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_7132041
_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 B2 Fe Mo2 N4 P5, 2(C H2 Cl2)'
_chemical_formula_sum            'C72 H97 B2 Cl4 Fe Mo2 N4 P5'
_chemical_formula_weight         1584.53
_chemical_name_systematic
Cp*Fe(\m3,\h5:2:2-P5)Mo2[\m,\k2-PhB(N-2,6-iPr2C6H3)2]2
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_audit_creation_date             2023-08-09
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-09 deposited with the CCDC.	2023-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.203(2)
_cell_angle_beta                 90.567(2)
_cell_angle_gamma                117.810(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7702(3)
_cell_length_b                   13.1154(3)
_cell_length_c                   24.2746(4)
_cell_measurement_reflns_used    15950
_cell_measurement_temperature    89.9(4)
_cell_measurement_theta_max      74.1630
_cell_measurement_theta_min      3.9150
_cell_volume                     3595.75(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.48a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.48a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.48a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      89.9(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.941
_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   -115.00 -21.00   0.50    4.00    --  -45.15 -57.00 -90.00  188
  2  \w    -66.00  24.00   0.50    4.00    --  -45.15  57.00  60.00  180
  3  \w    -22.00  67.00   0.50    4.00    --   45.15 -57.00-120.00  178
  4  \w     94.00 169.00   0.50   16.00    --  104.50  30.00  60.00  150
  5  \w     57.00 103.00   0.50   16.00    --  104.50 -94.00  60.00   92
  6  \w     32.00 125.00   0.50   16.00    --  104.50 -30.00-180.00  186
  7  \w     49.00  75.00   0.50   16.00    --  104.50 -77.00 150.00   52
  8  \w    112.00 168.00   0.50   16.00    --  104.50  77.00 120.00  112
  9  \w     32.00 127.00   0.50   16.00    --  104.50 -30.00  30.00  190
 10  \w     84.00 119.00   0.50   16.00    --  104.50 -77.00 150.00   70
 11  \w    104.00 176.00   0.50   16.00    --  104.50  77.00 -30.00  144
 12  \w     47.00 106.00   0.50   16.00    --  104.50 -94.00 150.00  118
 13  \w     64.00 112.00   0.50   16.00    --  104.50-125.00 -30.00   96
 14  \w     59.00 126.00   0.50   16.00    --  104.50 -45.00 -60.00  134
 15  \w     44.00 108.00   0.50   16.00    --  104.50-105.00 -14.11  128
;
_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      -0.0867956000
_diffrn_orient_matrix_UB_12      -0.0944674000
_diffrn_orient_matrix_UB_13      -0.0395245000
_diffrn_orient_matrix_UB_21      -0.0596476000
_diffrn_orient_matrix_UB_22      -0.0782346000
_diffrn_orient_matrix_UB_23      0.0494810000
_diffrn_orient_matrix_UB_31      -0.0866834000
_diffrn_orient_matrix_UB_32      0.0509162000
_diffrn_orient_matrix_UB_33      0.0042240000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            25909
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.319
_diffrn_reflns_theta_min         3.642
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.168
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.305
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.48a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       plate
_exptl_crystal_F_000             1640
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, n-hexane'
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.033
_refine_diff_density_max         1.004
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         13807
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0633P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0932
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11415
_reflns_number_total             13807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03282e2.cif
_cod_data_source_block           abs_gaus_error
_cod_original_cell_volume        3595.75(14)
_cod_database_code               7132041
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         (C20H30FeP5Mo2N2B2C20H30CH2Cl2)3
_shelx_estimated_absorpt_t_max   0.798
_shelx_estimated_absorpt_t_min   0.210
_olex2_refinement_description
;
1. 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
2.a Ternary CH refined with riding coordinates:
 C23(H23), C26(H26), C35(H35), C38(H38), C53(H53), C56(H56), C65(H65), C68(H68)
2.b Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C72(H72A,H72B)
2.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20),
 C21(H21), C31(H31), C32(H32), C33(H33), C42(H42), C43(H43), C44(H44), C45(H45),
  C46(H46), C49(H49), C50(H50), C51(H51), C61(H61), C62(H62), C63(H63)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C),
 C28(H28A,H28B,H28C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C57(H57A,
 H57B,H57C), C58(H58A,H58B,H58C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C),
 C69(H69A,H69B,H69C), C70(H70A,H70B,H70C)
;
_shelx_res_checksum              14096
_shelx_hkl_checksum              34
_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 3.773
_oxdiff_exptl_absorpt_empirical_full_min 0.590