Synthesis, Thermochemistry, Bonding, and 13C NMR Chemical Shift Analysis of a Phosphorano-Stabilized Carbene of Thorium
Smiles, Danil E.; Wu, Guang; Hrobárik, Peter; Hayton, Trevor W.; Organometallics 36 (2017) 4519–; doi:10.1021/acs.organomet.7b00202

data_4087262
_publ_section_title
;
 Synthesis, Thermochemistry, Bonding, and 13C NMR Chemical Shift Analysis
 of a Phosphorano-Stabilized Carbene of Thorium
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              4519
_journal_paper_doi               10.1021/acs.organomet.7b00202
_journal_volume                  36
_journal_year                    2017
_chemical_formula_sum            'C37 H70 N3 P Si6 Th'
_chemical_formula_weight         988.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.274(2)
_cell_angle_beta                 89.827(3)
_cell_angle_gamma                83.061(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7597(19)
_cell_length_b                   11.701(2)
_cell_length_c                   19.500(4)
_cell_measurement_reflns_used    1018
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.875
_cell_measurement_theta_min      21.125
_cell_volume                     2420.1(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30660
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    3.289
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.806
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         11981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0203
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+1.2717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0481
_refine_ls_wR_factor_ref         0.0491
_reflns_number_gt                11324
_reflns_number_total             11981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7b00202_si_003.cif
_cod_data_source_block           ds_10_96_0m_a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 4087262.cif.
;
_cod_original_cell_volume        2420.2(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4087262