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_7043315
_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_absolute_configuration ad
_chemical_formula_moiety         'C34 H27 N2 O2 P'
_chemical_formula_sum            'C34 H27 N2 O2 P'
_chemical_formula_weight         526.54
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6029(2)
_cell_length_b                   15.2183(3)
_cell_length_c                   20.4343(4)
_cell_measurement_reflns_used    9792
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.94
_cell_measurement_theta_min      2.40
_cell_volume                     2675.29(10)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            49141
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.171
_diffrn_reflns_theta_min         1.668
_diffrn_source                   'fine-focus X-ray tube'
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS version 2.10 (Sheldrick,Bruker AXS Inc.,2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.391
_exptl_crystal_size_mid          0.389
_exptl_crystal_size_min          0.152
_exptl_transmission_factor_max   0.7462
_exptl_transmission_factor_min   0.6975
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 2788 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         8492
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0613P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0976
_reflns_Friedel_coverage         0.760
_reflns_Friedel_fraction_full    0.976
_reflns_Friedel_fraction_max     0.958
_reflns_number_gt                7309
_reflns_number_total             8492
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01605k2.cif
_cod_data_source_block           alf1a
_cod_database_code               7043315
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.948
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              74896