A,H11B)
;
_shelx_res_checksum              53397
_shelx_hkl_checksum              18724
_olex2_submission_special_instructions 'No special instructions were received'