<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_7719314
_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 O2 Sr, 3(C4 H8 O)'
_chemical_formula_sum            'C80 H84 O5 Sr'
_chemical_formula_weight         1213.09
_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             2022-07-26
_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                 108.83(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.920(3)
_cell_length_b                   18.590(4)
_cell_length_c                   13.900(3)
_cell_measurement_reflns_used    11830
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     3159.9(13)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            56524
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         1.548
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       block
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 5118 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0034(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         11830
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0782P)^2^+0.6416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1064
_reflns_Friedel_coverage         0.916
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                11303
_reflns_number_total             11830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01881a2.cif
_cod_data_source_block           merge
_cod_depositor_comments
'Adding full bibliography for 7719312--7719315.cif.'
_cod_original_cell_volume        3159.8(12)
_cod_database_code               7719314
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.854
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H17(0.041) H45(0.047) H30A(0.038) H30B(0.038) H10(0.047)
 H38(0.042) H11(0.042) H28(0.047) H42(0.044) H44(0.041) H31A(0.038) H31B(0.038)
 H46(0.048) H14(0.048) H62A(0.05) H62B(0.05) H8(0.045) H16(0.044) H9(0.044)
 H13(0.042) H29(0.042) H40(0.056) H7(0.04) H39(0.052) H65A(0.05) H65B(0.05)
 H47(0.046) H41(0.052) H21(0.049) H63A(0.052) H63B(0.052) H26(0.052) H50(0.043)
 H60(0.043) H19(0.044) H51(0.049) H54(0.049) H27(0.052) H68A(0.051) H68B(0.051)
 H25(0.045) H58(0.052) H48(0.042) H59(0.05) H22(0.048) H15(0.046) H23(0.044)
 H57(0.054) H20(0.047) H66A(0.049) H66B(0.049) H61A(0.046) H61B(0.046)
 H53(0.057) H67A(0.056) H67B(0.056) H64A(0.049) H64B(0.049) H56(0.047)
 H52(0.055) H69A(0.079) H69B(0.079) H70A(0.095) H70B(0.095) H72A(0.088)
 H72B(0.088) H73A(0.121) H73B(0.121) H71A(0.13) H71B(0.13) H75A(0.092)
 H75B(0.092) H74A(0.12) H74B(0.12) H76A(0.089) H76B(0.089) H77A(0.097)
 H77B(0.097) H78A(0.098) H78B(0.098) H79A(0.18) H79B(0.18) H80A(0.17) H80B(0.17)
 Fixed X: H17(0.274319) H45(-0.23359) H30A(0.376534) H30B(0.467652)
 H10(0.255789) H38(0.202146) H11(0.251327) H28(0.371547) H42(0.085614) H44(-
 0.072809) H31A(0.330957) H31B(0.31994) H46(-0.355363) H14(0.502426) H62A(-
 0.044653) H62B(0.062477) H8(0.508272) H16(0.285354) H9(0.383406) H13(0.491554)
 H29(0.304577) H40(0.187039) H7(0.504503) H39(0.232237) H65A(-0.091643) H65B(-
 0.060409) H47(-0.312079) H41(0.112654) H21(0.536394) H63A(0.156351)
 H63B(0.046235) H26(0.645488) H50(-0.145634) H60(0.239303) H19(0.543422) H51(-
 0.292348) H54(-0.010748) H27(0.540842) H68A(0.171587) H68B(0.066214)
