The reaction behavior of [Cp<sub>2</sub>Mo<sub>2</sub>(CO)<sub>4</sub>(μ,η<sup>2:2</sup>-P<sub>2</sub>)] and [Cp''Ta(CO)<sub>2</sub>(η<sup>4</sup>-P<sub>4</sub>)] towards hydroxide and tert-butyl nucleophiles.
Riedlberger, Felix; Seidl, Michael; Scheer, Manfred; Chemical communications (Cambridge, England) 56 (2020) 13836–13839; doi:10.1039/d0cc06150f

data_7127410
_publ_section_title
;
 The reaction behavior of
 [Cp<sub>2</sub>Mo<sub>2</sub>(CO)<sub>4</sub>(\m,\h<sup>2:2</sup>-P<sub>2</sub>)]
 and [Cp''Ta(CO)<sub>2</sub>(\h<sup>4</sup>-P<sub>4</sub>)] towards
 hydroxide and tert-butyl nucleophiles.
;
_journal_issue                   89
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13836
_journal_page_last               13839
_journal_paper_doi               10.1039/d0cc06150f
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C15 H22 O3 P4 Ta, C27 H37 N2, 1[C4H10O]'
_chemical_formula_sum            'C46 H69 N2 O4 P4 Ta'
_chemical_formula_weight         1018.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-05-14
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.05.07 svn.rd67b107b for OlexSys, GUI svn.r6105)
;
_audit_update_record
;
2020-08-31 deposited with the CCDC.	2020-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.8677(4)
_cell_length_b                   17.9409(3)
_cell_length_c                   27.8048(6)
_cell_measurement_reflns_used    16989
_cell_measurement_temperature    122.99(19)
_cell_measurement_theta_max      73.8120
_cell_measurement_theta_min      3.1420
_cell_volume                     9910.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.54a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.54a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.54a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (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      122.99(19)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_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    -64.00  23.00   1.00    7.50    --  -44.08  57.00-180.00   87
  2  \w   -110.00 -53.00   1.00    7.50    --  -44.08 -38.00   0.00   57
  3  \w     82.00 164.00   1.00   60.00    --  104.50  45.00 120.00   82
  4  \w     79.00 170.00   1.00   60.00    --  104.50  61.00 -30.00   91
  5  \w     88.00 149.00   1.00   60.00    --  104.50  30.00-120.00   61
  6  \w     55.00  82.00   1.00   60.00    --  104.50 -30.00   0.00   27
  7  \w     35.00  76.00   1.00   60.00    --  104.50 -30.00  90.00   41
  8  \w     14.00 116.00   1.00    7.50    --   44.08  77.00-180.00  102
  9  \w     20.00 113.00   1.00    7.50    --   44.08  57.00  90.00   93
 10  \w     23.00 109.00   1.00   60.00    --  104.50 -94.00 -90.00   86
 11  \w     73.00 112.00   1.00   60.00    --  104.50 125.00-120.00   39
 12  \w     36.00  96.00   1.00   60.00    --  104.50 -45.00 -60.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0548867000
_diffrn_orient_matrix_UB_12      0.0601784000
_diffrn_orient_matrix_UB_13      0.0053229000
_diffrn_orient_matrix_UB_21      0.0360933000
_diffrn_orient_matrix_UB_22      -0.0308261000
_diffrn_orient_matrix_UB_23      -0.0448080000
_diffrn_orient_matrix_UB_31      -0.0411812000
_diffrn_orient_matrix_UB_32      0.0529477000
_diffrn_orient_matrix_UB_33      -0.0321565000
_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  0.0528
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            50470
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.366
_diffrn_reflns_theta_min         3.179
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'GV50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.631
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.562
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.54a (Rigaku Oxford Diffraction, 2020)
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    1.366
_exptl_crystal_description       block
_exptl_crystal_F_000             4192
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.476
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         9939
_refine_ls_number_restraints     220
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0772
_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^)+(0.0026P)^2^+99.5728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1496
_refine_ls_wR_factor_ref         0.1519
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8929
_reflns_number_total             9939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06150f2.cif
_cod_data_source_block           fr110_op_abs
_cod_depositor_comments
'Adding full bibliography for 7127408--7127410.cif.'
