Barriers to Racemization in C3-Symmetric Complexes Containing the Hydrotris(2-mercapto-1-ethylimidazolyl)borate (TmEt) Ligand
Philip J. Bailey; Alice Dawson; Chiara McCormack; Stephen A. Moggach; Iain D. H. Oswald; Simon Parsons; David W. H. Rankin; Andrew Turner; Inorganic Chemistry 44 (2005) 8884–8898; doi:10.1021/ic0505293

data_4310042
_publ_contact_author_email       S.Parsons@ed.ac.uk
_publ_contact_author_name        'Simon Parsons'
_publ_section_title
;
Barriers to Racemization in C3-Symmetric Complexes Containing the
Hydrotris(2-mercapto-1-ethylimidazolyl)borate (TmEt) Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8884
_journal_page_last               8898
_journal_paper_doi               10.1021/ic0505293
_journal_volume                  44
_journal_year                    2005
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C33 H37 B1 Cu1 N6 P1 S3'
_chemical_formula_sum            'C33 H37 B Cu N6 P S3'
_chemical_formula_weight         719.23
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             05-03-22
_audit_creation_method           CRYSTALS_ver_12.80
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   15.5870(16)
_cell_length_b                   15.5870(16)
_cell_length_c                   12.144(2)
_cell_measurement_reflns_used    1009
_cell_measurement_temperature    150
_cell_measurement_theta_max      24
_cell_measurement_theta_min      2
_cell_volume                     2555.2(6)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5114
_diffrn_reflns_theta_full        23.259
_diffrn_reflns_theta_max         23.259
_diffrn_reflns_theta_min         2.256
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.906
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       block
_exptl_crystal_F_000             1122
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.71
_refine_diff_density_min         -1.17
_refine_ls_abs_structure_details 'Flack, 31 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.058(10)
_refine_ls_extinction_coef       78(7)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   1.0175
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1619
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0213
_refine_ls_shift/su_max          0.001357
_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: 
 22.6 32.5 14.2 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0504
_refine_ls_wR_factor_gt          0.0503
_refine_ls_wR_factor_ref         0.0504
_reflns_limit_h_max              8
_reflns_limit_h_min              -17
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              -13
_reflns_number_gt                1606
_reflns_number_total             1619
_reflns_threshold_expression     I>2.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.4049(6)
_oxford_structure_analysis_title 'cm1051 in R3'
_cod_data_source_file            ic0505293si20050817_061150_3.cif
_cod_data_source_block           cm1051
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2555.1(6)
_cod_original_sg_symbol_H-M      'R 3 '
_cod_original_formula_sum        'C33 H37 B1 Cu1 N6 P1 S3'
_cod_database_code               4310042