Rearrangements and Reductive Cleavage of 3а,6а-Diaza-1,4-diphosphapentalenes
Panova, Yulia; Khristolyubova, Alexandra; Sushev, Vyacheslav; Zolotareva, Natalya; Baranov, Evgeny V.; Fukin, Georgii K.; Kornev, Alexander; New Journal of Chemistry 45 (2021) 18491–18496; doi:10.1039/D1NJ03341G

data_7060940
_publ_section_title
;
 Rearrangements and Reductive Cleavage of
 3&#x0430;,6&#x0430;-Diaza-1,4-diphosphapentalenes
;
_journal_issue                   39
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18491
_journal_page_last               18496
_journal_paper_doi               10.1039/D1NJ03341G
_journal_volume                  45
_journal_year                    2021
_chemical_formula_sum            'C14 H18 N Na O2 P2'
_chemical_formula_weight         317.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-06-16 deposited with the CCDC.	2021-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                106.580(2)
_cell_angle_beta                 107.348(2)
_cell_angle_gamma                90.391(2)
_cell_formula_units_Z            2
_cell_length_a                   7.1413(5)
_cell_length_b                   10.5119(7)
_cell_length_c                   11.2705(8)
_cell_measurement_reflns_used    6058
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      2.38
_cell_volume                     770.08(9)
_computing_cell_refinement       SAINT
_computing_data_collection       APEX3
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker D8 Quest (CMOS)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1239
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5745
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.183
_diffrn_reflns_theta_min         2.375
_diffrn_source                   'microfocus tube'
_exptl_absorpt_coefficient_mu    0.310
_exptl_absorpt_correction_T_max  0.958805
_exptl_absorpt_correction_T_min  0.644369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS-2012/1
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       plate
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         5745
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1434
_refine_ls_R_factor_gt           0.0770
_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^)+(0.0378P)^2^+1.2630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1571
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3582
_reflns_number_total             5745
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03341g2.cif
_cod_data_source_block           ppnnadme_a
_cod_database_code               7060940
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.958
_shelx_estimated_absorpt_t_max   0.994
_shelx_res_checksum              14548