Interplay between spin crossover and proton migration along short strong hydrogen bonds.
Jornet-Mollá, Verónica; Giménez-Saiz, Carlos; Cañadillas-Delgado, Laura; Yufit, Dmitry S.; Howard, Judith A. K.; Romero, Francisco M.; Chemical science 12 (2020) 1038–1053; doi:10.1039/d0sc04918b

data_1559653
_publ_section_title
;
 Interplay between spin crossover and proton migration along short strong
 hydrogen bonds.
;
_journal_issue                   3
_journal_name_full               'Chemical science'
_journal_page_first              1038
_journal_page_last               1053
_journal_paper_doi               10.1039/d0sc04918b
_journal_volume                  12
_journal_year                    2020
_chemical_formula_moiety
'C22 H18 Fe N10 2+, C12 H9 N2 O6 1-, C6 H4 N O3 1-, 5(H2 O)'
_chemical_formula_sum            'C40 H41 Fe N13 O14'
_chemical_formula_weight         983.705
_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
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-10-29 deposited with the CCDC.	2020-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                64.7142(13)
_cell_angle_beta                 71.0809(12)
_cell_angle_gamma                71.0628(12)
_cell_formula_units_Z            4
_cell_length_a                   13.63358(18)
_cell_length_b                   18.8075(2)
_cell_length_c                   19.6686(2)
_cell_measurement_reflns_used    62124
_cell_measurement_temperature    120.00(14)
_cell_measurement_theta_max      27.5760
_cell_measurement_theta_min      2.3050
_cell_volume                     4210.47(10)
_computing_cell_refinement
;
CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)
;
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(14)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.9379
_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    -41.00  52.00   0.75    7.50    --  -17.76  57.00   0.00  124
  2  \w    -20.00  26.50   0.75    7.50    --  -17.76 -99.00-120.00   62
  3  \w    -51.00  54.00   0.75    7.50    --  -17.76  77.00  90.00  140
  4  \w    -13.00  92.00   0.75    7.50    --   18.62  38.00 -90.00  140
  5  \w    -20.00  62.50   0.75    7.50    --   18.62 -99.00-180.00  110
  6  \w    -52.00  41.00   0.75    7.50    --   18.62 -57.00-120.00  124
  7  \w    -14.00  91.00   0.75    7.50    --   18.62  77.00 120.00  140
  8  \w    -14.00  91.00   0.75    7.50    --   18.62  77.00   0.00  140
  9  \w    -20.00  62.50   0.75    7.50    --   18.62 -99.00   0.00  110
 10  \w    -49.00  56.00   0.75    7.50    --  -17.76  38.00-120.00  140
 11  \w    -91.00  14.00   0.75    7.50    --  -17.76 -38.00   0.00  140
 12  \w    -97.00 -35.50   0.75    7.50    --  -17.76-178.00 -90.00   82
 13  \w    -97.00 -35.50   0.75    7.50    --  -17.76-178.00 120.00   82
 14  \w    -20.00  62.50   0.75    7.50    --   18.62 -99.00  60.00  110
 15  \w    -27.00  60.00   0.75    7.50    --   18.62 -93.00-129.00  116
 16  \w    -55.00  50.00   0.75    7.50    --   18.62 -38.00 120.00  140
 17  \w    -91.00  14.00   0.75    7.50    --  -17.76 -38.00 150.00  140
 18  \w   -100.00 -34.00   0.75    7.50    --  -17.76 178.00 150.00   88
 19  \w    -91.00  14.00   0.75    7.50    --  -17.76 -38.00-120.00  140
 20  \w    -56.00  94.00   0.75    7.50    --   18.62   0.00-120.00  200
 21  \w    -56.00  94.00   0.75    7.50    --   18.62   0.00-150.00  200
 22  \w    -56.00  94.00   0.75    7.50    --   18.62   0.00-180.00  200
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
;
SuperNova, Single source at offset, Sapphire3
;
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
;
CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      -0.0287072000
_diffrn_orient_matrix_UB_12      0.0406253000
_diffrn_orient_matrix_UB_13      -0.0103461000
_diffrn_orient_matrix_UB_21      -0.0359593000
_diffrn_orient_matrix_UB_22      -0.0096436000
_diffrn_orient_matrix_UB_23      0.0362999000
_diffrn_orient_matrix_UB_31      0.0325223000
_diffrn_orient_matrix_UB_32      0.0090936000
_diffrn_orient_matrix_UB_33      0.0156408000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1053
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.938
_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       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            162864
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.7456
_diffrn_reflns_theta_min         2.2224
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       cube
_exptl_crystal_F_000             2040.000
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol/water'
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.226
_exptl_crystal_size_min          0.166
_refine_diff_density_max         0.423
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    hetero
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1315
_refine_ls_number_reflns         18600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+1.7476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1125
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15687
_reflns_number_total             18600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc04918b2.cif
_cod_data_source_block           Fe_bpp_Noxid_NHoxid_120K
_cod_depositor_comments
;Adding full bibliography for 1559642--1559653.cif.

 Adding full bibliography for 1559642--1559653.cif.
;
_cod_original_cell_volume        4210.47(11)
_cod_database_code               1559653
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              34094