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_7703559
_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         'C39 H65 Cl1 N2 O Rh Ta'
_chemical_formula_sum            'C39 H65 Cl N2 O Rh Ta'
_chemical_formula_weight         897.26
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90
_cell_angle_beta                 94.253(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0011(7)
_cell_length_b                   15.5230(10)
_cell_length_c                   26.6754(19)
_cell_measurement_reflns_used    11274
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      29.3570
_cell_measurement_theta_min      3.3150
_cell_volume                     4129.9(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.891
_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  0.097
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            56886
_diffrn_reflns_theta_full        26.690
_diffrn_reflns_theta_max         29.760
_diffrn_reflns_theta_min         2.734
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.141
_exptl_absorpt_correction_T_max  0.600
_exptl_absorpt_correction_T_min  0.370
_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    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.356
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.197
_refine_diff_density_max         1.97
_refine_diff_density_min         -2.74
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         11821
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0702
_refine_ls_shift/su_max          0.0007544
_refine_ls_shift/su_mean         0.0000350
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.01P)^2^ +*****P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1813
_refine_ls_wR_factor_gt          0.1709
_refine_ls_wR_factor_ref         0.1813
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              21
_reflns_limit_k_min              -21
_reflns_limit_l_max              35
_reflns_limit_l_min              -36
_reflns_number_gt                10014
_reflns_number_total             10862
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.02
_oxford_diffrn_Wilson_scale      0.62
_oxford_refine_ls_r_factor_ref   0.0862
_oxford_refine_ls_scale          1.209(4)
_oxford_reflns_number_all        11821
_cod_data_source_file            d0dt00344a2.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 7703559--7703562.cif.'
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C39 H65 Cl1 N2 O Rh Ta'
_cod_database_code               7703559
_oxdiff_exptl_absorpt_empirical_full_min 0.912
_oxdiff_exptl_absorpt_empirical_full_max 1.099
_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)