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_7127409
_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         'C19 H30 O2 P4 Ta, C16 H31 Li O4'
_chemical_formula_sum            'C35 H61 Li O6 P4 Ta'
_chemical_formula_weight         889.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 94.0170(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.86250(10)
_cell_length_b                   21.7618(3)
_cell_length_c                   16.0909(2)
_cell_measurement_reflns_used    16553
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      74.0890
_cell_measurement_theta_min      3.4010
_cell_volume                     4143.65(8)
_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      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.970
_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   -113.00 -21.00   1.00    5.00    --  -44.58 -57.00  60.00   92
  2  \w    -69.00  25.00   1.00    5.00    --  -44.58  57.00-150.00   94
  3  \w     34.00 131.00   1.00    5.00    --   44.58-178.00  60.00   97
  4  \w     27.00 141.00   1.00   30.00    --  104.50 -15.00 -30.00  114
  5  \w     23.00 109.00   1.00   30.00    --  104.50 -94.00 120.00   86
  6  \w     32.00  91.00   1.00   30.00    --  104.50 -30.00-180.00   59
  7  \w     82.00 173.00   1.00   30.00    --  104.50  45.00 150.00   91
  8  \w     32.00  91.00   1.00   30.00    --  104.50 -30.00-120.00   59
  9  \w     32.00  91.00   1.00   30.00    --  104.50 -30.00 120.00   59
 10  \w     23.00 109.00   1.00   30.00    --  104.50 -94.00  30.00   86
 11  \w     33.00 135.00   1.00   30.00    --  104.50 -77.00-150.00  102
 12  \w   -113.00 -21.00   1.00    5.00    --  -44.58 -57.00 120.00   92
;
_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      0.0138986000
_diffrn_orient_matrix_UB_12      0.0629281000
_diffrn_orient_matrix_UB_13      -0.0418616000
_diffrn_orient_matrix_UB_21      0.1203521000
_diffrn_orient_matrix_UB_22      0.0053674000
_diffrn_orient_matrix_UB_23      0.0419965000
_diffrn_orient_matrix_UB_31      0.0476471000
_diffrn_orient_matrix_UB_32      -0.0319580000
_diffrn_orient_matrix_UB_33      -0.0754895000
_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  0.1071
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27131
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.316
_diffrn_reflns_theta_min         3.421
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'GV50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.664
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25310
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.54a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       plate
_exptl_crystal_F_000             1820
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.009
_refine_diff_density_min         -2.103
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         8180
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0949P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1366
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7348
_reflns_number_total             8180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06150f2.cif
_cod_data_source_block           fr073_mp_
_cod_depositor_comments
'Adding full bibliography for 7127408--7127410.cif.'
_cod_database_code               7127409
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C35 H62 Ta O3 P4 Li'
_shelx_estimated_absorpt_t_max   0.691
_shelx_estimated_absorpt_t_min   0.106
_reflns_odcompleteness_completeness 99.46
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C33A-C32A \\sim C33B-C32B \\sim C33A-C34A \\sim C34A-C35A \\sim C34B-C35B
 with sigma of 0.02
 O4A-C32A \\sim O4B-C32B \\sim O4A-C35A \\sim O4B-C35B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C32B \\sim O4B \\sim O4A \\sim C32A \\sim C33A \\sim C33B \\sim C34A \\sim C34B
\\sim C35A \\sim C35B: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.7A
4. Others
 Sof(H26C)=Sof(H26D)=Sof(C27B)=Sof(H27C)=Sof(H27D)=1-FVAR(1)
 Sof(H26A)=Sof(H26B)=Sof(C27A)=Sof(H27A)=Sof(H27B)=FVAR(1)
 Fixed Sof: O4A(0.52) C35A(0.52) H35A(0.52) H35B(0.52) C32A(0.52) H32A(0.52)
 H32B(0.52) C33A(0.52) H33A(0.52) H33B(0.52) C34A(0.52) H34A(0.52) H34B(0.52)
 O4B(0.48) C32B(0.48) H32C(0.48) H32D(0.48) C33B(0.48) H33C(0.48) H33D(0.48)
 C34B(0.48) H34C(0.48) H34D(0.48) C35B(0.48) H35C(0.48) H35D(0.48)
5.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C23(H23A,H23B), C30(H30A,H30B), C20(H20A,H20B), C29(H29A,
 H29B), C21(H21A,H21B), C28(H28A,H28B), C22(H22A,H22B), C26(H26A,H26B),
 C26(H26C,H26D), C25(H25A,H25B), C27A(H27A,H27B), C27B(H27C,H27D), C35A(H35A,
 H35B), C32A(H32A,H32B), C33A(H33A,H33B), C34A(H34A,H34B), C32B(H32C,H32D),
 C33B(H33C,H33D), C34B(H34C,H34D), C35B(H35C,H35D)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C5(H5), C4(H4), C24(H24)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C15(H15A,H15B,H15C), C9(H9A,H9B,
 H9C), C18(H18A,H18B,H18C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C11(H11A,
 H11B,H11C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              78343
_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 5.296
_oxdiff_exptl_absorpt_empirical_full_min 0.152