Organometallic Complexes of Bulky, Optically Active, C3-Symmetric Tris(4S-isopropyl-5,5-dimethyl-2-oxazolinyl)phenylborate (ToP*)
Xu, Songchen; Magoon, Yitzhak; Reinig, Regina R.; Schmidt, Bradley M.; Ellern, Arkady; Sadow, Aaron D.; Organometallics 34 (2015) 3508–; doi:10.1021/acs.organomet.5b00225

data_4087523
_publ_section_title
;
 Organometallic Complexes of Bulky, Optically Active, C3-Symmetric
 Tris(4S-isopropyl-5,5-dimethyl-2-oxazolinyl)phenylborate (ToP*)
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3508
_journal_paper_doi               10.1021/acs.organomet.5b00225
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_sum            'C30 H47 B N3 O3 Tl'
_chemical_formula_weight         712.88
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7724(6)
_cell_length_b                   16.1092(9)
_cell_length_c                   17.0180(9)
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.05
_cell_measurement_theta_min      2.39
_cell_volume                     3227.4(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32169
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.741
_exptl_absorpt_coefficient_mu    5.037
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
; 
 Flack x determined using 3228 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.003(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         7964
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+0.6774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0478
_refine_ls_wR_factor_ref         0.0488
_reflns_Friedel_coverage         0.785
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                7559
_reflns_number_total             7964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00225_si_002.cif
_cod_data_source_block           TlTopstar_2
_cod_database_code               4087523
_shelx_estimated_absorpt_t_min   0.354
_shelx_estimated_absorpt_t_max   0.418
_shelxl_version_number           2014/6
_shelx_res_checksum              81919
_shelx_hkl_checksum              31818