<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_7719313
_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         'C68 H60 Ba O2, 2(C4 H8 O)'
_chemical_formula_sum            'C76 H76 Ba O4'
_chemical_formula_weight         1190.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-06-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-06-16 deposited with the CCDC.	2025-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.361(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.2111(2)
_cell_length_b                   16.1916(2)
_cell_length_c                   16.8585(3)
_cell_measurement_reflns_used    51140
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      31.6780
_cell_measurement_theta_min      3.4680
_cell_volume                     2964.62(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.902
_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    -81.00   3.00   0.50   10.00    --   -8.90 -41.00-137.00  168
  2  \w    -21.00  64.00   0.50   10.00    --   -8.90  41.00  15.00  170
  3  \w    -63.00  21.00   0.50   10.00    --    9.22 -41.00-137.00  168
  4  \w    -84.00   4.00   0.50   10.00    --   -8.90 -19.00 120.00  176
  5  \w    -23.00  25.00   0.50   10.00    --   -8.90 -99.00  60.00   96
  6  \w    -23.00  23.00   0.50   10.00    --   -8.90 -99.00  30.00   92
  7  \w     -6.00  20.00   0.50   10.00    --   -8.90 -99.00 -90.00   52
  8  \w    -22.00  25.00   0.50   10.00    --   -8.90 -99.00-120.00   94
  9  \w    -24.00  38.00   0.50   10.00    --   -8.90  57.00 150.00  124
 10  \w    -21.00  35.00   0.50   10.00    --    9.22 -99.00 150.00  112
 11  \w    -22.00   3.00   0.50   10.00    --    9.22 -99.00 120.00   50
 12  \w    -22.00  43.00   0.50   10.00    --    9.22 -99.00 -30.00  130
 13  \w    -22.00  27.00   0.50   10.00    --    9.22 -99.00 -60.00   98
 14  \w     16.00  42.00   0.50   10.00    --    9.22 -99.00 120.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            81991
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.283
_diffrn_reflns_theta_min         3.474
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       prism
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.454
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 6551 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.029(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         18149
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+0.8851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0730
_reflns_Friedel_coverage         0.849
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.814
_reflns_number_gt                15559
_reflns_number_total             18149
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01881a2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7719312--7719315.cif.'
_cod_database_code               7719313
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.931
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Others
 Sof(H76C)=Sof(H76D)=Sof(H73C)=Sof(H73D)=Sof(O4)=1-FVAR(1)
 Sof(O4A)=Sof(H76A)=Sof(H76B)=Sof(H73A)=Sof(H73B)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C64(H64A,H64B), C61(H61A,H61B), C30(H30A,H30B), C31(H31A,H31B), C65(H65A,
 H65B), C75(H75A,H75B), C66(H66A,H66B), C68(H68A,H68B), C70(H70A,H70B),
 C63(H63A,H63B), C76(H76A,H76B), C76(H76C,H76D), C69(H69A,H69B), C62(H62A,H62B),
  C73(H73A,H73B), C73(H73C,H73D), C71(H71A,H71B), C72(H72A,H72B), C74(H74A,
 H74B), C67(H67A,H67B)
3.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C29(H29), C7(H7), C39(H39), C11(H11), C25(H25), C58(H58), C38(H38),
 C59(H59), C22(H22), C10(H10), C48(H48), C42(H42), C28(H28), C20(H20), C50(H50),
  C21(H21), C26(H26), C13(H13), C60(H60), C40(H40), C27(H27), C57(H57),
 C19(H19), C53(H53), C56(H56), C8(H8), C17(H17), C47(H47), C41(H41), C54(H54),
 C52(H52), C14(H14), C9(H9), C44(H44), C46(H46), C45(H45), C51(H51), C16(H16),
 C15(H15)
;
_shelx_res_checksum              88583
_shelx_hkl_checksum              61878
_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
;