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_7719078
_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         'C32 H42 Mn'
_chemical_formula_sum            'C32 H42 Mn'
_chemical_formula_weight         481.59
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-01-14
_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                102.1125(6)
_cell_angle_beta                 95.2335(5)
_cell_angle_gamma                115.4354(7)
_cell_formula_units_Z            2
_cell_length_a                   9.05112(6)
_cell_length_b                   10.38233(8)
_cell_length_c                   15.81224(10)
_cell_measurement_reflns_used    31884
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.4320
_cell_measurement_theta_min      2.8920
_cell_volume                     1284.035(18)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_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     42.00  77.00   0.50    0.66    --   57.25-132.00 140.00   70
  2  \w     30.00  64.00   0.50    0.66    --   57.25-137.00 -36.00   68
  3  \w     65.00 108.00   0.50    0.66    --   69.96-132.00 140.00   86
  4  \w     76.00 115.00   0.50    0.66    --   69.96 137.00  26.00   78
  5  \w     55.00 106.00   0.50    0.66    --   69.96-137.00 -36.00  102
  6  \w     78.00 103.00   0.50    0.66    --   84.02 137.00  26.00   50
  7  \w     54.00  79.00   0.50    0.66    --   84.02-137.00 -36.00   50
  8  \w     79.00 104.00   0.50    0.66    --   84.02 132.00-150.00   50
  9  \w     91.00 116.00   0.50    0.66    --   84.02-132.00 140.00   50
 10  \w      6.00  36.00   0.50    0.66    --   57.25 -30.00 -30.00   60
 11  \w      4.00  33.00   0.50    0.66    --   57.25 -30.00 -90.00   58
 12  \w     60.00  85.00   0.50    0.66    --   57.25  61.00 -30.00   50
 13  \w      4.00  36.00   0.50    0.66    --   57.25 -30.00-150.00   64
 14  \w      7.00  35.00   0.50    0.66    --   57.25 -30.00 -60.00   56
 15  \w     18.00  54.00   0.50    0.66    --   57.25 -61.00-180.00   72
 16  \w     20.00  49.00   0.50    0.66    --   69.96 -45.00   0.00   58
 17  \w     31.00  77.00   0.50    0.66    --   69.96 -95.00-180.00   92
 18  \w     20.00  51.00   0.50    0.66    --   69.96 -45.00 120.00   62
 19  \w     92.00 118.00   0.50    0.66    --   69.96  45.00  60.00   52
 20  \w     28.00  84.00   0.50    0.66    --   69.96 -95.00   0.00  112
 21  \w     22.00  61.00   0.50    0.66    --   69.96-125.00   0.00   78
 22  \w     75.00 109.00   0.50    0.66    --   69.96  45.00 120.00   68
 23  \w     79.00 115.00   0.50    0.66    --   69.96  45.00-150.00   72
 24  \w     23.00  48.00   0.50    0.66    --   69.96 -45.00  90.00   50
 25  \w     78.00 104.00   0.50    0.66    --   69.96-125.00   0.00   52
 26  \w     41.00  96.00   0.50    0.66    --   84.02 -95.00  90.00  110
 27  \w     40.00  92.00   0.50    0.66    --   84.02 -95.00 -90.00  104
 28  \w     89.00 114.00   0.50    0.66    --   84.02  45.00-180.00   50
 29  \w     51.00  76.00   0.50    0.66    --   84.02 178.00 -30.00   50
 30  \w     82.00 108.00   0.50    0.66    --   84.02-111.00-120.00   52
 31  \w     48.00  89.00   0.50    0.66    --   84.02-111.00 -90.00   82
 32  \w     37.00  66.00   0.50    0.66    --   84.02 -61.00   0.00   58
 33  \w     49.00  74.00   0.50    0.66    --   84.02 -95.00 120.00   50
 34  \w     55.00  80.00   0.50    0.66    --   84.02 -77.00  30.00   50
 35  \w     52.00  78.00   0.50    0.66    --   84.02-111.00 150.00   52
 36  \w     66.00 107.00   0.50    0.66    --   84.02-111.00  30.00   82
 37  \w     41.00  67.00   0.50    0.66    --   84.02 -95.00 150.00   52
