Design, synthesis, and redox properties of donor-π-donor ferrocenyl functionalized phenothiazine derivatives.
Gupta, Deeksha; Tiwari, Nikhil Ji; Singh, Prabal Pratap; Misra, Rajneesh; Dalton transactions (Cambridge, England : 2003) 54 (2025) 5906–5920; doi:10.1039/d4dt03552f

data_7718203
_publ_section_title
;
 Design, synthesis, and redox properties of donor-&#x3c0;-donor ferrocenyl
 functionalized phenothiazine derivatives.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5906
_journal_page_last               5920
_journal_paper_doi               10.1039/d4dt03552f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C60 H45 Fe3 N S'
_chemical_formula_sum            'C60 H45 Fe3 N S'
_chemical_formula_weight         979.58
_chemical_name_systematic        Phenothiazene
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-10-10
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-10-10 deposited with the CCDC.	2025-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.099(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6310(2)
_cell_length_b                   26.5578(5)
_cell_length_c                   14.6540(2)
_cell_measurement_reflns_used    40703
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.5630
_cell_measurement_theta_min      1.8150
_cell_volume                     4914.80(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5-beta (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -29.00  21.00   0.50    8.00    --   10.55 -41.00  67.00  100
  2  \w    -23.00  46.00   0.50    8.00    --   10.55 -99.00 150.00  138
  3  \w     12.00  60.00   0.50    8.00    --   10.55-125.00  90.00   96
  4  \w     23.00  61.00   0.50    8.00    --   10.55-125.00 -60.00   76
  5  \w     13.00  61.00   0.50    8.00    --   10.55-125.00-150.00   96
  6  \w     -8.00  18.00   0.50    8.00    --  -11.09 -99.00-120.00   52
  7  \w    -23.00   8.00   0.50    8.00    --  -11.09 -99.00-150.00   62
  8  \w    -18.00  23.00   0.50    8.00    --  -11.09 -99.00 -90.00   82
  9  \w    -23.00  19.00   0.50    8.00    --  -11.09 -99.00   0.00   84
 10  \w    -22.00  20.00   0.50    8.00    --  -11.09 -99.00  60.00   84
 11  \w    -23.00  18.00   0.50    8.00    --  -11.09 -99.00  90.00   82
 12  \w    -16.00  22.00   0.50    8.00    --  -11.09 -99.00 150.00   76
 13  \w    -49.00  21.00   0.50    8.00    --   10.55 -37.00  30.00  140
 14  \w    -53.00  21.00   0.50    8.00    --   10.55 -37.00   0.00  148
 15  \w     10.00  55.00   0.50    8.00    --  -11.09  41.00-139.00   90
 16  \w     11.00  36.00   0.50    8.00    --   10.55  41.00-139.00   50
 17  \w    -18.00   7.00   0.50    8.00    --  -11.09  41.00-139.00   50
 18  \w    -44.00 -10.00   0.50    8.00    --   10.55 -37.00-180.00   68
 19  \w    -64.00 -39.00   0.50    8.00    --  -11.09 -19.00  30.00   50
 20  \w    -67.00 -18.00   0.50    8.00    --  -11.09 -41.00  67.00   98
 21  \w    -59.00   5.00   0.50    8.00    --   10.55 -19.00 150.00  128
 22  \w    -14.00  12.00   0.50    8.00    --   10.55  77.00  60.00   52
 23  \w     25.00  79.00   0.50    8.00    --   10.55  77.00  60.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0193314000
_diffrn_orient_matrix_UB_12      -0.0111858000
_diffrn_orient_matrix_UB_13      -0.0403469000
_diffrn_orient_matrix_UB_21      0.0519632000
_diffrn_orient_matrix_UB_22      0.0081403000
_diffrn_orient_matrix_UB_23      0.0118448000
_diffrn_orient_matrix_UB_31      0.0090426000
_diffrn_orient_matrix_UB_32      -0.0228415000
_diffrn_orient_matrix_UB_33      0.0239871000
_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  0.0386
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            76112
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.786
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.955
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_preparation       'Hexane:DCM solution'
_exptl_crystal_recrystallization_method '293 K'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         8612
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+0.4909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6826
_reflns_number_total             8612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03552f2.cif
_cod_data_source_block           dg14
_cod_depositor_comments
'Adding full bibliography for 7718203--7718204.cif.'
_cod_database_code               7718203
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C60 H45 N Fe3 S'
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.894
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10),
 C12(H12), C13(H13), C15(H15), C16(H16), C18(H18), C19(H19), C22(H22), C25(H25),
  C27(H27), C28(H28), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35),
 C36(H36), C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C43(H43), C44(H44),
  C46(H46), C47(H47), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53),
 C54(H54), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              63073
_shelx_hkl_checksum              32971
_shelx_fab_checksum              62997
_olex2_exptl_crystal_mounting_method '293 K'
_olex2_submission_original_sample_id DG14
_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 1.109
_oxdiff_exptl_absorpt_empirical_full_min 0.745