Synthesis and N-C bond cleavage reactions for cyclic phosphazenium dications.
Miao, Linkun; Yeganeh-Salman, Amir; Yeung, Jason; Stephan, Douglas W.; Dalton transactions (Cambridge, England : 2003) 54 (2024) 368–375; doi:10.1039/d4dt02990a

data_7717491
_publ_section_title
;
 Synthesis and N-C bond cleavage reactions for cyclic phosphazenium
 dications.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              368
_journal_page_last               375
_journal_paper_doi               10.1039/d4dt02990a
_journal_volume                  54
_journal_year                    2024
_chemical_formula_moiety         '0.5(C34 H37 N2 P2), Cl, C H2 Cl2'
_chemical_formula_sum            'C18 H20.5 Cl3 N P'
_chemical_formula_weight         388.17
_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
_audit_creation_date             2023-08-03
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-10-09 deposited with the CCDC.	2024-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                78.484(15)
_cell_angle_beta                 81.149(19)
_cell_angle_gamma                67.190(15)
_cell_formula_units_Z            4
_cell_length_a                   9.434(3)
_cell_length_b                   9.825(2)
_cell_length_c                   22.843(6)
_cell_measurement_reflns_used    3227
_cell_measurement_temperature    149.89
_cell_measurement_theta_max      26.10
_cell_measurement_theta_min      2.32
_cell_volume                     1905.6(9)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      149.89
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1235
_diffrn_reflns_av_unetI/netI     0.1107
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28713
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         0.913
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.563
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       blocks
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         6719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0600
_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^)+(0.0777P)^2^+0.0410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4423
_reflns_number_total             6719
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02990a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7717491--7717494.cif.'
_cod_original_cell_volume        1905.5(8)
_cod_original_formula_sum        'C18 H20.50 Cl3 N P'
_cod_database_code               7717491
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.849
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C40(H40A,H40B), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
  C28(H28), C29(H29), C30(H30), C31(H31), C34(H34), C38(H38), C39(H39)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C33(H33A,H33B,H33C), C35(H35A,H35B,
 H35C)
;
_shelx_res_checksum              85548
_shelx_hkl_checksum              24088
_olex2_submission_special_instructions 'No special instructions were received'