Resolution and Stereochemistry of tert-Butylphenylphosphinous Acid-Borane
Marek Stankevič; K. Michał Pietrusiewicz; Journal of Organic Chemistry 72 (2007) 816–822; doi:10.1021/jo061896e

data_4022627
_publ_section_title
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 Resolution and Stereochemistry of tert-Butylphenylphosphinous Acid-Borane
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_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              816
_journal_page_last               822
_journal_paper_doi               10.1021/jo061896e
_journal_volume                  72
_journal_year                    2007
_chemical_formula_sum            'C29 H40 B N2 O2 P'
_chemical_formula_weight         490.41
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.11
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.250
_cell_length_b                   13.014
_cell_length_c                   12.342
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      46.48
_cell_measurement_theta_min      41.15
_cell_volume                     1447.0
_computing_cell_refinement       'Express, Nonius BV'
_computing_data_collection       'Express, Nonius BV'
_computing_data_reduction        'OpenMoleN, Nonius BV'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.763
_diffrn_measured_fraction_theta_max 0.763
_diffrn_measurement_device_type  MACH3
_diffrn_measurement_method       omega\2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2347
_diffrn_reflns_theta_full        73.90
_diffrn_reflns_theta_max         73.90
_diffrn_reflns_theta_min         3.68
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  3600s
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.038
_exptl_absorpt_correction_T_max  99.97
_exptl_absorpt_correction_T_min  84.54
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.77
_exptl_crystal_size_mid          0.385
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_coef       0.0085(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         2347
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.238
_refine_ls_shift/su_mean         0.098
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1022P)^2^+0.0126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1274
_reflns_number_gt                2347
_reflns_number_total             2347
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo061896esi20060913_120535.cif
_cod_data_source_block           sw_78_Stankewicz
_cod_depositor_comments
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The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'P 21'
_cod_database_code               4022627