Substituent effects on spin-crossover Fe(II)N<sub>4</sub>O<sub>2</sub> pyrenylhydrazone complexes.
Wang, Xuan; Zhang, Nan; Kou, Hui-Zhong; Dalton transactions (Cambridge, England : 2003) 53 (2024) 16592–16597; doi:10.1039/d4dt00904e

data_7716761
_publ_section_title
;
 Substituent effects on spin-crossover Fe(II)N<sub>4</sub>O<sub>2</sub>
 pyrenylhydrazone complexes.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16592
_journal_page_last               16597
_journal_paper_doi               10.1039/d4dt00904e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C50 H36 Fe N6 O2,6[H2O]'
_chemical_formula_sum            'C50 H48 Fe N6 O8'
_chemical_formula_weight         916.79
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-02-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-03-08 deposited with the CCDC.	2024-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.7568(8)
_cell_length_b                   15.7568(8)
_cell_length_c                   38.012(2)
_cell_measurement_reflns_used    5207
_cell_measurement_temperature    220.00(10)
_cell_measurement_theta_max      25.6430
_cell_measurement_theta_min      3.9710
_cell_volume                     9437.5(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      220.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.858
_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     31.00  60.00   1.00    9.59    --  -10.83  38.00 120.00   29
  2  \w    -34.00  17.00   1.00    9.59    --  -10.83  77.00 120.00   51
  3  \w    -31.00  -2.00   1.00    9.59    --  -10.83  38.00 120.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0295411000
_diffrn_orient_matrix_UB_12      -0.0198251000
_diffrn_orient_matrix_UB_13      0.0114342000
_diffrn_orient_matrix_UB_21      -0.0255066000
_diffrn_orient_matrix_UB_22      -0.0370570000
_diffrn_orient_matrix_UB_23      0.0003420000
_diffrn_orient_matrix_UB_31      0.0223304000
_diffrn_orient_matrix_UB_32      -0.0162917000
_diffrn_orient_matrix_UB_33      -0.0147381000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.1051
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            12828
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.432
_diffrn_reflns_theta_min         3.657
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.362
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       flake
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         5614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1516
_refine_ls_R_factor_gt           0.0969
_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^)+(0.1224P)^2^+13.5962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2603
_refine_ls_wR_factor_ref         0.3004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2887
_reflns_number_total             5614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00904e2.cif
_cod_data_source_block           exp_7949
_cod_depositor_comments
'Adding full bibliography for 7716761--7716766.cif.'
_cod_original_cell_volume        9437.5(11)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7716761
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHONFeCl
_chemical_oxdiff_usercomment     CHONFeCl
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00G(H00G), C00J(H00J), C00K(H00K), C00M(H00M), C00N(H00N),
 C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R), C00T(H00T), C00V(H00V)
2.b Idealised Me refined as rotating group:
 C00L(H00A,H00C,H00D), C00S(H00E,H00F,H00H)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 477 electrons were 
found in a volume of 2298\%A^3^ in 4 voids per unit cell. 
This is consistent with the presence of 
6[H2O] per Formula Unit 
which account for 480 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              48210
_shelx_hkl_checksum              57040
_shelx_fab_checksum              10879
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.158
_oxdiff_exptl_absorpt_empirical_full_min 0.862