Construction of spin crossover-fluorescence bifunctional iron(ii) complexes with modified bis(pyrazole)pyridine ligands
Zhao, Guo-Hui; Zhang, Shi-Hui; Yi, Cheng; Liu, Tao; Meng, Yin-Shan; New Journal of Chemistry 47 (2023) 10967–10972; doi:10.1039/D3NJ01431B

data_7062475
_publ_section_title
;
 Construction of spin crossover-fluorescence bifunctional iron(ii)
 complexes with modified bis(pyrazole)pyridine ligands
;
_journal_issue                   23
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10967
_journal_page_last               10972
_journal_paper_doi               10.1039/D3NJ01431B
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C42 H30 Fe N10, 2(Cl O4)'
_chemical_formula_sum            'C42 H30 Cl2 Fe N10 O8'
_chemical_formula_weight         929.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           54
_space_group_name_Hall           '-P 2a 2ac'
_space_group_name_H-M_alt        'P c c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-02
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-05-02 deposited with the CCDC.	2023-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.6912(18)
_cell_length_b                   11.9055(10)
_cell_length_c                   14.9444(18)
_cell_measurement_reflns_used    2155
_cell_measurement_temperature    399.99(10)
_cell_measurement_theta_max      23.0350
_cell_measurement_theta_min      1.7790
_cell_volume                     4037.2(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      399.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -26.00  28.00   0.50   14.68    --    9.48  95.00 131.00  108
  2  \w     13.00  63.00   0.50   14.68    --    9.48  45.00  26.00  100
  3  \w    -43.00  34.00   0.50   14.68    --  -11.20  89.00-125.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0282944000
_diffrn_orient_matrix_UB_12      -0.0216417000
_diffrn_orient_matrix_UB_13      -0.0103903000
_diffrn_orient_matrix_UB_21      -0.0014777000
_diffrn_orient_matrix_UB_22      0.0252691000
_diffrn_orient_matrix_UB_23      -0.0429019000
_diffrn_orient_matrix_UB_31      0.0132025000
_diffrn_orient_matrix_UB_32      0.0494028000
_diffrn_orient_matrix_UB_33      0.0174793000
_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  0.1253
_diffrn_reflns_av_unetI/netI     0.0973
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17163
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.710
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull dark red'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       needle
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3557
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.2130
_refine_ls_R_factor_gt           0.1030
_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^)+(0.0251P)^2^+12.4501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1437
_refine_ls_wR_factor_ref         0.1805
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1664
_reflns_number_total             3557
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj01431b2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7062474--7062476.cif.'
_cod_database_code               7062475
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         FeC40S2N6H18Cl4O2
_chemical_oxdiff_usercomment     MYS-2-400K
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.846
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
O4 \\sim Cl2 \\sim O6 \\sim O3 \\sim O5: within 3A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 3A
Uanis(O2) = Uanis(O2A)
3. Others
 Fixed Sof: O2(0.5) O4(0.5) O6(0.5) O3(0.5) O5(0.5) O2A(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C19(H19), C17(H17), C12(H12), C5(H5), C15(H15), C18(H18), C1(H1),
 C3(H3), C20(H20), C4(H4), C21(H21), C16(H16), C6(H6), C9(H9)
;
_shelx_res_checksum              64104
_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 1.235
_oxdiff_exptl_absorpt_empirical_full_min 0.889