_cod_database_code               7127410
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C46H69N2O5P4Ta
_shelx_estimated_absorpt_t_max   0.766
_shelx_estimated_absorpt_t_min   0.427
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 C8A-C9A \\sim C14B-C12B \\sim C10A-C8A \\sim C11A-C8A \\sim C12B-C15B \\sim
C13B-C12B
 with sigma of 0.02
 C11A-C9A \\sim C9A-C10A \\sim C10A-C11A
 with sigma of 0.02
 C10B-C8B \\sim C13A-C12A \\sim C9B-C8B \\sim C11B-C8B \\sim C15A-C12A \\sim
C8B-C14A
 with sigma of 0.02
 C8B-C3B \\sim C5A-C12A \\sim C3A-C8A \\sim C12B-C5B
 with sigma of 0.02
 C13A-C15A \\sim C15A-C14A \\sim C14A-C13A
 with sigma of 0.02
 C4A-C5A \\sim C6A-C5A \\sim C6A-C7A \\sim C7A-C3A \\sim C3A-C4A \\sim C4B-C5B
\\sim C4B-C3B \\sim C7B-C3B
 \\sim C7B-C6B \\sim C6B-C5B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C18 \\sim C17 \\sim N2: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.7A
C8A \\sim C9A \\sim C15B \\sim C12A \\sim C14A \\sim C13A \\sim C15A \\sim C11A
\\sim C12B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 1.7A
C29B \\sim C29A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
C6A \\sim C7A \\sim C3A \\sim C4A \\sim C5A \\sim C5B \\sim C3B: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
4. Others
 Sof(H28A)=Sof(C29B)=Sof(H29D)=Sof(H29E)=Sof(H29F)=1-FVAR(1)
 Sof(H28)=Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(H29C)=FVAR(1)
 Sof(C5B)=Sof(C3B)=Sof(C4B)=Sof(H4B)=Sof(C15B)=Sof(H15A)=Sof(H15B)=Sof(H15C)=
 Sof(C8B)=Sof(C6B)=Sof(H6B)=Sof(C12B)=Sof(C7B)=Sof(H7B)=Sof(C10B)=Sof(H10A)=
 Sof(H10B)=Sof(H10C)=Sof(C14B)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C13B)=
 Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=Sof(C11B)=
 Sof(H11A)=Sof(H11B)=Sof(H11C)=1-FVAR(2)
 Sof(C12A)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C15A)=Sof(H15D)=
 Sof(H15E)=Sof(H15F)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C5A)=Sof(C4A)=
 Sof(H4A)=Sof(C3A)=Sof(C7A)=Sof(H7A)=Sof(C6A)=Sof(H6A)=Sof(C11A)=Sof(H11D)=
 Sof(H11E)=Sof(H11F)=Sof(C8A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=
 Sof(H10D)=Sof(H10E)=Sof(H10F)=FVAR(2)
 Sof(Ta1B)=1-FVAR(3)
 Sof(Ta1A)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C28(H28), C28(H28A), C25(H25), C37(H37), C40(H40)
5.b Me refined with everything fixed:
 C15A(H15D,H15E,H15F)
5.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C18(H18), C35(H35), C33(H33), C34(H34), C17(H17), C4B(H4B),
 C21(H21), C23(H23), C22(H22), C6B(H6B), C7B(H7B), C4A(H4A), C7A(H7A), C6A(H6A)
5.d Idealised Me refined as rotating group:
 C15B(H15A,H15B,H15C), C26(H26A,H26B,H26C), C39(H39A,H39B,H39C), C10B(H10A,
 H10B,H10C), C30(H30A,H30B,H30C), C27(H27A,H27B,H27C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C14B(H14A,H14B,H14C), C38(H38A,H38B,H38C), C13B(H13A,H13B,
 H13C), C9B(H9BA,H9BB,H9BC), C29A(H29A,H29B,H29C), C11B(H11A,H11B,H11C),
 C29B(H29D,H29E,H29F), C13A(H13D,H13E,H13F), C14A(H14D,H14E,H14F), C11A(H11D,
 H11E,H11F), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F)
;
_smtbx_masks_void_probe_radius   1.1
_smtbx_masks_void_truncation_radius 1.1
_shelx_res_checksum              99149
_shelx_fab_checksum              384
_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 1.709
_oxdiff_exptl_absorpt_empirical_full_min 0.587