 H25(0.579352) H58(0.260987) H48(-0.146758) H59(0.294466) H22(0.38743)
 H15(0.397697) H23(0.320606) H57(0.179395) H20(0.612385) H66A(-0.130783) H66B(-
 0.042181) H61A(-0.085853) H61B(-0.041245) H53(-0.153241) H67A(0.079291) H67B(-
 0.005488) H64A(0.185625) H64B(0.064297) H56(0.129919) H52(-0.293422) H69A(-
 0.28452) H69B(-0.325947) H70A(-0.498737) H70B(-0.453402) H72A(-0.404952) H72B(-
 0.462203) H73A(0.294212) H73B(0.331588) H71A(-0.568294) H71B(-0.490959)
 H75A(0.017358) H75B(0.059949) H74A(0.195358) H74B(0.183011) H76A(0.066978)
 H76B(0.076495) H77A(-0.010242) H77B(-0.031771) H78A(-0.116577) H78B(-0.189233)
 H79A(-0.190139) H79B(-0.296835) H80A(-0.264606) H80B(-0.215112)
 Fixed Y: H17(0.21811) H45(0.515496) H30A(0.562575) H30B(0.558739)
 H10(0.425405) H38(0.634624) H11(0.384155) H28(0.440992) H42(0.431699)
 H44(0.552816) H31A(0.557994) H31B(0.628222) H46(0.438885) H14(0.213986)
 H62A(0.25158) H62B(0.301507) H8(0.556562) H16(0.115139) H9(0.512405)
 H13(0.317476) H29(0.404644) H40(0.540903) H7(0.515995) H39(0.638823)
 H65A(0.336353) H65B(0.308128) H47(0.400739) H41(0.437729) H21(0.125287)
 H63A(0.207567) H63B(0.169818) H26(0.517394) H50(0.612377) H60(0.683575)
 H19(0.246397) H51(0.620743) H54(0.457026) H27(0.497347) H68A(0.281394)
 H68B(0.322119) H25(0.480422) H58(0.716732) H48(0.431444) H59(0.754306)
 H22(0.192625) H15(0.112403) H23(0.288736) H57(0.605249) H20(0.151908)
 H66A(0.217958) H66B(0.192134) H61A(0.298685) H61B(0.369167) H53(0.469064)
 H67A(0.17802) H67B(0.211292) H64A(0.244441) H64B(0.22135) H56(0.532444)
 H52(0.552821) H69A(0.35639) H69B(0.317828) H70A(0.34173) H70B(0.396443)
 H72A(0.226274) H72B(0.195473) H73A(0.188796) H73B(0.142066) H71A(0.284006)
 H71B(0.323837) H75A(0.169316) H75B(0.21232) H74A(0.246076) H74B(0.174508)
 H76A(0.065396) H76B(0.106358) H77A(0.343846) H77B(0.420337) H78A(0.393685)
 H78B(0.434921) H79A(0.281033) H79B(0.331825) H80A(0.346019) H80B(0.266391)
 Fixed Z: H17(0.560879) H45(0.771333) H30A(0.571316) H30B(0.68088)
 H10(0.201133) H38(0.816495) H11(0.358423) H28(1.035677) H42(0.808902)
 H44(0.746696) H31A(0.760017) H31B(0.691277) H46(0.654235) H14(0.360757)
 H62A(0.817483) H62B(0.860803) H8(0.343) H16(0.470762) H9(0.192934)
 H13(0.450011) H29(0.866764) H40(1.074681) H7(0.500069) H39(0.991316)
 H65A(0.367305) H65B(0.482675) H47(0.510569) H41(0.983046) H21(0.931977)
 H63A(0.82635) H63B(0.754434) H26(0.991664) H50(0.456363) H60(0.549381)
 H19(0.691916) H51(0.305411) H54(0.331359) H27(1.098335) H68A(0.362406)
 H68B(0.287812) H25(0.82223) H58(0.268701) H48(0.491354) H59(0.437264)
 H22(0.943114) H15(0.367386) H23(0.833218) H57(0.218375) H20(0.804038)
 H66A(0.332865) H66B(0.438089) H61A(0.655393) H61B(0.723899) H53(0.17797)
 H67A(0.355404) H67B(0.253281) H64A(0.68371) H64B(0.614976) H56(0.329624)
 H52(0.164627) H69A(0.275732) H69B(0.360344) H70A(0.275756) H70B(0.208987)
 H72A(0.099689) H72B(0.178041) H73A(1.065312) H73B(1.16825) H71A(0.135827)
 H71B(0.082398) H75A(1.087955) H75B(1.007308) H74A(1.149594) H74B(1.210736)
 H76A(1.042966) H76B(0.944495) H77A(1.036886) H77B(1.07921) H78A(0.897694)
 H78B(0.956032) H79A(0.917939) H79B(0.90007) H80A(1.075787) H80B(1.078581)
;
_shelx_res_checksum              15215
_shelx_hkl_checksum              71985
_olex2_submission_special_instructions 'No special instructions were received'