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_2243979
_publ_section_title
;
 The structures of 1:1 and 1:2 adducts of phosphanetricarbonitrile with
 1,4-diazabicyclo[2.2.2]octane
;
_journal_coeditor_code           YY2005
_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          'C6 H12 N2, C3 N3 P'
_chemical_formula_moiety         'C6 H12 N2, C3 N3 P'
_chemical_formula_sum            'C9 H12 N5 P'
_chemical_formula_weight         221.21
_chemical_name_systematic
;
Phosphanetricarbonitrile--1,4-diazabicyclo[2.2.2]octane (1/1)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
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_cell_angle_beta                 90
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_cell_length_a                   6.0092(2)
_cell_length_b                   13.6227(5)
_cell_length_c                   13.4716(5)
_cell_measurement_reflns_used    7580
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.99
_cell_volume                     1102.81(7)
_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      105(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0353
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16377
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.579
_diffrn_reflns_theta_min         3.024
_exptl_absorpt_coefficient_mu    0.225
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6843
_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    1.332
_exptl_crystal_description       plate
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.273
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         1764
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0261P)^2^+0.5245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0682
_reflns_number_gt                1578
_reflns_number_total             1764
_reflns_threshold_expression     'I > 2\s(I)'
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