The structures of 1:1 and 1:2 adducts of phosphanetricarbonitrile with 1,4-diazabicyclo[2.2.2]octane
Purdy, Andrew P.; Butcher, Ray J.; Klug, Christopher A.; Acta Crystallographica Section E 77 (2021) 1190–1196; doi:10.1107/S2056989021011464

data_2243980
_publ_section_title
;
 The structures of 1:1 and 1:2 adducts of phosphanetricarbonitrile with
 1,4-diazabicyclo[2.2.2]octane
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1190
_journal_page_last               1196
_journal_paper_doi               10.1107/S2056989021011464
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '2C6 H12 N2, C3 N3 P'
_chemical_formula_moiety         '2(C6 H12 N2), C3 N3 P'
_chemical_formula_sum            'C15 H24 N7 P'
_chemical_formula_weight         333.38
_chemical_name_systematic
;
Phosphanetricarbonitrile--1,4-diazabicyclo[2.2.2]octane (1/2)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 104.555(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.5807(2)
_cell_length_b                   12.3447(4)
_cell_length_c                   10.7719(4)
_cell_measurement_reflns_used    4473
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      35.61
_cell_measurement_theta_min      2.56
_cell_volume                     846.99(5)
_computing_cell_refinement
;
SAINT (Bruker, 2002)
;
_computing_data_collection
;
APEX2 (Bruker, 2005)
;
_computing_data_reduction
;
SAINT (Bruker, 2002)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick 2015a)
;
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19743
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.294
_diffrn_reflns_theta_min         2.557
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       plate
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.373
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         4235
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0428P)^2^+0.3013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1093
_reflns_number_gt                3117
_reflns_number_total             4235
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yy2005sup1.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               2243980
_shelx_estimated_absorpt_t_min   0.950
_shelx_estimated_absorpt_t_max   0.997
_shelx_hkl_checksum              55017
_shelx_res_checksum              43215
_cod_database_fobs_code 2243980