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_7717494
_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
'C27 H27 N P2, 2(B C24 F20), [+ solvents]2[C5H12]'
_chemical_formula_sum            'C75 H27 B2 F40 N P2'
_chemical_formula_weight         1785.53
_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   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                90
_cell_angle_beta                 101.146(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5651(11)
_cell_length_b                   21.2162(11)
_cell_length_c                   23.6425(16)
_cell_measurement_reflns_used    5930
_cell_measurement_temperature    149.99
_cell_measurement_theta_max      21.29
_cell_measurement_theta_min      2.21
_cell_volume                     7660.2(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      149.99
_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  0.1777
_diffrn_reflns_av_unetI/netI     0.1247
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            47683
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.643
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.198
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       shard
_exptl_crystal_F_000             3536
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.0021(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         6750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.0657
_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^)+(0.0840P)^2^+4.5544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1973
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3990
_reflns_number_total             6750
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02990a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7717491--7717494.cif.'
_cod_original_cell_volume        7660.3(9)
_cod_database_code               7717494
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.980
_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. Others
 Fixed Sof: H2A(0.5) H2B(0.5) H2C(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B)
3.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C34(H34), C46(H46), C48(H48), C50(H50), C52(H52), C55(H55),
 C56(H56), C57(H57), C60(H60)
3.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              21026
_shelx_hkl_checksum              20242
_shelx_fab_checksum              91717
_olex2_submission_special_instructions 'No special instructions were received'