<i>Ansa</i>-effects in alkaline earth metal octaphenylmetallocenophanes and a derived <i>ansa</i>-ferrocene.
Shephard, Angus C. G.; Bouammali, Amal; Delon, Aymeric; Guo, Zhifang; Chevreux, Sylviane; Niebel, Claude; Dautel, Olivier; Simler, Thomas; Deacon, Glen B.; Junk, Peter C.; Jaroschik, Florian; Dalton transactions (Cambridge, England : 2003) 54 (2025) 13918–13928; doi:10.1039/d5dt01881a

data_7719315
_publ_section_title
;
 <i>Ansa</i>-effects in alkaline earth metal octaphenylmetallocenophanes
 and a derived <i>ansa</i>-ferrocene.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13918
_journal_page_last               13928
_journal_paper_doi               10.1039/d5dt01881a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C60 H44 Fe, 2(C4 H8 O), 0.35[C5H12]'
_chemical_formula_sum            'C69.75 H64.2 Fe O2'
_chemical_formula_weight         990.26
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-05-22
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-06-16 deposited with the CCDC.	2025-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   44.8795(7)
_cell_length_b                   44.8795(7)
_cell_length_c                   10.3923(2)
_cell_measurement_reflns_used    30447
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.39
_cell_volume                     20931.9(6)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)
;
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_details
;
 368 frames, detector distance = 80 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -59
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_k_min       -58
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            44799
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.689
_diffrn_reflns_theta_min         2.553
_diffrn_source                   Axo_Mo
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.336
_exptl_absorpt_correction_T_max  0.9521
_exptl_absorpt_correction_T_min  0.8067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             8395
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.089
_exptl_crystal_size_rad          0.088
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         12226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0573P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1111
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8412
_reflns_number_total             12226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01881a2.cif
_cod_data_source_block           ansa-fe
_cod_depositor_comments
'Adding full bibliography for 7719312--7719315.cif.'
_cod_original_cell_volume        20931.9(8)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'C69.75 H64.20 Fe O2'
_cod_database_code               7719315
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,
 H63B), C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B),
 C68(H68A,H68B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25),
  C26(H26), C27(H27), C28(H28), C29(H29), C38(H38), C39(H39), C40(H40),
 C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50),
  C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C58(H58),
 C59(H59), C60(H60)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 236 electrons were 
found in a volume of 1320\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
0.35[C5H12] per Asymmetric Unit 
which account for 235 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              89328
_shelx_hkl_checksum              99475
_shelx_fab_checksum              57688
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '80.0 mm'
_stoe_detector_pixelsize_x       '0.075 mm'
_stoe_detector_pixelsize_y       '0.075 mm'
_stoe_detector_size_x            '8.0 cm'
_stoe_detector_size_y            '7.7 cm'
_stoe_evaluation_integration_a   7.2
_stoe_evaluation_integration_b   0.1
_stoe_evaluation_integration_ems 0.011
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 90.5
_stoe_evaluation_lana_dxs_max_order 1
_stoe_evaluation_lana_dys_max_order 1
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 57.4
_stoe_evaluation_lana_max_2theta_desired 57.4
_stoe_evaluation_lana_mean_redundancy 3.7
_stoe_evaluation_lana_number_refls_after_or 44801
_stoe_evaluation_lana_number_refls_outliers 6635
_stoe_evaluation_lana_number_refls_total 51436
_stoe_evaluation_lana_number_refls_unique 12227
_stoe_evaluation_lana_number_refls_written 44801
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group 4/m
_stoe_evaluation_lana_table
;
2Theta           7.0   13.0   19.0   25.0   31.0   37.0   43.0   49.0   55.0
<Resolution>    5.06   3.02   2.12   1.64   1.32   1.11   0.97   0.86   0.79
N(total)         423   1647   3583   5363   5739   8486  10275  10723   5197
<Redundancy>     4.8    5.6    5.6    5.0    3.7    4.0    3.7    3.3    2.4
Complet. [%%]    98.6  100.0  100.0  100.0   98.9  100.0  100.0   99.5   61.1
<I/sigma>      107.6   67.8   35.5   24.4   12.7    8.3    5.5    3.0    1.9
R(int)         0.013  0.013  0.016  0.019  0.027  0.040  0.059  0.104  0.153
;
_stoe_measurement_identifier     Ansa-Fe
_stoe_measurement_max_exposure_per_frame '200.0 s'
_stoe_measurement_mean_exposure_per_frame '200.0 s'
_stoe_measurement_min_exposure_per_frame '200.0 s'
_stoe_measurement_total_exposure_time '20.4 h'
_stoe_measurement_total_frame_number 368
_stoe_measurement_total_run_number 6
_stoe_measurement_tube_power     '50.0 W'