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_7127408
_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         'C60 H72 K3 Mo6 O16.5 P3'
_chemical_formula_sum            'C60 H72 K3 Mo6 O16.5 P3'
_chemical_formula_weight         1843.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2020-02-14
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6020)
;
_audit_update_record
;
2020-08-31 deposited with the CCDC.	2020-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.9442(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   43.5147(8)
_cell_length_b                   7.94643(15)
_cell_length_c                   20.3986(3)
_cell_measurement_reflns_used    19822
_cell_measurement_temperature    122.99(13)
_cell_measurement_theta_max      74.1740
_cell_measurement_theta_min      2.6880
_cell_volume                     6925.3(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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    'SIR97  (Burla et al.,  2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122.99(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.7272
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -25.00   68.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0756  -57.0000  150.0000 93

  2 omega   35.00  123.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0756 -178.0000  150.0000 88

  3 omega   20.00  113.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0756   57.0000  -60.0000 93

  4 omega   32.00   87.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  120.0000 55

  5 omega   33.00  130.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000  120.0000 97

  6 omega   33.00  121.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000  -30.0000 88

  7 omega   82.00  170.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000  120.0000 88

  8 omega   33.00  135.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000  -30.0000 102

  9 omega   40.00   93.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000 -180.0000 53

 10 omega   27.00  141.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -15.0000  -60.0000 114

 11 omega   20.00  113.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0756   57.0000    0.0000 93

 12 omega   14.00  116.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0756   77.0000 -180.0000 102

 13 omega   20.00  113.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0756   57.0000   90.0000 93

 14 omega   79.00  174.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   61.0000 -120.0000 95

 15 omega   82.00  173.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000  -60.0000 91

 16 omega   79.00  174.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   61.0000 -180.0000 95

 17 omega   74.00  176.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   77.0000  -30.0000 102

 18 omega   74.00  176.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   77.0000   60.0000 102

 19 omega   82.00  173.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000   30.0000 91

 20 omega  -50.00   27.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -44.0756   38.0000    0.0000 77

 21 omega   14.00  116.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0756   77.0000 -120.0000 102

 22 omega   20.00  113.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0756   57.0000  150.0000 93

 23 omega   79.00  174.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   61.0000 -150.0000 95

 24 omega   23.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000   60.0000 86

