Sequential Deprotonation-Alkylation of Binaphthyloxy-Substituted Phosphonochalcogenoates: Chiral Tri- and Tetrasubstituted Carbon Centers Adjacent to a Phosphorus Atom.
Maekawa, Yuuki; Maruyama, Toshifumi; Murai, Toshiaki; Organic letters 18 (2016) 5264–5267; doi:10.1021/acs.orglett.6b02578

data_1555819
_publ_section_title
;
 Sequential Deprotonation-Alkylation of Binaphthyloxy-Substituted
 Phosphonochalcogenoates: Chiral Tri- and Tetrasubstituted Carbon Centers
 Adjacent to a Phosphorus Atom.
;
_journal_issue                   20
_journal_name_full               'Organic letters'
_journal_page_first              5264
_journal_page_last               5267
_journal_paper_doi               10.1021/acs.orglett.6b02578
_journal_volume                  18
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C30 H25 O2 P Se'
_chemical_formula_sum            'C30 H25 O2 P Se'
_chemical_formula_weight         527.43
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.480(2)
_cell_length_b                   16.779(4)
_cell_length_c                   19.319(5)
_cell_measurement_reflns_used    4971
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      30.1003
_cell_measurement_theta_min      1.6075
_cell_volume                     2424.7(11)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0975
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_diffrn_reflns_Laue_measured_fraction_max 0.999
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_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
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_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
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_exptl_absorpt_correction_T_max  0.8664
_exptl_absorpt_correction_T_min  0.8028
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Flack x determined using 1016 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.055(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
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_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1112
_refine_ls_R_factor_gt           0.0665
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+0.8121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1273
_reflns_Friedel_coverage         0.761
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3698
_reflns_number_total             5565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b02578_si_004.cif
_cod_data_source_block           sep
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Numerical' was
changed to 'numerical' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/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 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               1555819
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.803
_shelx_estimated_absorpt_t_max   0.866
_shelx_res_checksum              96584
_shelx_hkl_checksum              63568