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_7716763
_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         'C46 H26 Br2 Fe N6 O2, 2(C3 H6 O)'
_chemical_formula_sum            'C52 H38 Br2 Fe N6 O4'
_chemical_formula_weight         1026.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 94.632(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1295(3)
_cell_length_b                   8.9127(2)
_cell_length_c                   29.6320(5)
_cell_measurement_reflns_used    9264
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      64.9320
_cell_measurement_theta_min      4.0770
_cell_volume                     4509.14(15)
_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      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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   -116.00 -18.00   1.00    1.13    --  -42.06 -38.00-150.00   98
  2  \w   -122.00  -1.00   1.00    1.13    --  -42.06 -19.00 -60.00  121
  3  \w    103.00 166.00   1.00    4.51    --   89.35  77.00 -90.00   63
  4  \w    103.00 166.00   1.00    4.51    --   89.35  77.00-150.00   63
  5  \w     97.00 163.00   1.00    4.51    --   89.35 125.00 120.00   66
  6  \w     16.00 115.00   1.00    4.51    --   89.35 -45.00 120.00   99
  7  \w     60.00 162.00   1.00    4.51    --   89.35  61.00 -30.00  102
  8  \w     16.00 115.00   1.00    4.51    --   89.35 -45.00   0.00   99
  9  \w    103.00 166.00   1.00    4.51    --   89.35  77.00-180.00   63
;
_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      -0.0736199000
_diffrn_orient_matrix_UB_12      -0.0986407000
_diffrn_orient_matrix_UB_13      -0.0085075000
_diffrn_orient_matrix_UB_21      -0.0064353000
_diffrn_orient_matrix_UB_22      0.0463187000
_diffrn_orient_matrix_UB_23      -0.0502519000
_diffrn_orient_matrix_UB_31      0.0517682000
_diffrn_orient_matrix_UB_32      -0.1342124000
_diffrn_orient_matrix_UB_33      -0.0110439000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            21922
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        65.288
_diffrn_reflns_theta_max         65.288
_diffrn_reflns_theta_min         3.796
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.194
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34216
_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    1.512
_exptl_crystal_description       needle
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         7597
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0619P)^2^+4.2212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1355
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6079
_reflns_number_total             7597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00904e2.cif
_cod_data_source_block           2206
_cod_depositor_comments
'Adding full bibliography for 7716761--7716766.cif.'
_cod_original_cell_volume        4509.15(15)
_cod_database_code               7716763
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHONFeCl
_chemical_oxdiff_usercomment     CHONFeCl
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_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 Me refined with riding coordinates:
 C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C53(H53A,H53B,
 H53C)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C10(H10), C11(H11), C13(H13), C14(H14),
 C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C27(H27), C28(H28), C29(H29),
  C31(H31), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C42(H42),
 C43(H43), C45(H45), C46(H46)
;
_shelx_res_checksum              53597
_shelx_hkl_checksum              40714
_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 1.999
_oxdiff_exptl_absorpt_empirical_full_min 0.568