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_7060942
_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            'C64 H92 N4 Na4 O12 P4'
_chemical_formula_weight         1325.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2021-06-16 deposited with the CCDC.	2021-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.9970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7757(3)
_cell_length_b                   21.2281(4)
_cell_length_c                   19.6970(4)
_cell_measurement_reflns_used    9723
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.65
_cell_volume                     6806.2(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            79557
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.291
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.198
_exptl_absorpt_correction_T_max  0.9705
_exptl_absorpt_correction_T_min  0.8521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       cube
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     935
_refine_ls_number_reflns         16394
_refine_ls_number_restraints     230
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0486P)^2^+2.8337P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.0996
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13699
_reflns_number_total             16394
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03341g2.cif
_cod_data_source_block           nannppttrlnm
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7060942
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.958
_shelx_estimated_absorpt_t_max   0.962
_shelx_res_checksum              55487