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_7060941
_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            'C16 H14 N2 P2'
_chemical_formula_weight         296.23
_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'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 97.827(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5266(7)
_cell_length_b                   5.1677(2)
_cell_length_c                   12.6369(4)
_cell_measurement_reflns_used    2615
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.2130
_cell_measurement_theta_min      3.5280
_cell_volume                     1392.67(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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 0.990
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9820
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.991
_diffrn_reflns_theta_min         3.255
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.919
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       stick
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.556
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1673
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0404P)^2^+0.3860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0744
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1423
_reflns_number_total             1673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03341g2.cif
_cod_data_source_block           pnnpph
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7060941
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.850
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              3503