An acetylene-bridged ferrocene macrocycle: efficient synthesis and electron transfer mechanism in mixed-valence systems.
Li, Longfei; Zhang, Beijing; Xie, Yi; Xiong, Qi; Zhong, Yuanbo; Jiang, Yansong; Wang, Yu; Wang, Haobing; Jiang, Shang-Da; Zhou, Shen; Jiang, Xing; Chemical science 16 (2025) 17268–17275; doi:10.1039/d5sc02322j

data_1575547
_publ_section_title
;
 An acetylene-bridged ferrocene macrocycle: efficient synthesis and
 electron transfer mechanism in mixed-valence systems.
;
_journal_issue                   37
_journal_name_full               'Chemical science'
_journal_page_first              17268
_journal_page_last               17275
_journal_paper_doi               10.1039/d5sc02322j
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C36 H30 Fe3, C H2 Cl2'
_chemical_formula_sum            'C37 H32 Cl2 Fe3'
_chemical_formula_weight         715.07
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-05-12
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-05-23 deposited with the CCDC.	2025-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                78.104(13)
_cell_angle_beta                 64.935(15)
_cell_angle_gamma                60.235(14)
_cell_formula_units_Z            2
_cell_length_a                   11.8646(16)
_cell_length_b                   11.9852(17)
_cell_length_c                   13.0247(18)
_cell_measurement_reflns_used    3916
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.4260
_cell_measurement_theta_min      2.1050
_cell_volume                     1456.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.44.91a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 42.73a 64-bit (release 27-10-2022))'
_computing_data_reduction        'CrysAlisPro 1.171.44.91a (Rigaku OD, 2025)'
_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      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.704
_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    -76.00   6.00   0.50    1.50    --   -4.93 -48.00  69.00  164
  2  \w    -14.00  31.00   0.50    1.50    --    4.00 -99.00   0.00   90
  3  \w      9.00  34.00   0.50    1.50    --    4.00 -99.00 -30.00   50
  4  \w    -12.00  15.00   0.50    1.50    --    4.00 -99.00-180.00   54
  5  \w    -16.00  67.00   0.50    1.50    --   -4.93  48.00-142.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0324438000
_diffrn_orient_matrix_UB_12      -0.0324736000
_diffrn_orient_matrix_UB_13      -0.0074706000
_diffrn_orient_matrix_UB_21      0.0103886000
_diffrn_orient_matrix_UB_22      0.0234230000
_diffrn_orient_matrix_UB_23      -0.0558840000
_diffrn_orient_matrix_UB_31      0.0663335000
_diffrn_orient_matrix_UB_32      -0.0552102000
_diffrn_orient_matrix_UB_33      -0.0209017000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0971
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.704
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10851
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.704
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.373
_diffrn_reflns_theta_min         1.957
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.685
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.91a (Rigaku Oxford Diffraction, 2025)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             732
_exptl_crystal_recrystallization_method
'The crystals were growth by means of evaporation of a mixture of n-hexane and toluene at RT.'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.367
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         10851
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0639
_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^)+(0.1429P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1714
_refine_ls_wR_factor_ref         0.1790
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9151
_reflns_number_total             10851
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9257\% 
around [-0.00 1.00 -0.03] (reciprocal) or [-0.45 0.89 -0.00] (direct)
;
_cod_data_source_file            d5sc02322j2.cif
_cod_data_source_block           vinylfc3mer_twin1_hklf5
_cod_depositor_comments
'Adding full bibliography for 1575546--1575548.cif.'
_cod_database_code               1575547
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         FeCH
_shelx_estimated_absorpt_t_max   0.850
_shelx_estimated_absorpt_t_min   0.811
_exptl_crystal_mounting_method
;
 Crystals were removed from the crystallisation vial and immediately
 coated with polybutenes oil (CAS: 9003-29-6) on a glass slide.
 A suitable single crystal coated with polybutenes oil as less as possible
 was sealed in capillary tube filled with argon. The capillary tube with
 single crystal was mounted on copper pin with solid paraffin.
;
_diffrn_oxdiff_digest_od_ed
;

;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.58889
 0.41111
2.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C10(H10), C21(H21), C14(H14), C15(H15), C35(H35), C16(H16), C3(H3),
 C12(H12), C11(H11), C2(H2), C33(H33), C1(H1), C9(H9), C24(H24), C22(H22),
 C18(H18), C25(H25), C4(H4), C26(H26), C19(H19), C23(H23), C34(H34), C36(H36),
 C27(H27), C28(H28), C31(H31), C7(H7), C30(H30), C6(H6)
;
_shelx_res_checksum              73945
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.446
_oxdiff_exptl_absorpt_empirical_full_min 0.326
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2