Temperature dependence of desolvation effects in hydrogen-bonded spin crossover complexes.
Jornet-Mollá, Verónica; Giménez-Saiz, Carlos; Vieira, Bruno J. C.; Waerenborgh, João C; Romero, Francisco M.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 2536–2544; doi:10.1039/d0dt03986a

data_7706480
_publ_section_title
;
 Temperature dependence of desolvation effects in hydrogen-bonded spin
 crossover complexes.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2536
_journal_page_last               2544
_journal_paper_doi               10.1039/d0dt03986a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         '(C22 H18 Fe N10 2+) (C6 H8 O4 2-)'
_chemical_formula_sum            'C28 H26 Fe N10 O4'
_chemical_formula_weight         622.44
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2016-10-03 deposited with the CCDC.	2021-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.730(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.3091(5)
_cell_length_b                   20.1160(4)
_cell_length_c                   14.9144(3)
_cell_measurement_reflns_used    13333
_cell_measurement_temperature    119.9(2)
_cell_measurement_theta_max      27.3750
_cell_measurement_theta_min      3.0460
_cell_volume                     5481.4(2)
_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-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.9(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.954
_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    -96.00   8.50   0.95   21.00    --  -22.74 -38.00-150.00  110
  2  \w    -89.00  52.55   0.95   21.00    --  -22.74  19.00-150.00  149
  3  \w   -102.00 -35.50   0.95   21.00    --  -22.74-178.00  30.00   70
  4  \w    -95.00   9.50   0.95   21.00    --  -22.74 -77.00 -60.00  110
  5  \w    -20.00  67.40   0.95   21.00    --   23.37 -99.00-150.00   92
  6  \w     34.00 105.25   0.95   21.00    --   23.37-178.00 150.00   75
  7  \w    -93.00   0.10   0.95   21.00    --  -22.74 -57.00  90.00   98
  8  \w    -93.00   0.10   0.95   21.00    --  -22.74 -57.00  30.00   98
  9  \w    -93.00   0.10   0.95   21.00    --  -22.74 -57.00-180.00   98
 10  \w   -102.00 -35.50   0.95   21.00    --  -22.74-178.00-150.00   70
 11  \w     35.00 102.45   0.95   21.00    --   23.37 178.00   0.00   71
 12  \w    -95.00   9.50   0.95   21.00    --  -22.74 -77.00  60.00  110
 13  \w    -49.00  55.50   0.95   21.00    --   23.37 -77.00   0.00  110
;
_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      0.0038086000
_diffrn_orient_matrix_UB_12      0.0199332000
_diffrn_orient_matrix_UB_13      -0.0386502000
_diffrn_orient_matrix_UB_21      -0.0382772000
_diffrn_orient_matrix_UB_22      -0.0019120000
_diffrn_orient_matrix_UB_23      -0.0105095000
_diffrn_orient_matrix_UB_31      -0.0052053000
_diffrn_orient_matrix_UB_32      0.0290254000
_diffrn_orient_matrix_UB_33      0.0258378000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            65275
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        28.500
_diffrn_reflns_theta_max         29.792
_diffrn_reflns_theta_min         3.012
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       prism
_exptl_crystal_F_000             2576
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.059
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         7476
_refine_ls_number_restraints     294
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+11.8154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1094
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6047
_reflns_number_total             7476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03986a2.cif
_cod_data_source_block           Fe_bpp_adip_anh
_cod_depositor_comments
'Adding full bibliography for 7706480--7706481.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7706480
_shelxl_version_number           2014-3
_shelx_res_checksum              99369
_shelx_hkl_checksum              63640