The chameleonic reactivity of dilithio bis(alkylamido)cyclodiphosph(iii)azanes with chlorophosphines.
Otang, Mathew E.; Josephson, David; Duppong, Todd; Stahl, Lothar; Dalton transactions (Cambridge, England : 2003) 47 (2018) 11625–11635; doi:10.1039/c8dt02087f

data_7047224
_publ_section_title
;
 The chameleonic reactivity of dilithio
 bis(alkylamido)cyclodiphosph(iii)azanes with chlorophosphines.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11625
_journal_page_last               11635
_journal_paper_doi               10.1039/c8dt02087f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C40 H55.82 N4 P4'
_chemical_formula_sum            'C40 H56 N4 P4'
_chemical_formula_weight         716.79
_chemical_melting_point          419
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-05-14 deposited with the CCDC.
2018-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.2670(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9400(3)
_cell_length_b                   9.8845(2)
_cell_length_c                   24.8587(5)
_cell_measurement_reflns_used    9578
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      40.64
_cell_measurement_theta_min      2.41
_cell_volume                     4015.53(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            95036
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.567
_diffrn_reflns_theta_min         2.408
_exptl_absorpt_coefficient_mu    0.229
_exptl_absorpt_correction_T_max  0.7480
_exptl_absorpt_correction_T_min  0.6744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             1535
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.68
_exptl_crystal_size_min          0.39
_refine_diff_density_max         1.837
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         11350
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0511P)^2^+6.3337P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1443
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9880
_reflns_number_total             11350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02087f2.cif
_cod_data_source_block           mat35_0
_cod_depositor_comments
'Adding full bibliography for 7047223--7047227.cif.'
_cod_database_code               7047224
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C1A \\sim C1B \\sim C2A \\sim C2B \\sim C3A \\sim C3B \\sim C4B \\sim C4A \\sim
C5A \\sim C5B \\sim C6A \\sim C6B: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C6B) = Uanis(C5B) = Uanis(C4B) = Uanis(C3B) = Uanis(C2B) = Uanis(C1B) =
Uanis(C1A) = Uanis(C2A) = Uanis(C3A) = Uanis(C4A) = Uanis(C5A) = Uanis(C6A)
Uanis(C6A) = Uanis(C1A) = Uanis(C2A) = Uanis(C3A) = Uanis(C4A) = Uanis(C5A)
3. Others
 Sof(P1B)=1-FVAR(1)
 Sof(P1A)=FVAR(1)
 Sof(P2B)=1-FVAR(2)
 Sof(P2A)=Sof(H19)=FVAR(2)
 Sof(C5B)=Sof(H5B)=Sof(C6B)=Sof(C4B)=Sof(H4B)=Sof(C3B)=Sof(H3B)=Sof(C1B)=
 Sof(H1B)=Sof(C2B)=Sof(H2B)=1-FVAR(3)
 Sof(C6A)=Sof(H6A)=Sof(C1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=
 Sof(H4A)=Sof(C5A)=Sof(H5A)=FVAR(3)
4.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C6A(H6A), C2A(H2A), C3A(H3A), C4A(H4A), C18(H18), C5A(H5A),
 C16(H16), C15(H15), C17(H17), C5B(H5B), C4B(H4B), C3B(H3B), C1B(H1B), C2B(H2B)
4.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C22(H22A,H22B,
 H22C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C)
;
_olex2_submission_special_instructions 'No special instructions were received'