Small molecule activation by frustrated Lewis pairs.
Travis, Alastair L.; Binding, Samantha C.; Zaher, Hasna; Arnold, Thomas A. Q.; Buffet, Jean-Charles; O'Hare, Dermot; Dalton transactions (Cambridge, England : 2003) 42 (2013) 2431–2437; doi:10.1039/c2dt32525j

data_7020936
_publ_section_title
;
 Small molecule activation by frustrated Lewis pairs.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2431
_journal_page_last               2437
_journal_paper_doi               10.1039/c2dt32525j
_journal_volume                  42
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_compound_source        syn
_chemical_formula_moiety         'C48 H29.00 B1 F27 O1 P1'
_chemical_formula_sum            'C48 H29 B F27 O P'
_chemical_formula_weight         1176.49
_chemical_melting_point          ?
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             12-09-25
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   16.0095(3)
_cell_length_b                   16.0095(3)
_cell_length_c                   15.8189(4)
_cell_measurement_reflns_used    1778
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3511.26(13)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19434
_diffrn_reflns_theta_full        26.925
_diffrn_reflns_theta_max         27.475
_diffrn_reflns_theta_min         5.362
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.55
_refine_ls_abs_structure_details 'Flack (1983), 1762 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.68(18)
_refine_ls_extinction_coef       340(60)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9714
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3541
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.0032642
_refine_ls_shift/su_mean         0.0000668
_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:
22.8 37.8 23.7 10.4 2.49
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1056
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.1056
_reflns_limit_h_max              10
_reflns_limit_h_min              -20
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              -20
_reflns_number_gt                2478
_reflns_number_total             3541
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.40
_oxford_diffrn_Wilson_scale      38.38
_oxford_refine_ls_r_factor_ref   0.0719
_oxford_refine_ls_scale          0.17706(19)
_oxford_reflns_number_all        3541
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 008TAQA12
_cod_data_source_file            c2dt32525j.txt
_cod_data_source_block           '[PBB-OH][HP(t-Bu)3]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_Hall     'R 3 '
_cod_original_sg_symbol_H-M      'R 3 '
_cod_original_formula_sum        'C48 H29.00 B1 F27 O1 P1'
_cod_database_code               7020936
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
CONT EXTPARAM
CONT ENANTIO
RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S) H ( 143,X'S)
RIDE C ( 15,X'S) H ( 151,X'S) H ( 152,X'S) H ( 153,X'S)
RIDE C ( 16,X'S) H ( 161,X'S) H ( 162,X'S) H ( 163,X'S)
RIDE P ( 1,X'S) H ( 15,X'S)
RIDE O ( 2,X'S) H ( 23,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;