Synthesis, characterisation, and magnetic properties of a permethylindenyl manganocene.
Evans, Alexander; Arnold, Thomas A. Q.; Ransom, Paul; Binding, Samantha C.; Myers, William K.; Crumpton, Agamemnon E.; Turner, Zoë R; Buffet, Jean-Charles; O'Hare, Dermot; Dalton transactions (Cambridge, England : 2003) 54 (2025) 11427–11433; doi:10.1039/d5dt01345c

data_7719079
_publ_section_title
;
 Synthesis, characterisation, and magnetic properties of a
 permethylindenyl manganocene.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11427
_journal_page_last               11433
_journal_paper_doi               10.1039/d5dt01345c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C16 H22'
_chemical_formula_sum            'C16 H22'
_chemical_formula_weight         214.33
_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             2024-12-11
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-02 deposited with the CCDC.	2025-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.765(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0353(4)
_cell_length_b                   10.9285(4)
_cell_length_c                   9.0453(3)
_cell_measurement_reflns_used    11656
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      76.3090
_cell_measurement_theta_min      5.2030
_cell_volume                     1287.95(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_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    -20.00  27.00   1.00    2.50    --  -41.40  37.00 -30.00   47
  2  \w    -14.00  28.00   1.00    2.50    --  -41.40  37.00 -90.00   42
  3  \w     -4.00  34.00   1.00    2.50    --  -41.40  19.00  30.00   38
  4  \w      0.00  35.00   1.00    2.50    --  -41.40  19.00-120.00   35
  5  \w      0.00  29.00   1.00    2.50    --  -41.40  19.00 120.00   29
  6  \w     45.00  77.00   1.00    2.50    --   41.40-125.00 -90.00   32
  7  \w     27.00  54.00   1.00    2.50    --   41.40-125.00 150.00   27
  8  \w     41.00  98.00   1.00   10.98    --  111.00-125.00-150.00   57
  9  \w    111.00 162.00   1.00   10.98    --  111.00  77.00  60.00   51
 10  \w     44.00  72.00   1.00   10.98    --  111.00 -45.00 -90.00   28
 11  \w     56.00  91.00   1.00   10.98    --  111.00 -61.00-120.00   35
 12  \w    105.00 155.00   1.00   10.98    --  111.00  77.00 -30.00   50
 13  \w     41.00  68.00   1.00   10.98    --  111.00 -45.00  30.00   27
 14  \w     40.00  69.00   1.00   10.98    --  111.00 -45.00 -60.00   29
 15  \w    103.00 130.00   1.00   10.98    --  111.00  77.00-120.00   27
 16  \w     95.00 123.00   1.00   10.98    --  111.00 -77.00-120.00   28
 17  \w     39.00  81.00   1.00   10.98    --  111.00 -77.00-120.00   42
 18  \w    104.00 178.00   1.00   10.98    --  111.00  77.00 -90.00   74
 19  \w    145.00 172.00   1.00   10.98    --  111.00  77.00-120.00   27
 20  \w     42.00  68.00   1.00   10.98    --  111.00 -45.00-180.00   26
 21  \w     40.00  65.00   1.00   10.98    --  111.00 -45.00 150.00   25
 22  \w    112.00 156.00   1.00   10.98    --  111.00  77.00 -60.00   44
 23  \w     47.00  87.00   1.00   10.98    --  111.00-125.00 -90.00   40
 24  \w     -2.00  32.00   1.00    2.50    --  -41.40  19.00-180.00   34
 25  \w     -5.00  37.00   1.00    2.50    --  -41.40  19.00 -90.00   42
 26  \w    -18.00  18.00   1.00    2.50    --   41.40 -77.00 150.00   36
 27  \w     27.00  93.00   1.00    2.50    --   41.40-125.00  90.00   66
 28  \w     25.00  64.00   1.00    2.50    --   41.40 -77.00 150.00   39
 29  \w     33.00  60.00   1.00    2.50    --   41.40-125.00   0.00   27
 30  \w     61.00 112.00   1.00   10.98    --  111.00-125.00 150.00   51
 31  \w     48.00  75.00   1.00   10.98    --  111.00 -61.00 -60.00   27
 32  \w    153.00 178.00   1.00   10.98    --  111.00  45.00 150.00   25
