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_7715707
_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+, C14 H8 O4 2-, 5(H2 O)'
_chemical_formula_sum            'C36 H36 Fe N10 O9'
_chemical_formula_weight         808.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_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                   28.8805(5)
_cell_length_b                   15.3810(2)
_cell_length_c                   8.49297(12)
_cell_measurement_reflns_used    18200
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      24.9870
_cell_measurement_theta_min      3.4420
_cell_volume                     3772.67(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 0.996
_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    -46.00  48.00   1.00   22.50    --  -22.59  57.00 -30.00   94
  2  \w    -93.00   1.00   1.00   22.50    --  -22.59 -57.00-180.00   94
  3  \w    -75.00   8.00   1.00   22.50    --  -22.59 113.00  52.00   83
  4  \w   -102.00 -35.00   1.00   22.50    --  -22.59-178.00  60.00   67
  5  \w   -102.00 -35.00   1.00   22.50    --  -22.59-178.00 -90.00   67
  6  \w    -46.00  48.00   1.00   22.50    --  -22.59  57.00 -60.00   94
  7  \w     -8.00  76.00   1.00   22.50    --   23.52-113.00 -39.00   84
  8  \w    -43.00  99.00   1.00   22.50    --   23.52  19.00   0.00  142
  9  \w    -93.00   1.00   1.00   22.50    --  -22.59 -57.00  30.00   94
 10  \w    -95.00 -70.00   1.00   22.50    --  -22.59 -77.00 120.00   25
 11  \w   -102.00 -35.00   1.00   22.50    --  -22.59-178.00 120.00   67
 12  \w    -95.00  10.00   1.00   22.50    --  -22.59 -77.00  90.00  105
 13  \w    -10.00  96.00   1.00   22.50    --   23.52  77.00   0.00  106
 14  \w      0.00  94.00   1.00   22.50    --   23.52  57.00 -90.00   94
;
_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      0.0239881000
_diffrn_orient_matrix_UB_12      -0.0074385000
_diffrn_orient_matrix_UB_13      -0.0117143000
_diffrn_orient_matrix_UB_21      0.0026702000
_diffrn_orient_matrix_UB_22      -0.0087242000
_diffrn_orient_matrix_UB_23      0.0815186000
_diffrn_orient_matrix_UB_31      -0.0045175000
_diffrn_orient_matrix_UB_32      -0.0446681000
_diffrn_orient_matrix_UB_33      -0.0139601000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            91426
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.761
_diffrn_reflns_theta_min         3.391
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.468
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46732
_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            yellow
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       plate
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.3441
_exptl_crystal_size_mid          0.1026
_exptl_crystal_size_min          0.0199
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.083(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         10240
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0347P)^2^+2.2793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1061
_reflns_Friedel_coverage         0.758
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.925
_reflns_number_gt                8885
_reflns_number_total             10240
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00579a2.cif
_cod_data_source_block           MRT14c-6
_cod_depositor_comments
'Adding full bibliography for 7715705--7715707.cif.'
_cod_database_code               7715707
_shelx_res_checksum              44219