Lability of Ta-NHC adducts as a synthetic route towards heterobimetallic Ta/Rh complexes.
Srivastava, Ravi; Quadrelli, Elsje Alessandra; Camp, Clément; Dalton transactions (Cambridge, England : 2003) 49 (2020) 3120–3128; doi:10.1039/d0dt00344a

data_7703562
_publ_section_title
;
 Lability of Ta-NHC adducts as a synthetic route towards heterobimetallic
 Ta/Rh complexes.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3120
_journal_page_last               3128
_journal_paper_doi               10.1039/d0dt00344a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C43 H81 N2 O5 Si Ta, C12 H28 O4 Si'
_chemical_formula_sum            'C55 H111 N2 O9 Si2 Ta'
_chemical_formula_weight         1181.58
_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             2019-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-30 deposited with the CCDC.	2020-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                95.525(3)
_cell_angle_beta                 102.339(3)
_cell_angle_gamma                93.414(3)
_cell_formula_units_Z            2
_cell_length_a                   9.7495(4)
_cell_length_b                   16.7483(7)
_cell_length_c                   21.3697(8)
_cell_measurement_reflns_used    31353
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.8360
_cell_measurement_theta_min      3.8700
_cell_volume                     3381.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.901
_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    -43.00  65.00   1.00    4.24    --  -10.87  77.00 -30.00  108
  2  \w    -39.00  62.00   1.00    4.24    --  -10.87  57.00 120.00  101
  3  \w    -35.00  64.00   1.00    4.24    --  -10.87  37.00 -90.00   99
  4  \w    -85.00  13.00   1.00    4.24    --  -10.87 -37.00-150.00   98
  5  \w    -80.00 -10.00   1.00    4.24    --  -10.87 146.00  20.64   70
  6  \w     -4.00  53.00   1.00    4.24    --   11.65 -99.00-180.00   57
  7  \w    -45.00   2.00   1.00    4.24    --   11.65 126.00  92.00   47
  8  \w    -84.00  17.00   1.00    4.24    --  -10.87 -57.00 120.00  101
  9  \w    -85.00  13.00   1.00    4.24    --  -10.87 -37.00 -60.00   98
 10  \w    -68.00   2.00   1.00    4.24    --  -10.87 126.00-131.95   70
 11  \w    -67.00   3.00   1.00    4.24    --  -10.87 125.00 -26.68   70
 12  \w     -4.00  53.00   1.00    4.24    --   11.65 -99.00 -90.00   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0552715000
_diffrn_orient_matrix_UB_12      -0.0176392000
_diffrn_orient_matrix_UB_13      0.0198581000
_diffrn_orient_matrix_UB_21      -0.0232626000
_diffrn_orient_matrix_UB_22      0.0152973000
_diffrn_orient_matrix_UB_23      0.0277204000
_diffrn_orient_matrix_UB_31      -0.0445866000
_diffrn_orient_matrix_UB_32      -0.0357432000
_diffrn_orient_matrix_UB_33      -0.0025010000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            90751
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.014
_diffrn_reflns_theta_min         2.965
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.707
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_correction_T_min  0.585
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_description       plate
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.402
_exptl_crystal_size_mid          0.354
_exptl_crystal_size_min          0.123
_refine_diff_density_max         1.788
_refine_diff_density_min         -2.688
_refine_diff_density_rms         0.174
_refine_ls_extinction_coef       0.00287(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         17805
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0187P)^2^+20.3888P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15596
_reflns_number_total             17805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00344a2.cif
_cod_data_source_block           rs273
_cod_depositor_comments
'Adding full bibliography for 7703559--7703562.cif.'
_cod_database_code               7703562
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C55 H109 N2 O9 Si2 Ta'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
Uanis(C5) = Uanis(C4)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C6(H6A,H6B), C11(H11A,H11B), C30(H30A,H30B)
3.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C32(H32), C36(H36), C38(H38)
3.c Idealised Me refined as rotating group:
 C01O(H01A,H01B,H01C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C),
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C),
 C29(H29A,H29B,H29C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C),
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C)
3.d Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_shelx_res_checksum              37787
_shelx_fab_checksum              1534
_olex2_date_sample_data_collection 2019-05-23
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop in perfluoroether oil'
_olex2_submission_original_sample_id RS2773
_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 1.216
_oxdiff_exptl_absorpt_empirical_full_min 0.850