 38  \w     69.00 116.00   0.50    0.66    --   84.02   0.00 -60.00   94
 39  \w     43.00  82.00   0.50    0.66    --   84.02 -77.00-150.00   78
 40  \w     77.00 107.00   0.50    0.66    --   84.02-111.00-180.00   60
 41  \w     40.00  65.00   0.50    0.66    --   84.02-111.00   0.00   50
 42  \w     91.00 135.00   0.50    0.66    --   84.02  45.00 -90.00   88
 43  \w     48.00  77.00   0.50    0.66    --   84.02 -77.00-180.00   58
 44  \w     40.00  65.00   0.50    0.66    --   84.02 -61.00 150.00   50
 45  \w     41.00  66.00   0.50    0.66    --   84.02 -61.00 120.00   50
 46  \w     45.00  70.00   0.50    0.66    --   84.02 -77.00 -90.00   50
 47  \w     99.00 135.00   0.50    0.66    --   84.02  45.00 -30.00   72
 48  \w     73.00 108.00   0.50    0.66    --   84.02-111.00 -30.00   70
 49  \w     40.00  71.00   0.50    0.66    --   84.02 -95.00   0.00   62
 50  \w     40.00  66.00   0.50    0.66    --   84.02-111.00  90.00   52
 51  \w     83.00 108.00   0.50    0.66    --   84.02-111.00  90.00   50
 52  \w     96.00 121.00   0.50    0.66    --   84.02  45.00-150.00   50
 53  \w     57.00  86.00   0.50    0.66    --   84.02 -77.00 150.00   58
 54  \w     46.00  71.00   0.50    0.66    --   84.02-111.00 -30.00   50
 55  \w     97.00 125.00   0.50    0.66    --   84.02  45.00-120.00   56
 56  \w     79.00 108.00   0.50    0.66    --   84.02-111.00 150.00   58
 57  \w     60.00  87.00   0.50    0.66    --   84.02 -95.00  30.00   54
 58  \w     92.00 119.00   0.50    0.66    --   84.02  45.00  60.00   54
 59  \w     53.00  78.00   0.50    0.66    --   84.02 -95.00 -30.00   50
 60  \w     66.00 119.00   0.50    0.66    --   86.00  25.00 166.13  106
 61  \w     61.00 103.00   0.50    0.66    --   86.75  19.00   5.10   84
 62  \w     65.00 103.00   0.50    0.66    --   86.75  25.00-138.79   76
 63  \w     60.00  85.00   0.50    0.66    --   86.75  18.00  34.11   50
 64  \w     69.00 115.00   0.50    0.66    --   86.75  11.00 -33.08   92
 65  \w     65.00 110.00   0.50    0.66    --   86.75  25.00  56.80   90
 66  \w     70.00 135.00   0.50    0.66    --   86.75   6.00-129.37  130
 67  \w     48.00 114.00   0.50    0.66    --   86.75  10.00 169.73  132
 68  \w     76.00 121.00   0.50    0.66    --   69.96  45.00 -30.00   90
 69  \w     -4.00  21.00   0.50    0.66    --   -6.75  61.00-180.00   50
 70  \w     10.00  39.00   0.50    0.66    --   -6.75  61.00 -90.00   58
 71  \w     -9.00  16.00   0.50    0.66    --   10.00 101.00-104.97   50
 72  \w     -9.00  16.00   0.50    0.66    --   10.00 101.00   8.39   50
 73  \w     -7.00  18.00   0.50    0.66    --   10.00  99.00 127.18   50
 74  \w      3.00  28.00   0.50    0.66    --   18.00  96.00 147.72   50
 75  \w     15.00  40.00   0.50    0.66    --   26.00  89.00  -6.16   50
 76  \w     16.00  41.00   0.50    0.66    --   26.00  88.00  79.33   50
 77  \w     13.00  38.00   0.50    0.66    --   26.00  92.00-111.52   50
 78  \w     16.00  41.00   0.50    0.66    --   26.00  88.00 159.76   50
 79  \w     28.00  53.00   0.50    0.66    --   30.00  75.00  49.72   50
 80  \w     31.00  56.00   0.50    0.66    --   34.00  77.00 -64.19   50
 81  \w     31.00  56.00   0.50    0.66    --   34.00  77.00 123.79   50
 82  \w     32.00  57.00   0.50    0.66    --   34.00  74.00  94.56   50
 83  \w     38.00  63.00   0.50    0.66    --   38.00  72.00  73.94   50
 84  \w     39.00  64.00   0.50    0.66    --   38.00  68.00 172.21   50
 85  \w     36.00  62.00   0.50    0.66    --   38.00  75.00-116.51   52
 86  \w     35.00  60.00   0.50    0.66    --   38.00  77.00-152.10   50
