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_7047227
_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         'C28 H54.46 Li2 N4 O2 P2'
_chemical_formula_sum            'C28 H54.05 Li2 N4 O2 P2'
_chemical_formula_weight         554.62
_chemical_melting_point          391
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-05-13
_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                 118.0191(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8882(6)
_cell_length_b                   10.0899(3)
_cell_length_c                   19.7056(6)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.08
_cell_measurement_theta_min      2.36
_cell_volume                     3315.32(18)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.94
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            62159
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.387
_diffrn_reflns_theta_min         2.071
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.7035
_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    1.111
_exptl_crystal_description       plank
_exptl_crystal_F_000             1208
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.59
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.308
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         11816
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0666P)^2^+2.1831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1392
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9714
_reflns_number_total             11816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02087f2.cif
_cod_data_source_block           mat38n
_cod_depositor_comments
'Adding full bibliography for 7047223--7047227.cif.'
_cod_original_cell_volume        3315.31(18)
_cod_database_code               7047227
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.906
_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. Restrained distances
 C2-C1 \\sim C4-C2 \\sim C4-C3
 with sigma of 0.02
 O1-C1 \\sim O1-C4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2A) = Uanis(C4A) = Uanis(C1A) = Uanis(C3A)
Uanis(C1A) = Uanis(C2A) = Uanis(C3A) = Uanis(C4A)
Uanis(C1) = Uanis(C2) = Uanis(C4) = Uanis(C3)
Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4)
Uanis(C1A) = Uanis(C1) = Uanis(C2A) = Uanis(C2) = Uanis(C3) = Uanis(C3A) =
Uanis(C4) = Uanis(C4A)
4. Others
 Sof(C1A)=Sof(H1AA)=Sof(C2A)=Sof(H2AA)=Sof(C3A)=Sof(H3AA)=Sof(C4A)=Sof(H4AA)=
 Sof(H4AB)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=Sof(H3B)=
 Sof(C4)=Sof(H4)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C24(H24), C30(H30)
5.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C25(H25A,H25B), C26(H26A,
 H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C31(H31A,H31B),
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C1(H1A,H1B),
 C2(H2A,H2B), C3(H3A,H3B), C4A(H4AA,H4AB)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C1A(H1AA), C2A(H2AA), C3A(H3AA)
5.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
;
_olex2_submission_special_instructions 'No special instructions were received'