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_1573145
_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, C H4 O, C H O'
_chemical_formula_sum            'C38 H29 B Cl Co F10 Fe N15 O7'
_chemical_formula_weight         1158.80
_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             2023-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-12-21 deposited with the CCDC.	2024-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.782(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.867(4)
_cell_length_b                   20.702(6)
_cell_length_c                   15.437(4)
_cell_measurement_reflns_used    9700
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      21.87
_cell_measurement_theta_min      2.39
_cell_volume                     4614(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 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      200.0
_diffrn_measured_fraction_theta_full 0.987
_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  0.1188
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            109592
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.326
_diffrn_reflns_theta_min         2.607
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1015 before and 0.0730 after correction.
The Ratio of minimum to maximum transmission is 0.9206.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2332
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         8253
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0395P)^2^+5.6821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.1103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5597
_reflns_number_total             8253
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05792a3.cif
_cod_data_source_block           1_4MeOH_2H2O_200K
_cod_depositor_comments
'Adding full bibliography for 1573142--1573157.cif.'
_cod_database_code               1573145
_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 C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O5(H5A,H5B)
2.b Ternary CH refined with riding coordinates:
 B1(H1)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C35(H35), C34(H34), C13(H13), C33(H33), C16(H16),
 C36(H36), C3(H3), C11(H11), C8(H8), C9(H9), C10(H10), C5(H5), C6(H6), C4(H4),
 C7(H7)
2.d X=CH2 refined with riding coordinates:
 N14(H14A,H14B), N11(H11A,H11B)
2.e Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C)
2.f Idealised tetrahedral OH refined as rotating group:
 O6(H6A), O7(H7A)
;
_shelx_res_checksum              99778
_shelx_hkl_checksum              79728
_olex2_submission_special_instructions 'No special instructions were received'