The isomeric structure of pentacoordinate chiral spirophosphoranes in solution by the combined use of NMR experiments and GIAO DFT calculations of NMR parameters
Polyancev, Fedor M.; Metlushka, Kirill E.; Sadkova, Dilyara N.; Khisametdinova, Zilya R.; Kataeva, Olga N.; Alfonsov, Vladimir A.; Latypov, Shamil K.; Sinyashin, Oleg G.; Dalton Trans.  (2017) –; doi:10.1039/C7DT01605K

data_7043314
_publ_section_title
;
 The isomeric structure of pentacoordinate chiral spirophosphoranes in
 solution by the combined use of NMR experiments and GIAO DFT calculations
 of NMR parameters
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01605K
_journal_year                    2017
_chemical_formula_sum            'C37 H28 F2 N2 O2 P'
_chemical_formula_weight         601.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-06 deposited with the CCDC.
2017-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.512(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.86(2)
_cell_length_b                   8.799(5)
_cell_length_c                   17.269(9)
_cell_measurement_reflns_used    1744
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.86
_cell_measurement_theta_min      2.37
_cell_volume                     5877(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1310
_diffrn_reflns_av_unetI/netI     0.1799
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28391
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.598
_diffrn_reflns_theta_min         2.106
_diffrn_source                   'fine-focus X-ray tube'
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       block
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.120
_exptl_transmission_factor_max   0.983
_exptl_transmission_factor_min   0.966
_refine_diff_density_max         0.185
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.738
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6119
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.737
_refine_ls_R_factor_all          0.1981
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0356P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.1084
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1891
_reflns_number_total             6119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01605k2.cif
_cod_data_source_block           kir9-final
_cod_original_cell_volume        5878(6)
_cod_database_code               7043314
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              4459