 87  \w     40.00  65.00   0.50    0.66    --   42.00  75.00 167.82   50
 88  \w     43.00  68.00   0.50    0.66    --   42.00  69.00  -0.98   50
 89  \w     40.00  65.00   0.50    0.66    --   42.00  75.00  15.74   50
 90  \w     44.00  69.00   0.50    0.66    --   46.00  74.00  41.66   50
 91  \w     48.00  73.00   0.50    0.66    --   46.00  66.00-151.55   50
 92  \w     43.00  68.00   0.50    0.66    --   46.00  76.00 -52.88   50
 93  \w     47.00  72.00   0.50    0.66    --   46.00  69.00-179.84   50
 94  \w     44.00  69.00   0.50    0.66    --   46.00  75.00 -80.50   50
 95  \w     47.00  72.00   0.50    0.66    --   50.00  76.00  99.69   50
 96  \w     48.00  73.00   0.50    0.66    --   50.00  74.00-111.48   50
 97  \w     48.00  73.00   0.50    0.66    --   50.00  74.00  74.98   50
 98  \w     48.00  92.00   0.50    0.66    --   50.00  74.00 125.52   88
 99  \w     47.00  72.00   0.50    0.66    --   50.00  77.00  -0.97   50
100  \w     49.00  74.00   0.50    0.66    --   50.00  73.00 133.58   50
101  \w     52.00  77.00   0.50    0.66    --   54.00  74.00  66.64   50
102  \w     54.00  79.00   0.50    0.66    --   54.00  72.00 139.99   50
103  \w     52.00  77.00   0.50    0.66    --   54.00  74.00-149.21   50
104  \w     53.00  78.00   0.50    0.66    --   54.00  73.00 -36.37   50
105  \w     57.00  96.00   0.50    0.66    --   54.00  60.00 173.44   78
106  \w      4.00  29.00   0.50    0.66    --   57.25 -30.00  30.00   50
107  \w     60.00  85.00   0.50    0.66    --   57.25  61.00  90.00   50
108  \w     22.00  72.00   0.50    0.66    --   57.25  15.00  90.00  100
109  \w     65.00  98.00   0.50    0.66    --   57.25  61.00-120.00   66
110  \w     76.00 105.00   0.50    0.66    --   57.25  15.00  90.00   58
111  \w     63.00  92.00   0.50    0.66    --   57.25  61.00 150.00   58
112  \w     10.00  36.00   0.50    0.66    --   57.25 -30.00   0.00   52
113  \w     58.00  83.00   0.50    0.66    --   58.00  71.00  27.47   50
114  \w     58.00  83.00   0.50    0.66    --   58.00  71.00 -83.59   50
115  \w     59.00  84.00   0.50    0.66    --   58.00  68.00  61.53   50
116  \w     60.00  85.00   0.50    0.66    --   58.00  65.00 -58.53   50
117  \w     58.00  83.00   0.50    0.66    --   58.00  72.00 -32.08   50
118  \w     63.00 103.00   0.50    0.66    --   62.00  70.00-105.05   80
119  \w     62.00  87.00   0.50    0.66    --   62.00  71.00 -57.59   50
120  \w     61.00  86.00   0.50    0.66    --   62.00  73.00 -28.51   50
121  \w     63.00  88.00   0.50    0.66    --   62.00  70.00 172.77   50
122  \w     64.00  89.00   0.50    0.66    --   66.00  74.00  97.64   50
123  \w     64.00  89.00   0.50    0.66    --   66.00  74.00  90.68   50
124  \w     65.00  91.00   0.50    0.66    --   66.00  74.00 -15.20   52
125  \w     64.00  89.00   0.50    0.66    --   66.00  74.00 174.91   50
126  \w     66.00 102.00   0.50    0.66    --   66.00  73.00-165.12   72
127  \w     66.00  92.00   0.50    0.66    --   66.00  74.00  83.75   52
128  \w     70.00 107.00   0.50    0.66    --   69.96  30.00 -30.00   74
129  \w     19.00  49.00   0.50    0.66    --   69.96 -45.00  60.00   60
130  \w     19.00  44.00   0.50    0.66    --   69.96 -45.00  30.00   50
131  \w     89.00 114.00   0.50    0.66    --   84.02  45.00 -30.00   50
132  \w     70.00  96.00   0.50    0.66    --   84.02 178.00 -30.00   52
133  \w     67.00 100.00   0.50    0.66    --   84.02 178.00 -60.00   66
134  \w     89.00 114.00   0.50    0.66    --   84.02  45.00 150.00   50
135  \w     89.00 114.00   0.50    0.66    --   84.02  45.00-120.00   50
136  \w     65.00  98.00   0.50    0.66    --   84.02 178.00 120.00   66
