Absolute Configuration and Conformation of (-)-<i>R</i>-<i>t</i>-Butylphenylphosphinoamidate: Chiroptical Spectroscopy and X-ray Analysis.
Petrovic, Ana G.; Polavarapu, Prasad L.; Łopusiński, Andrzej; Krasowska, Dorota; Wieczorek, Wanda; Szyrej, Małgorzata; Błaszczyk, Jarosław; Drabowicz, Józef; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.0c00756

data_4038700
_publ_section_title
;
 Absolute Configuration and Conformation of
 (-)-<i>R</i>-<i>t</i>-Butylphenylphosphinoamidate: Chiroptical
 Spectroscopy and X-ray Analysis.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c00756
_journal_year                    2020
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C30 H30 N O3 P'
_chemical_formula_sum            'C30 H30 N O3 P'
_chemical_formula_weight         483.52
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_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
_audit_update_record
;
2020-01-23 deposited with the CCDC.	2020-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.83(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.085(2)
_cell_length_b                   7.2789(15)
_cell_length_c                   14.672(3)
_cell_measurement_reflns_used    5285
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.87
_cell_measurement_theta_min      2.07
_cell_volume                     1281.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Kuma KM4-CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0114
_diffrn_reflns_av_sigmaI/netI    0.0132
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16269
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.139
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.128
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         4913
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0688
_reflns_number_gt                4652
_reflns_number_total             4913
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo0c00756_si_001.cif
_cod_data_source_block           jd18
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_absolute_configuration' value ' rm' was changed
to 'rm' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4038700