 33  \w     32.00  59.00   1.00   10.98    --  111.00 -94.00-120.00   27
 34  \w    125.00 156.00   1.00   10.98    --  111.00  77.00  90.00   31
 35  \w     76.00 111.00   1.00   10.98    --  111.00-125.00-180.00   35
 36  \w     73.00 112.00   1.00   10.98    --  111.00-125.00 120.00   39
 37  \w    103.00 130.00   1.00   10.98    --  111.00 125.00 -30.00   27
 38  \w     42.00  68.00   1.00   10.98    --  111.00 -45.00 -30.00   26
 39  \w     41.00  66.00   1.00   10.98    --  111.00 -61.00 120.00   25
 40  \w    103.00 154.00   1.00   10.98    --  111.00  77.00  30.00   51
 41  \w     52.00  90.00   1.00   10.98    --  111.00 -61.00   0.00   38
 42  \w     64.00  98.00   1.00   10.98    --  111.00 -94.00 -30.00   34
 43  \w    145.00 172.00   1.00   10.98    --  111.00 125.00 -30.00   27
 44  \w     92.00 119.00   1.00   10.98    --  111.00-134.00 -28.00   27
 45  \w     63.00  90.00   1.00   10.98    --  111.00 -94.00-120.00   27
 46  \w    112.00 152.00   1.00   10.98    --  111.00  45.00  30.00   40
 47  \w    100.00 127.00   1.00   10.98    --  111.00  45.00 150.00   27
 48  \w     70.00 107.00   1.00   10.98    --  111.00 -94.00-180.00   37
 49  \w     63.00 107.00   1.00   10.98    --  111.00-102.00  17.67   44
 50  \w      8.00  33.00   1.00    2.50    --   38.00  73.00 -89.86   25
 51  \w      5.00  30.00   1.00    2.50    --   38.00  83.00 -10.59   25
 52  \w    -56.00 -21.00   1.00    2.50    --  -41.40 -37.00  90.00   35
 53  \w    -81.00 -20.00   1.00    2.50    --  -41.40 -37.00-120.00   61
 54  \w   -112.00 -67.00   1.00    2.50    --  -41.40 -37.00  90.00   45
 55  \w      3.00  36.00   1.00    2.50    --  -41.40  19.00  60.00   33
 56  \w     -2.00  33.00   1.00    2.50    --  -41.40  19.00-150.00   35
 57  \w   -114.00 -86.00   1.00    2.50    --  -41.40 -37.00-120.00   28
 58  \w     10.00  35.00   1.00    2.50    --   41.40  75.00 108.68   25
 59  \w     13.00  40.00   1.00    2.50    --   46.00  82.00 150.44   27
 60  \w     14.00  39.00   1.00    2.50    --   46.00  78.00 -35.80   25
 61  \w     13.00  38.00   1.00    2.50    --   46.00  82.00  52.17   25
 62  \w    101.00 126.00   1.00    2.50    --   54.00  71.00 -99.43   25
 63  \w     24.00  51.00   1.00    2.50    --   54.00  70.00   1.05   27
 64  \w     24.00  51.00   1.00    2.50    --   54.00  71.00 -99.43   27
 65  \w     30.00  57.00   1.00    2.50    --   58.00  63.00 150.02   27
 66  \w     29.00  56.00   1.00    2.50    --   58.00  70.00  85.37   27
 67  \w     88.00 115.00   1.00    2.50    --   58.00  63.00 150.02   27
 68  \w     34.00  61.00   1.00    2.50    --   62.00  69.00  29.09   27
 69  \w     37.00  64.00   1.00    2.50    --   66.00  70.00 -83.58   27
 70  \w     40.00  67.00   1.00    2.50    --   66.00  68.00-109.78   27
 71  \w     36.00  63.00   1.00    2.50    --   66.00  70.00 -50.84   27
 72  \w     40.00  66.00   1.00    2.50    --   70.00  71.00 173.65   26
 73  \w     41.00  68.00   1.00    2.50    --   70.00  71.00 -24.18   27
 74  \w     46.00  71.00   1.00    2.50    --   74.00  68.00 138.99   25
 75  \w     44.00  73.00   1.00    2.50    --   74.00  71.00-159.02   29
 76  \w     44.00  71.00   1.00    2.50    --   74.00  71.00  20.87   27
 77  \w     46.00  72.00   1.00    2.50    --   74.00  69.00-109.87   26
 78  \w     49.00  76.00   1.00   10.98    --   78.00  71.00  59.86   27
 79  \w     56.00  83.00   1.00   10.98    --   82.00  64.00 -40.63   27
 80  \w     54.00  79.00   1.00   10.98    --   82.00  69.00  23.96   25
 81  \w     53.00  80.00   1.00   10.98    --   82.00  71.00 -76.88   27
 82  \w     54.00  79.00   1.00   10.98    --   82.00  66.00 163.09   25
 83  \w     53.00  79.00   1.00   10.98    --   82.00  68.00  78.24   26
 84  \w     59.00  84.00   1.00   10.98    --   86.00  64.00 -20.31   25
