Synthetic strategies to bicyclic tetraphosphanes using P1, P2 and P4 building blocks.
Bresien, Jonas; Faust, Kirill; Hering-Junghans, Christian; Rothe, Julia; Schulz, Axel; Villinger, Alexander; Dalton transactions (Cambridge, England : 2003) 45 (2016) 1998–2007; doi:10.1039/c5dt02757h

data_7036324
_publ_section_title
;
 Synthetic strategies to bicyclic tetraphosphanes using P1, P2 and P4
 building blocks.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1998
_journal_page_last               2007
_journal_paper_doi               10.1039/c5dt02757h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C36 H58 Cl3 Ga P4, 0.5(C6 H14)'
_chemical_formula_sum            'C39 H65 Cl3 Ga P4'
_chemical_formula_weight         833.86
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-07-20 deposited with the CCDC.
2015-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.7411(7)
_cell_length_b                   13.5063(4)
_cell_length_c                   12.5618(3)
_cell_measurement_reflns_used    9840
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      57.587
_cell_measurement_theta_min      4.449
_cell_volume                     4537.0(2)
_computing_cell_refinement       'Bruker Apex v2.0-2'
_computing_data_collection       'Bruker Apex v2.0-2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker-Nonius Apex X8-CCD-diffractometer'
_diffrn_measurement_method       'phi and psi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            69297
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_T_max  0.8113
_exptl_absorpt_correction_T_min  0.7324
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.23
_platon_squeeze_details
;
The unit cell contains two n-hexane molecules which have been treated 
as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.248
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         6840
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+4.9244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1357
_reflns_number_gt                5540
_reflns_number_total             6840
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c5dt02757h2.cif
_cod_data_source_block           is_jb73_exo_exo_MesP4Mes_GaCl3_hexane
_cod_depositor_comments
'Adding full bibliography for 7036321--7036328.cif.'
_cod_database_code               7036324