Highly selective additions of hydride and organolithium nucleophiles to helical carbenium ions
Guin, Joyram; Besnard, Céline; Pattison, Philip; Lacour, Jérôme; Chemical Science 2 (2011) 425–; doi:10.1039/c0sc00525h

data_1515502
_publ_section_title
;
 Highly selective additions of hydride and organolithium nucleophiles to
 helical carbenium ions
;
_journal_issue                   3
_journal_name_full               'Chemical Science'
_journal_page_first              425
_journal_paper_doi               10.1039/c0sc00525h
_journal_volume                  2
_journal_year                    2011
_chemical_formula_moiety         'C41 H36 F6 N2 O2'
_chemical_formula_sum            'C41 H36 F6 N2 O2'
_chemical_formula_weight         702.74
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                91.073(4)
_cell_angle_beta                 92.167(10)
_cell_angle_gamma                100.384(11)
_cell_formula_units_Z            2
_cell_length_a                   8.641(2)
_cell_length_b                   12.453(3)
_cell_length_c                   16.039(3)
_cell_measurement_reflns_used    11705
_cell_measurement_temperature    120
_cell_measurement_theta_max      26
_cell_measurement_theta_min      6
_cell_volume                     1695.8(7)
_computing_cell_refinement       'XDS (Kabsch, 1988)'
_computing_data_collection       'IPDS (Stoe & Cie, 1996)'
_computing_data_reduction        'XDS (Kabsch 1988)'
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15780
_diffrn_reflns_theta_full        26.216
_diffrn_reflns_theta_max         26.731
_diffrn_reflns_theta_min         5.449
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.600
_exptl_crystal_size_min          0.600
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.32
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1087
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         6254
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.0015235
_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:
1.42 1.44 0.149
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0800
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0800
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                5812
_reflns_number_total             7048
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.87
_oxford_diffrn_Wilson_scale      27.02
_oxford_refine_ls_r_factor_ref   0.0486
_oxford_refine_ls_scale          0.25471(13)
_oxford_reflns_number_all        6254
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            c0sc00525h.txt
_cod_data_source_block           1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/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 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               1515502