 85  \w     59.00  84.00   1.00   10.98    --   86.00  64.00  90.57   25
 86  \w     61.00  88.00   1.00   10.98    --   90.00  67.00  38.56   27
 87  \w     61.00  88.00   1.00   10.98    --   90.00  66.00 122.04   27
 88  \w     67.00  92.00   1.00   10.98    --   94.00  63.00  99.62   25
 89  \w     74.00 110.00   1.00   10.98    --   98.00  49.00 -72.07   36
 90  \w     69.00  96.00   1.00   10.98    --   98.00  69.00  -9.11   27
 91  \w     68.00 100.00   1.00   10.98    --   98.00  70.00-138.31   32
 92  \w     73.00  98.00   1.00   10.98    --  102.00  71.00-159.46   25
 93  \w     73.00  99.00   1.00   10.98    --  102.00  68.00  50.89   26
 94  \w     88.00 113.00   1.00   10.98    --  111.00  45.00-180.00   25
 95  \w     43.00  68.00   1.00   10.98    --  111.00-125.00  90.00   25
 96  \w    128.00 172.00   1.00   10.98    --  111.00  61.00 120.00   44
 97  \w    130.00 157.00   1.00   10.98    --  111.00  61.00 -90.00   27
 98  \w     83.00 110.00   1.00   10.98    --  111.00  61.00 -90.00   27
 99  \w     84.00 131.00   1.00   10.98    --  111.00  61.00   0.00   47
100  \w     85.00 170.00   1.00   10.98    --  111.00  61.00-150.00   85
101  \w    150.00 177.00   1.00   10.98    --  111.00  61.00  60.00   27
102  \w     84.00 123.00   1.00   10.98    --  111.00  61.00  60.00   39
103  \w     84.00 113.00   1.00   10.98    --  111.00  61.00 120.00   29
104  \w    140.00 167.00   1.00   10.98    --  111.00  71.00 -73.07   27
105  \w     84.00 111.00   1.00   10.98    --  111.00  61.00 -30.00   27
106  \w    132.00 167.00   1.00   10.98    --  111.00  61.00-120.00   35
107  \w     81.00 129.00   1.00   10.98    --  111.00  71.00 -73.07   48
108  \w     83.00 121.00   1.00   10.98    --  111.00  61.00-120.00   38
109  \w    118.00 149.00   1.00   10.98    --  111.00  61.00 150.00   31
110  \w     84.00 109.00   1.00   10.98    --  111.00  61.00 150.00   25
111  \w    153.00 178.00   1.00   10.98    --  111.00  61.00  90.00   25
112  \w     91.00 139.00   1.00   10.98    --  111.00  61.00  90.00   48
113  \w    151.00 178.00   1.00   10.98    --  111.00  61.00  30.00   27
114  \w     83.00 110.00   1.00   10.98    --  111.00  61.00  30.00   27
115  \w     84.00 166.00   1.00   10.98    --  111.00  61.00-180.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5161
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.388
_diffrn_reflns_theta_min         5.283
_exptl_absorpt_coefficient_mu    0.451
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83349
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_recrystallization_method
'Crystallised from concentrated pentane solution at room temperature'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.041
_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     153
_refine_ls_number_reflns         5161
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0949P)^2^+0.0222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1431
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4125
_reflns_number_total             5161
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9221\% 
around [-0.04 -0.00 1.00] (reciprocal) or [-0.00 -0.00 1.00] (direct)
;
_cod_data_source_file            d5dt01345c2.cif
_cod_data_source_block           IndStarH
_cod_depositor_comments
'Adding full bibliography for 7719078--7719079.cif.'
_cod_database_code               7719079
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.907
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5431(16)
 0.4569(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C1(H1)
3.b Idealised Me refined as rotating group:
 C00C(H00A,H00B,H00C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              56384
_shelx_hkl_checksum              16426
_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
;