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_7706481
_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, C6 H8 O4'
_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-2017/1
_audit_update_record
;
2018-01-26 deposited with the CCDC.	2021-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 94.2540(10)
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   18.4520(2)
_cell_length_b                   20.1395(3)
_cell_length_c                   15.0697(2)
_cell_measurement_reflns_used    17942
_cell_measurement_temperature    298.00(10)
_cell_measurement_theta_max      28.3000
_cell_measurement_theta_min      2.9880
_cell_volume                     5584.68(13)
_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      air
_diffrn_ambient_temperature      298.00(10)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.9989
_diffrn_measured_fraction_theta_max 0.9524
_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    -90.00  10.00   0.50    7.00    --  -19.87 -77.00-120.00  200
  2  \w    -90.00  10.00   0.50    7.00    --  -19.87 -77.00 -30.00  200
  3  \w    -96.00 -34.00   0.50    7.00    --  -19.87 178.00  90.00  124
  4  \w    -96.00 -35.00   0.50    7.00    --  -19.87-178.00  30.00  122
  5  \w    -20.00  63.00   0.50    7.00    --   20.73 -99.00-120.00  166
  6  \w    -20.00  63.00   0.50    7.00    --   20.73 -99.00 120.00  166
  7  \w    -20.00  63.00   0.50    7.00    --   20.73 -99.00  60.00  166
  8  \w    -48.00  42.00   0.50    7.00    --   20.73 -57.00  90.00  180
  9  \w    -23.00  94.00   0.50    7.00    --   20.73  19.00 -90.00  234
 10  \w    -96.00 -35.00   0.50    7.00    --  -19.87-178.00-150.00  122
 11  \w    -89.00   2.00   0.50    7.00    --  -19.87 -57.00   0.00  182
 12  \w    -90.00 -11.00   0.50    7.00    --  -19.87 -77.00 120.00  158
 13  \w    -92.00   6.00   0.50    7.00    --  -19.87 -38.00  60.00  196
;
_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      0.0049721000
_diffrn_orient_matrix_UB_12      0.0239674000
_diffrn_orient_matrix_UB_13      -0.0335056000
_diffrn_orient_matrix_UB_21      0.0373372000
_diffrn_orient_matrix_UB_22      0.0023871000
_diffrn_orient_matrix_UB_23      0.0145551000
_diffrn_orient_matrix_UB_31      0.0081174000
_diffrn_orient_matrix_UB_32      -0.0257124000
_diffrn_orient_matrix_UB_33      -0.0298715000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            69177
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        27.4248
_diffrn_reflns_theta_max         29.9887
_diffrn_reflns_theta_min         2.4345
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       prism
_exptl_crystal_F_000             2576
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Single crystal to single crystal thermal dehydration'
_exptl_crystal_size_max          0.406
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.073
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         7758
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0421P)^2^+4.2937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.1029
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5712
_reflns_number_total             7758
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03986a2.cif
_cod_data_source_block           Fe_bpp_adip_anh_298K
_cod_depositor_comments
'Adding full bibliography for 7706480--7706481.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7706481
_shelx_shelxl_version_number     2017/1
_exptl_absorpt_special_details
;
 ?
;
_shelx_res_checksum              72049
_shelx_hkl_checksum              33555