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_7718204
_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         'C50 H37 Fe2 N S'
_chemical_formula_sum            'C50 H37 Fe2 N S'
_chemical_formula_weight         795.56
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-08-09
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-08-09 deposited with the CCDC.	2025-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.229(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.8411(5)
_cell_length_b                   10.6895(3)
_cell_length_c                   16.3082(3)
_cell_measurement_reflns_used    28922
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.2670
_cell_measurement_theta_min      2.1150
_cell_volume                     3806.61(15)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -28.00   4.00   0.50   15.00    --  -11.09  57.00   0.00   64
  2  \w     17.00  55.00   0.50   15.00    --  -11.09  57.00   0.00   76
  3  \w     50.00  77.00   0.50   15.00    --   10.55  37.00  90.00   54
  4  \w      6.00  79.00   0.50   15.00    --   10.55  75.00 -48.00  146
  5  \w    -34.00  -1.00   0.50   15.00    --  -11.09  75.00 -48.00   66
  6  \w      0.00  47.00   0.50   15.00    --   10.55  37.00  90.00   94
  7  \w    -22.00  46.00   0.50   15.00    --   10.55 -99.00 150.00  136
  8  \w     12.00  50.00   0.50   15.00    --   10.55-125.00  60.00   76
  9  \w     -8.00  24.00   0.50   15.00    --  -11.09 -99.00 120.00   64
 10  \w    -20.00  24.00   0.50   15.00    --  -11.09 -99.00  60.00   88
 11  \w    -20.00   7.00   0.50   15.00    --  -11.09 -99.00   0.00   54
 12  \w    -23.00  24.00   0.50   15.00    --  -11.09 -99.00 -60.00   94
 13  \w     20.00  61.00   0.50   15.00    --   10.55-125.00-120.00   82
 14  \w     12.00  47.00   0.50   15.00    --   10.55-125.00-150.00   70
 15  \w    -15.00  15.00   0.50   15.00    --  -11.09 -75.00-176.00   60
 16  \w    -23.00  21.00   0.50   15.00    --  -11.09 -99.00-150.00   88
 17  \w    -23.00   2.00   0.50   15.00    --  -11.09 -99.00 -90.00   50
 18  \w    -46.00  21.00   0.50   15.00    --   10.55 -37.00-120.00  134
 19  \w    -57.00  15.00   0.50   15.00    --   10.55 -75.00-176.00  144
 20  \w    -77.00 -26.00   0.50   15.00    --  -11.09 -75.00-176.00  102
 21  \w    -77.00  -4.00   0.50   15.00    --  -11.09 -37.00   0.00  146
 22  \w    -62.00   5.00   0.50   15.00    --   10.55 -19.00 120.00  134
;
_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      0.0105574000
_diffrn_orient_matrix_UB_12      0.0210161000
_diffrn_orient_matrix_UB_13      0.0390644000
_diffrn_orient_matrix_UB_21      0.0154082000
_diffrn_orient_matrix_UB_22      0.0504472000
_diffrn_orient_matrix_UB_23      -0.0188385000
_diffrn_orient_matrix_UB_31      -0.0265778000
_diffrn_orient_matrix_UB_32      0.0376240000
_diffrn_orient_matrix_UB_33      0.0034385000
_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  0.0411
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            58498
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.865
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.854
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78187
_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 yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1648
_exptl_crystal_preparation       'hexane:DCM mixture at 293 K'
_exptl_crystal_recrystallization_method '293 K'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         6696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+0.6354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1047
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5110
_reflns_number_total             6696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03552f2.cif
_cod_data_source_block           dg_11_red
_cod_depositor_comments
;

2025-04-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel

 Adding full bibliography for 7718203--7718204.cif.
;
_cod_original_formula_moiety     '4(C50 H37 Fe2 N S)'
_cod_original_formula_sum        'C200 H148 Fe8 N4 S4'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     3182.26
_cod_database_code               7718204
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C192 H148 Fe8 N12 S4 '
_shelx_estimated_absorpt_t_max   0.848
_shelx_estimated_absorpt_t_min   0.784
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C6(H6), C8(H8), C10(H10)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C12(H12), C13(H13), C15(H15), C16(H16),
 C18(H18), C21(H21), C22(H22), C25(H25), C27(H27), C28(H28), C30(H30), C31(H31),
  C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40),
 C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
  C49(H49)
;
_shelx_res_checksum              8079
_shelx_hkl_checksum              21138
_olex2_exptl_crystal_mounting_method '293 K'
_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 1.274
_oxdiff_exptl_absorpt_empirical_full_min 0.720