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_7703561
_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         'C51 H93 Cl1 N2 O5 Rh1 Si1 Ta1'
_chemical_formula_sum            'C51 H93 Cl N2 O5 Rh Si Ta'
_chemical_formula_weight         1161.70
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2020-01-30 deposited with the CCDC.	2020-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                68.473(5)
_cell_angle_beta                 71.745(5)
_cell_angle_gamma                85.878(5)
_cell_formula_units_Z            2
_cell_length_a                   14.7519(8)
_cell_length_b                   15.0383(9)
_cell_length_c                   15.8880(8)
_cell_measurement_reflns_used    20295
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      28.9660
_cell_measurement_theta_min      3.1740
_cell_volume                     3110.1(3)
_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    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.880
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            70217
_diffrn_reflns_theta_full        26.530
_diffrn_reflns_theta_max         29.725
_diffrn_reflns_theta_min         2.898
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.124
_exptl_absorpt_correction_T_max  0.714
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.263
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.197
_refine_diff_density_max         6.83
_refine_diff_density_min         -3.32
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9557
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         15552
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.0018321
_refine_ls_shift/su_mean         0.0000416
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.222E+04 0.313E+04 0.169E+04 453. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1301
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1301
_reflns_limit_h_max              20
_reflns_limit_h_min              -18
_reflns_limit_k_max              20
_reflns_limit_k_min              -19
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                12684
_reflns_number_total             15794
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.35
_oxford_diffrn_Wilson_scale      0.12
_oxford_refine_ls_r_factor_ref   0.0802
_oxford_refine_ls_scale          2.825(15)
_oxford_reflns_number_all        15552
_cod_data_source_file            d0dt00344a2.cif
_cod_data_source_block           I_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7703559--7703562.cif.'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C51 H93 Cl1 N2 O5 Rh1 Si1 Ta1'
_cod_database_code               7703561
_oxdiff_exptl_absorpt_empirical_full_min 0.867
_oxdiff_exptl_absorpt_empirical_full_max 1.148
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxford_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_platon_squeeze_void_probe_radius 1.20