 25 omega   74.00  176.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   77.0000   30.0000 102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0214671000
_diffrn_orient_matrix_UB_12      -0.0170921000
_diffrn_orient_matrix_UB_13      -0.0516397000
_diffrn_orient_matrix_UB_21      -0.0289463000
_diffrn_orient_matrix_UB_22      -0.0048517000
_diffrn_orient_matrix_UB_23      -0.0566925000
_diffrn_orient_matrix_UB_31      0.0011720000
_diffrn_orient_matrix_UB_32      0.1930610000
_diffrn_orient_matrix_UB_33      -0.0059766000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0796
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            53433
_diffrn_reflns_point_group_measured_fraction_full 0.914
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.437
_diffrn_reflns_theta_min         2.723
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'GV50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.430
_exptl_absorpt_correction_T_max  0.484
_exptl_absorpt_correction_T_min  0.056
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_description       plate
_exptl_crystal_F_000             3672
_exptl_crystal_size_max          0.4084
_exptl_crystal_size_mid          0.387
_exptl_crystal_size_min          0.0787
_refine_diff_density_max         1.066
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.274(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1116
_refine_ls_number_reflns         12674
_refine_ls_number_restraints     562
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0811P)^2^+10.1942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1196
_reflns_Friedel_coverage         0.680
_reflns_Friedel_fraction_full    0.813
_reflns_Friedel_fraction_max     0.786
_reflns_number_gt                11748
_reflns_number_total             12674
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06150f2.cif
_cod_data_source_block           abs
_cod_depositor_comments
'Adding full bibliography for 7127408--7127410.cif.'
_cod_original_formula_sum        'C60 H72 K3 Mo6 O16.50 P3'
_cod_database_code               7127408
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C53 H40 K3 Mo6 O14 P3'
_shelx_estimated_absorpt_t_max   0.467
_shelx_estimated_absorpt_t_min   0.089
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.726(18)
 0.274(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 P3-H3A = P3-H3B = P2-H2B = P2-H2A = P1-H1B = P1-H1A
 1.4 with sigma of 0.02
 O17-C59 = O17-C62
 1.44 with sigma of 0.02
 C60-C61
 1.54 with sigma of 0.02
 C59-C60 = C61-C62
 1.53 with sigma of 0.02
 O17-C60 = O17-C61 = C59-C61 = C60-C62
 2.38 with sigma of 0.04
 O13A-C43A \\sim O13B-C43B \\sim O13A-C46A \\sim O13B-C46B
 with sigma of 0.02
 C43B-C44B \\sim C45A-C46A \\sim C44B-C45B \\sim C45B-C46B \\sim C43A-C44A
\\sim C44A-C45A
 with sigma of 0.02
 O16A-C55A \\sim O16B-C58B \\sim O16B-C55B \\sim O16A-C58A
 with sigma of 0.02
 C56A-C55A \\sim C58B-C57B \\sim C57A-C56A \\sim C57B-C56B \\sim C56B-C55B
\\sim C58A-C57A
 with sigma of 0.02
 C59-C60 \\sim C60-C61 \\sim C61-C62
 with sigma of 0.02
 O17-C59 \\sim O17-C62
 with sigma of 0.02
 O17-C60 \\sim O17-C61
 with sigma of 0.04
 C60-C62 \\sim C59-C61
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
C41A \\sim C40A \\sim C42A \\sim C38A \\sim C39A \\sim C38B \\sim C42B \\sim
C41B \\sim C40B \\sim C39B: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
C46B \\sim C43A \\sim C44A \\sim C45B \\sim C45A \\sim C44B \\sim C43B \\sim
C46A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 1.7A
C53B \\sim C51A \\sim O15A \\sim C54B: within 1.7A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 1.7A
C29B \\sim C29A \\sim O9B \\sim O9A: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
C37A \\sim C37B \\sim O12B \\sim O12A: within 1.7A with sigma of 0.02 and sigma
for terminal atoms of 0.02 within 1.7A
C58A \\sim C55A \\sim C55B \\sim C58B \\sim C57A \\sim C56A \\sim C57B \\sim
C56B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 1.7A
O17 \\sim C59 \\sim C60 \\sim C61 \\sim C62: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O13A \\sim O13B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
C47B \\sim O14A \\sim O14B \\sim C50B \\sim C48B \\sim C50A: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
C62 \\sim O17: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
Uanis(C40B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 O17, C59, C60, C61, C62
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: K3A(0.56) C37A(0.56) O9B(0.44) C41A(0.56) H41A(0.56) C40A(0.56)
 H40A(0.56) C42A(0.56) H42A(0.56) C38A(0.56) H38A(0.56) C39A(0.56) H39A(0.56)
 K3B(0.44) O9A(0.56) C29A(0.56) C29B(0.44) C38B(0.44) H38B(0.44) C42B(0.44)
 H42B(0.44) C41B(0.44) H41B(0.44) C40B(0.44) H40B(0.44) C39B(0.44) H39B(0.44)
 O12A(0.56) C37B(0.44) O12B(0.44) O16A(0.56) C55A(0.56) H55A(0.56) H55B(0.56)
 C56A(0.56) H56A(0.56) H56B(0.56) C57A(0.56) H57A(0.56) H57B(0.56) C58A(0.56)
 H58A(0.56) H58B(0.56) O15A(0.54) C54A(0.54) H54A(0.54) H54B(0.54) C53A(0.54)
 H53A(0.54) H53B(0.54) C52A(0.54) H52A(0.54) H52B(0.54) C51A(0.54) H51A(0.54)
 H51B(0.54) O15B(0.46) C51B(0.46) H51C(0.46) H51D(0.46) C52B(0.46) H52C(0.46)
 H52D(0.46) C53B(0.46) H53C(0.46) H53D(0.46) C54B(0.46) H54C(0.46) H54D(0.46)
 O16B(0.44) C55B(0.44) H55C(0.44) H55D(0.44) C56B(0.44) H56C(0.44) H56D(0.44)
 C57B(0.44) H57C(0.44) H57D(0.44) C58B(0.44) H58C(0.44) H58D(0.44) O14A(0.56)
 C47A(0.56) H47A(0.56) H47B(0.56) C48A(0.56) H48A(0.56) H48B(0.56) C49A(0.56)
 H49A(0.56) H49B(0.56) C50A(0.56) H50A(0.56) H50B(0.56) O14B(0.44) C47B(0.44)
 H47C(0.44) H47D(0.44) C48B(0.44) H48C(0.44) H48D(0.44) C49B(0.44) H49C(0.44)
 H49D(0.44) C50B(0.44) H50C(0.44) H50D(0.44) O13A(0.56) C46A(0.56) H46A(0.56)
 H46B(0.56) C45A(0.56) H45A(0.56) H45B(0.56) C44A(0.56) H44A(0.56) H44B(0.56)
 C43A(0.56) H43A(0.56) H43B(0.56) O13B(0.44) C46B(0.44) H46C(0.44) H46D(0.44)
 C45B(0.44) H45C(0.44) H45D(0.44) C44B(0.44) H44C(0.44) H44D(0.44) C43B(0.44)
 H43C(0.44) H43D(0.44) O17(0.5) C59(0.5) H59A(0.5) H59B(0.5) C60(0.5) H60A(0.5)
 H60B(0.5) C61(0.5) H61A(0.5) H61B(0.5) C62(0.5) H62A(0.5) H62B(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C55A(H55A,H55B), C56A(H56A,H56B), C57A(H57A,H57B), C58A(H58A,H58B), C54A(H54A,
 H54B), C53A(H53A,H53B), C52A(H52A,H52B), C51A(H51A,H51B), C51B(H51C,H51D),
 C52B(H52C,H52D), C53B(H53C,H53D), C54B(H54C,H54D), C55B(H55C,H55D), C56B(H56C,
 H56D), C57B(H57C,H57D), C58B(H58C,H58D), C47A(H47A,H47B), C48A(H48A,H48B),
 C49A(H49A,H49B), C50A(H50A,H50B), C47B(H47C,H47D), C48B(H48C,H48D), C49B(H49C,
 H49D), C50B(H50C,H50D), C46A(H46A,H46B), C45A(H45A,H45B), C44A(H44A,H44B),
 C43A(H43A,H43B), C46B(H46C,H46D), C45B(H45C,H45D), C44B(H44C,H44D), C43B(H43C,
 H43D), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C10(H10), C4(H4), C6(H6), C21(H21), C7(H7), C24(H24),
 C25(H25), C34(H34), C11(H11), C13(H13), C27(H27), C12(H12), C19(H19), C20(H20),
  C33(H33), C32(H32), C26(H26), C31(H31), C17(H17), C28(H28), C35(H35),
 C14(H14), C18(H18), C41A(H41A), C40A(H40A), C42A(H42A), C38A(H38A), C39A(H39A),
  C38B(H38B), C42B(H42B), C41B(H41B), C40B(H40B), C39B(H39B)
;
_shelx_res_checksum              95741
_olex2_submission_special_instructions 'No special instructions were received'