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_7047223
_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 H60 N4 P4, 0.5(C7 H8)'
_chemical_formula_sum            'C43.5 H60 N4 P4'
_chemical_formula_weight         762.83
_chemical_melting_point          453
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                97.9385(14)
_cell_angle_beta                 92.7290(15)
_cell_angle_gamma                102.0334(15)
_cell_formula_units_Z            2
_cell_length_a                   9.6038(3)
_cell_length_b                   13.3765(3)
_cell_length_c                   16.9285(4)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    100.04
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.39
_cell_volume                     2099.99(10)
_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      100.04
_diffrn_measured_fraction_theta_full 0.999
_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  0.0480
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35470
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.572
_diffrn_reflns_theta_min         1.839
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.215
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7098
_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    1.206
_exptl_crystal_description       needle
_exptl_crystal_F_000             818
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.056
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         9670
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0403P)^2^+1.7373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1202
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7532
_reflns_number_total             9670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02087f2.cif
_cod_data_source_block           mat42_0m
_cod_depositor_comments
'Adding full bibliography for 7047223--7047227.cif.'
_cod_original_formula_sum        'C43.50 H60 N4 P4'
_cod_database_code               7047223
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.942
_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. Rigid bond restraints
 C1, C2, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
C7 \\sim C1 \\sim C6 \\sim C5 \\sim C4 \\sim C3 \\sim C2: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(P0AA)=1-FVAR(1)
 Sof(P4A)=Sof(H75)=FVAR(1)
 Fixed Sof: C1(0.5) C2(0.5) H2A(0.5) C3(0.5) H3(0.5) C4(0.5) H4(0.5) C5(0.5)
 H5(0.5) C6(0.5) H6(0.5) C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C61(H61), C62(H62),
 C63(H63), C64(H64), C65(H65), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75),
  C81(H81), C82(H82), C83(H83), C84(H84), C85(H85), C2(H2A), C3(H3), C4(H4),
 C5(H5), C6(H6)
5.b 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), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C), C7(H7A,H7B,H7C)
;
_olex2_submission_special_instructions 'No special instructions were received'