An iron(ii) coordination polymer of a triazolyl tris-heterocycle showing a spin state conversion triggered by loss of lattice solvent
Galadzhun, Iurii; Capel Berdiell, Izar; Shahid, Namrah; Halcrow, Malcolm A.; CrystEngComm 21 (2019) 6330–; doi:10.1039/C9CE01496A

data_7234535
_publ_section_title
;
 An iron(ii) coordination polymer of a triazolyl tris-heterocycle showing
 a spin state conversion triggered by loss of lattice solvent
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              6330
_journal_paper_doi               10.1039/C9CE01496A
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety
'C40 H36 Fe2 N24 O2, 4(B F4), 0.66(H2 O), C H3 N O2'
_chemical_formula_sum            'C41 H40.32 B4 F16 Fe2 N25 O4.66'
_chemical_formula_weight         1416.80
_chemical_name_systematic
;
catena-Bis-[/m-{2-(pyrazol-1-yl)-6-(1,2,4-triazol-1-yl)pyridine}]-
bis [2-(pyrazol-1-yl)-6-(1,2,4-triazol-1-yl)pyridine]diaqua-di-iron(II)
tetrakis-tetrafluoroborate hydrate (2/0.66) nitromethane solvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-07-03
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_audit_update_record
;
2019-09-04 deposited with the CCDC.    2019-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.397(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.9010(5)
_cell_length_b                   15.9683(4)
_cell_length_c                   18.7282(6)
_cell_measurement_reflns_used    7325
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      73.40
_cell_measurement_theta_min      4.43
_cell_volume                     5871.7(3)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      290(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19128
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.87
_diffrn_reflns_theta_min         4.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.013
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2858
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         5822
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0834
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1571P)^2^+6.4738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2363
_refine_ls_wR_factor_ref         0.2454
_reflns_number_gt                5051
_reflns_number_total             5822
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9ce01496a2.cif
_cod_data_source_block           ig12c4rt
_cod_depositor_comments
'Adding full bibliography for 7234530--7234535.cif.'
_cod_database_code               7234535
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 B36-F37A = B36-F38A = B36-F39A = B36-F40A
 1.37971 with sigma of 0.02
 B36-F37B = B36-F38B = B36-F39B = B36-F40B
 1.37971 with sigma of 0.02
 B36-F37C = B36-F38C = B36-F39C = B36-F40C
 1.37971 with sigma of 0.02
 F37A-F38A = F37A-F39A = F37A-F40A = F38A-F39A = F38A-F40A = F39A-F40A
 2.253066 with sigma of 0.02
 F37B-F38B = F37B-F39B = F37B-F40B = F38B-F39B = F38B-F40B = F39B-F40B
 2.253066 with sigma of 0.02
 F37C-F38C = F37C-F39C = F37C-F40C = F38C-F39C = F38C-F40C = F39C-F40C
 2.253066 with sigma of 0.02
 B41-F42A = B41-F43A = B41-F44A = B41-F45A
 1.37971 with sigma of 0.02
 B41-F42B = B41-F43B = B41-F44B = B41-F45B
 1.37971 with sigma of 0.02
 B41-F42C = B41-F43C = B41-F44C = B41-F45C
 1.37971 with sigma of 0.02
 F42A-F43A = F42A-F44A = F42A-F45A = F43A-F44A = F43A-F45A = F44A-F45A
 2.253066 with sigma of 0.02
 F42B-F43B = F42B-F44B = F42B-F45B = F43B-F44B = F43B-F45B = F44B-F45B
 2.253066 with sigma of 0.02
 F42C-F43C = F42C-F44C = F42C-F45C = F43C-F44C = F43C-F45C = F44C-F45C
 2.253066 with sigma of 0.02
 O35-H35A = O35-H35B
 0.9 with sigma of 0.02
 H35A-H35B
 1.37 with sigma of 0.02
 C47A-N48 = C47B-N48
 1.45 with sigma of 0.02
 N48-O49A = N48-O50A = N48-O49B = N48-O50B
 1.22 with sigma of 0.02
 O49A-O50A = O49B-O50B
 2.09 with sigma of 0.02
 C47A-O49A = C47A-O50A = C47B-O49B = C47B-O50B
 2.3 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: N3A(0.51) C4A(0.51) C5A(0.51) H5A(0.51) C6A(0.51) H6A(0.51)
 C7A(0.51) H7A(0.51) C8A(0.51) N9A(0.51) N10A(0.51) C11A(0.51) H11A(0.51)
 C12A(0.51) H12A(0.51) C13A(0.51) H13A(0.51) N3B(0.49) C4B(0.49) C5B(0.49)
 H5B(0.49) C6B(0.49) H6B(0.49) C7B(0.49) H7B(0.49) C8B(0.49) N9B(0.49)
 N10B(0.49) C11B(0.49) H11B(0.49) C12B(0.49) H12B(0.49) C13B(0.49) H13B(0.49)
 F37A(0.34) F38A(0.34) F39A(0.34) F40A(0.34) F37B(0.33) F38B(0.33) F39B(0.33)
 F40B(0.33) F37C(0.33) F38C(0.33) F39C(0.33) F40C(0.33) F42A(0.34) F43A(0.34)
 F44A(0.34) F45A(0.34) F42B(0.33) F43B(0.33) F44B(0.33) F45B(0.33) F42C(0.33)
 F43C(0.33) F44C(0.33) F45C(0.33) O46(0.33) C47A(0.3) H47A(0.3) H47B(0.3)
 H47C(0.3) O49A(0.3) O50A(0.3) C47B(0.2) H47D(0.2) H47E(0.2) H47F(0.2)
 O49B(0.2) O50B(0.2)
4.a Me refined with riding coordinates:
 C47A(H47A,H47B,H47C)
4.b Aromatic/amide H refined with riding coordinates:
 C5A(H5A), C6A(H6A), C7A(H7A), C11A(H11A), C12A(H12A), C13A(H13A), C5B(H5B),
 C6B(H6B), C7B(H7B), C11B(H11B), C12B(H12B), C13B(H13B), C16(H16), C18(H18),
 C21(H21), C22(H22), C23(H23), C27(H27), C28(H28), C29(H29), C32(H32), C34(H34)
4.c Idealised Me refined as rotating group:
 C47B(H47D,H47E,H47F)
;