Hydrogen-bonded assemblies of iron(II) spin crossover complexes.
Jornet-Mollá, Verónica; Rodríguez-Tarrazó, Marina I; Dolz-Lozano, Miquel J; Giménez-Saiz, Carlos; Romero, Francisco M.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7848–7856; doi:10.1039/d4dt00579a

data_7715705
_publ_section_title
;
 Hydrogen-bonded assemblies of iron(II) spin crossover complexes.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7848
_journal_page_last               7856
_journal_paper_doi               10.1039/d4dt00579a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C22 H18 Fe N10 2+, C16 H8 O4 2-, 9(H2 O)'
_chemical_formula_sum            'C38 H44 Fe N10 O13'
_chemical_formula_weight         904.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-02-27 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9374(2)
_cell_length_b                   14.5137(2)
_cell_length_c                   23.8247(3)
_cell_measurement_reflns_used    14889
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      27.7400
_cell_measurement_theta_min      3.3830
_cell_volume                     4127.77(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SIR2014 (Burla et al., 2015)'
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.971
_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    -95.00  28.00   1.00   22.50    --  -20.96 -19.00  60.00  123
  2  \w    -92.00  11.00   1.00   22.50    --  -20.96 -77.00-120.00  103
  3  \w    -90.00   1.00   1.00   22.50    --  -20.96 -57.00   0.00   91
  4  \w    -20.00  65.00   1.00   22.50    --   21.90 -99.00 150.00   85
  5  \w    -20.00  65.00   1.00   22.50    --   21.90 -99.00  30.00   85
  6  \w    -20.00  65.00   1.00   22.50    --   21.90 -99.00 -30.00   85
  7  \w    -99.00 -35.00   1.00   22.50    --  -20.96-178.00 120.00   64
  8  \w    -48.00  52.00   1.00   22.50    --  -20.96  38.00-120.00  100
  9  \w    -90.00   1.00   1.00   22.50    --  -20.96 -57.00 -90.00   91
 10  \w    -10.00  93.00   1.00   22.50    --   21.90  77.00 150.00  103
 11  \w     35.00 100.00   1.00   22.50    --   21.90 178.00 150.00   65
 12  \w    -49.00  15.00   1.00   22.50    --   21.90 -77.00-180.00   64
 13  \w      0.00  91.00   1.00   22.50    --   21.90  57.00 -90.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
;
'SuperNova, Single source at offset, Sapphire3'
;
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0338553000
_diffrn_orient_matrix_UB_12      -0.0235491000
_diffrn_orient_matrix_UB_13      0.0198145000
_diffrn_orient_matrix_UB_21      -0.0402597000
_diffrn_orient_matrix_UB_22      0.0358637000
_diffrn_orient_matrix_UB_23      -0.0014358000
_diffrn_orient_matrix_UB_31      -0.0276290000
_diffrn_orient_matrix_UB_32      -0.0234016000
_diffrn_orient_matrix_UB_33      -0.0221743000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1169
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            100177
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.923
_diffrn_reflns_theta_min         3.285
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58260
_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    1.456
_exptl_crystal_description       needle
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.2448
_exptl_crystal_size_mid          0.0738
_exptl_crystal_size_min          0.0333
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 3126 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         11400
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0454P)^2^+2.0430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1238
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.927
_reflns_number_gt                9136
_reflns_number_total             11400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00579a2.cif
_cod_data_source_block           MRT4C-2-H
_cod_depositor_comments
'Adding full bibliography for 7715705--7715707.cif.'
_cod_database_code               7715705
_shelx_res_checksum              27123