Cycloaddition and C‒H Activation Reactions of a Tantalum Alkylidyne
Ramírez-Contreras, Rodrigo; Bhuvanesh, Nattamai; Ozerov, Oleg V.; Organometallics 34 (2015) 1143–; doi:10.1021/acs.organomet.5b00205

data_4087513
_publ_section_title
;
 Cycloaddition and C--H Activation Reactions of a Tantalum Alkylidyne
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1143
_journal_paper_doi               10.1021/acs.organomet.5b00205
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C27 H40 B11 Cl11 P Ta'
_chemical_formula_weight         1085.37
_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_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.7560(10)
_cell_angle_beta                 74.7910(10)
_cell_angle_gamma                84.2530(10)
_cell_formula_units_Z            2
_cell_length_a                   9.2542(9)
_cell_length_b                   15.4298(15)
_cell_length_c                   17.0711(17)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      29.39
_cell_measurement_theta_min      2.29
_cell_volume                     2322.9(4)
_computing_cell_refinement
; 
  APEX-II(BRUKER-NONIUS, 2003) 
;
_computing_data_collection       'APEX-II (BRUKER-NONIUS, 2003)'
_computing_data_reduction        APEX-II
_computing_molecular_graphics    Olex2
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'APEX II'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25039
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.054
_exptl_absorpt_correction_T_max  0.8380
_exptl_absorpt_correction_T_min  0.5530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
Solvent molecule was present and could not be 
uniquely identified. It resembles close to toluene
which was used for crystallzation. However, very short
bond distances with the Ta-complex rules out toluene.
Eventually, the solvent was squeezed out which results
in 37 electrons in the void, again not clearly 
accounting for toluene.
;
_refine_diff_density_max         3.567
_refine_diff_density_min         -1.624
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         10429
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+2.2663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0957
_reflns_number_gt                9683
_reflns_number_total             10429
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00205_si_002.cif
_cod_data_source_block           rrc
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4087513