Co-existence of five- and six-coordinate iron(ii) species captured in a geometrically strained spin-crossover Hofmann framework
Xu, Luonan; Xie, Zixi; Zenere, Katrina A.; Clegg, Jack K.; Kenny, Elise; Rijs, Nicole J.; Jameson, Guy N. L.; Kepert, Cameron J.; Powell, Benjamin J.; Neville, Suzanne M.; Dalton Transactions  (2022) –; doi:10.1039/D2DT01371A

data_7710441
_publ_section_title
;
 Co-existence of five- and six-coordinate iron(ii) species captured in a
 geometrically strained spin-crossover Hofmann framework
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01371A
_journal_year                    2022
_chemical_formula_moiety         'C42 H26 Fe3 N18 O2 Pt3, C2 H6 O'
_chemical_formula_sum            'C44 H32 Fe3 N18 O3 Pt3'
_chemical_formula_weight         1613.69
_chemical_name_systematic        1_250
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-05-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2022-05-31 deposited with the CCDC.	2022-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                96.57(3)
_cell_angle_beta                 102.935(16)
_cell_angle_gamma                103.22(3)
_cell_formula_units_Z            1
_cell_length_a                   7.398(4)
_cell_length_b                   13.352(9)
_cell_length_c                   14.812(7)
_cell_measurement_reflns_used    6270
_cell_measurement_temperature    250.0
_cell_measurement_theta_max      26.44
_cell_measurement_theta_min      2.32
_cell_volume                     1366.9(14)
_computing_cell_refinement       'APEX 3'
_computing_data_collection       'APEX 3'
_computing_data_reduction        'APEX 3'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      250.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            48661
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.446
_diffrn_reflns_theta_min         2.866
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.476
_exptl_absorpt_correction_T_max  0.175
_exptl_absorpt_correction_T_min  0.280
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS - Bruker- v2018.1.0'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.961
_exptl_crystal_description       block
_exptl_crystal_F_000             758
_exptl_crystal_preparation       'vial-in-vail slow diffusion'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   0.280
_exptl_transmission_factor_min   0.175
_refine_diff_density_max         2.435
_refine_diff_density_min         -1.472
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         5597
_refine_ls_number_restraints     251
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0391P)^2^+3.5074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4885
_reflns_number_total             5597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01371a2.cif
_cod_data_source_block           1_250
_cod_original_cell_volume        1366.7(14)
_cod_database_code               7710441
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.363
_shelx_estimated_absorpt_t_min   0.141
_exptl_absorpt_special_details
;
 Rint before absorption correction = 0.1806
 Rint after absorption correction = 0.0910
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Others
 Fixed Sof: O2(0.5) H2(0.5) C22(0.5) H22A(0.5) H22B(0.5) C23(0.5) H23A(0.5)
 H23B(0.5) H23C(0.5)
4.a Rotating group:
 O1(H1A,H1B)
4.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B)
4.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C7(H7), C8(H8), C10(H10), C18(H18), C19(H19), C15(H15), C21(H21),
 C20(H20), C14(H14), C13(H13)
4.d Tetrahedral OH refined with riding coordinates:
 O2(H2)
4.e Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C)
;
_shelx_res_checksum              95560
_olex2_submission_original_sample_id 1_250
_olex2_submission_special_instructions 'No special instructions were received'