Novel enantiopure monophospholes: synthesis, spatial and electronic structure, photophysical characteristics and conjugation effects.
Oshchepkova, Elena; Zagidullin, Almaz; Burganov, Timur; Katsyuba, Sergey; Miluykov, Vasily; Lodochnikova, Olga; Dalton transactions (Cambridge, England : 2003) 47 (2018) 11521–11529; doi:10.1039/c8dt02208a

data_7047162
_publ_section_title
;
 Novel enantiopure monophospholes: synthesis, spatial and electronic
 structure, photophysical characteristics and conjugation effects.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11521
_journal_page_last               11529
_journal_paper_doi               10.1039/c8dt02208a
_journal_volume                  47
_journal_year                    2018
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C39 H41 O P'
_chemical_formula_sum            'C39 H41 O P'
_chemical_formula_weight         556.69
_chemical_melting_point          298
_chemical_name_systematic
2,3,4,5-tetraphenyl-1-(1R,2S,5R)-menthyl)oxymethyl-1-phosphacyclopentadiene-2,4
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-07-23 deposited with the CCDC.
2018-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.693(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
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_cell_length_b                   5.501(5)
_cell_length_c                   23.97(2)
_cell_measurement_reflns_used    704
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      18.16
_cell_measurement_theta_min      3.62
_cell_volume                     1624(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    SHELXT-2014/5
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1396
_diffrn_reflns_av_unetI/netI     0.1302
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            11580
_diffrn_reflns_point_group_measured_fraction_full 0.670
_diffrn_reflns_point_group_measured_fraction_max 0.670
_diffrn_reflns_theta_full        24.984
_diffrn_reflns_theta_max         24.984
_diffrn_reflns_theta_min         2.296
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.177
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         3844
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.1496
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0625P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1562
_reflns_Friedel_coverage         0.211
_reflns_Friedel_fraction_full    0.263
_reflns_Friedel_fraction_max     0.263
_reflns_number_gt                2017
_reflns_number_total             3844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02208a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7047162--7047163.cif.'
_cod_database_code               7047162
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.951
_shelx_estimated_absorpt_t_max   0.994
_shelx_res_checksum              96314