Cyclo-E5-bridged Trinuclear Triple-decker Complexes (E = P, As) Containing a Triply-bonded Mo2 Unit and Their Isomerisation
Lee, Meng-Wei; Balazs, Gabor; Reichl, Stephan; Zimmermann, Lisa; Scheer, Manfred; Tsai, Yi-Chou; Chemical Communications  (2023) –; doi:10.1039/D3CC03282E

data_7132042
_publ_section_title
;
 Cyclo-E5-bridged Trinuclear Triple-decker Complexes (E = P, As)
 Containing a Triply-bonded Mo2 Unit and Their Isomerisation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03282E
_journal_year                    2023
_chemical_formula_moiety         'C70 H93 As5 B2 Fe Mo2 N4, C4 H8 O, 0.3[C4H8O]'
_chemical_formula_sum            'C75.2 H103.4 As5 B2 Fe Mo2 N4 O1.3'
_chemical_formula_weight         1728.16
_chemical_name_systematic
Cp*Fe(\m3,\h5:2:2-As5)Mo2[\m,\k2-PhB(N-2,6-iPr2C6H3)2]2
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-02
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2023-07-07 deposited with the CCDC.	2023-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.7410(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.4267(2)
_cell_length_b                   12.75610(10)
_cell_length_c                   48.9677(5)
_cell_measurement_reflns_used    21336
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      67.8410
_cell_measurement_theta_min      3.6650
_cell_volume                     14602.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.951
_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     -5.00  31.00   0.25   15.00    --  -43.39  19.00-180.00  144
  2  \w      0.00  26.00   0.25   15.00    --  -43.39  19.00-150.00  104
  3  \w   -120.00 -10.00   0.25   15.00    --  -43.39 -19.00-150.00  440
  4  \w     25.00  57.00   0.25   60.00    --   91.74 -30.00 -30.00  128
  5  \w     13.00  45.00   0.25   60.00    --   91.74 -15.00   0.00  128
  6  \w     40.00  74.00   0.25   60.00    --   91.74-125.00  30.00  136
  7  \w     25.00  91.00   0.25   60.00    --   91.74 -61.00 -90.00  264
  8  \w     87.00 112.00   0.25   60.00    --   91.74-125.00  30.00  100
  9  \w     34.00 164.00   0.25   60.00    --   91.74   0.00-180.00  520
 10  \w     22.00  69.00   0.25   60.00    --   91.74 -45.00-150.00  188
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0065575000
_diffrn_orient_matrix_UB_12      0.0127782000
_diffrn_orient_matrix_UB_13      0.0278623000
_diffrn_orient_matrix_UB_21      0.0551346000
_diffrn_orient_matrix_UB_22      -0.0381243000
_diffrn_orient_matrix_UB_23      0.0058374000
_diffrn_orient_matrix_UB_31      0.0215513000
_diffrn_orient_matrix_UB_32      0.1014341000
_diffrn_orient_matrix_UB_33      -0.0013651000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\b'
_diffrn_radiation_wavelength     1.39222
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            32515
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        56.650
_diffrn_reflns_theta_max         67.720
_diffrn_reflns_theta_min         3.688
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.376
_exptl_absorpt_correction_T_max  0.68973
_exptl_absorpt_correction_T_min  0.67082
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       sphere
_exptl_crystal_F_000             7024
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_exptl_crystal_size_rad          0.048
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     824
_refine_ls_number_reflns         32515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0704P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1026
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25936
_reflns_number_total             32515
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9580\% 
around [-0.03 1.00 -0.01] (reciprocal) or [-0.01 1.00 -0.00] (direct)
;
_cod_data_source_file            d3cc03282e2.cif
_cod_data_source_block           res462_cub2_twin1_hklf4
_cod_original_formula_sum        'C75.20 H103.40 As5 B2 Fe Mo2 N4 O1.30'
_cod_database_code               7132042
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C78H70B2N4O2FeAs5Mo2
_shelx_estimated_absorpt_t_max   0.814
_shelx_estimated_absorpt_t_min   0.480
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5676(4)
 0.4324(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C40(H40), C60(H60), C72(H72), C39(H39), C23(H23), C47(H47), C25(H25), C53(H53)
3.b Secondary CH2 refined with riding coordinates:
 C69(H69A,H69B), C35(H35A,H35B), C71(H71A,H71B), C9(H9A,H9B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C22(H22), C48(H48), C50(H50), C54(H54), C56(H56),
 C64(H64), C66(H66), C68(H68), C70(H70), C74(H74), C19(H19), C5(H5), C41(H41),
 C43(H43), C27(H27), C7(H7), C57(H57), C59(H59), C61(H61)
3.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C42(H42A,H42B,H42C), C46(H46A,H46B,H46C), C21(H21A,H21B,
 H21C), C11(H11A,H11B,H11C), C45(H45A,H45B,H45C), C3(H3A,H3B,H3C), C49(H49A,
 H49B,H49C), C51(H51A,H51B,H51C), C13(H13A,H13B,H13C), C55(H55A,H55B,H55C),
 C29(H29A,H29B,H29C), C15(H15A,H15B,H15C), C31(H31A,H31B,H31C), C63(H63A,H63B,
 H63C), C2(H2A,H2B,H2C), C65(H65A,H65B,H65C), C33(H33A,H33B,H33C), C67(H67A,
 H67B,H67C), C17(H17A,H17B,H17C), C73(H73A,H73B,H73C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 104 electrons were 
found in a volume of 480\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.3[C4H8O] per Asymmetric Unit 
which account for 96 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.4
_smtbx_masks_void_truncation_radius 1.0
_shelx_res_checksum              32348
_shelx_hkl_checksum              9725
_shelx_fab_checksum              99143
_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 1.404
_oxdiff_exptl_absorpt_empirical_full_min 0.850
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_publcif_funding_html
;
;