137  \w     89.00 129.00   0.50    0.66    --   84.02  45.00  30.00   80
138  \w     60.00  86.00   0.50    0.66    --   84.02 178.00  60.00   52
139  \w     65.00 103.00   0.50    0.66    --   84.02 178.00 -90.00   76
140  \w     63.00  98.00   0.50    0.66    --   84.02 178.00-120.00   70
141  \w     68.00 109.00   0.50    0.66    --   84.02 178.00-150.00   82
142  \w    100.00 125.00   0.50    0.66    --   84.02 132.00-150.00   50
143  \w     89.00 114.00   0.50    0.66    --   84.02  45.00 120.00   50
144  \w     89.00 114.00   0.50    0.66    --   84.02  45.00  90.00   50
145  \w     89.00 114.00   0.50    0.66    --   84.02  45.00  60.00   50
146  \w     93.00 119.00   0.50    0.66    --   84.02 137.00  26.00   52
147  \w     89.00 114.00   0.50    0.66    --   84.02  45.00 -60.00   50
148  \w     37.00  62.00   0.50    0.66    --   84.02 -61.00 -60.00   50
149  \w     38.00  63.00   0.50    0.66    --   84.02-111.00 -30.00   50
150  \w     73.00  99.00   0.50    0.66    --   84.02 178.00  90.00   52
151  \w     89.00 114.00   0.50    0.66    --   84.02  45.00   0.00   50
152  \w     79.00 124.00   0.50    0.66    --   84.02   0.00-180.00   90
153  \w     48.00  74.00   0.50    0.66    --   84.02   0.00-180.00   52
154  \w     97.00 123.00   0.50    0.66    --   86.75   4.00  84.52   52
155  \w     41.00  68.00   0.50    0.66    --   86.75 -58.00  16.80   54
156  \w     54.00  90.00   0.50    0.66    --   86.75   4.00  84.52   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0257174000
_diffrn_orient_matrix_UB_12      0.0354108000
_diffrn_orient_matrix_UB_13      0.1014461000
_diffrn_orient_matrix_UB_21      -0.1735495000
_diffrn_orient_matrix_UB_22      -0.1302302000
_diffrn_orient_matrix_UB_23      -0.0086278000
_diffrn_orient_matrix_UB_31      0.0794143000
_diffrn_orient_matrix_UB_32      -0.1050026000
_diffrn_orient_matrix_UB_33      -0.0009986000
_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  0.0273
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_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            48161
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.883
_diffrn_reflns_theta_min         2.921
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.284
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       block
_exptl_crystal_F_000             518
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         5237
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0449P)^2^+0.4651P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0810
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5061
_reflns_number_total             5237
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01345c2.cif
_cod_data_source_block           IndStar2Mn
_cod_depositor_comments
'Adding full bibliography for 7719078--7719079.cif.'
_cod_original_cell_volume        1284.033(17)
_cod_database_code               7719078
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C32 H42 Mn1'
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.360
_olex2_refinement_description
;
1.a Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C10(H10A,H10B,H10C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C13(H13A,H13B,H13C), C30(H30A,H30B,H30C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C26(H26A,H26B,H26C), C14(H14A,H14B,H14C), C12(H12A,H12B,H12C),
 C15(H15A,H15B,H15C), C27(H27A,H27B,H27C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              85846
_shelx_hkl_checksum              13158
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.802
_oxdiff_exptl_absorpt_empirical_full_min 0.677