Unexpected formation of a novel macrocyclic tetraphosphine: (RSSR)-1,9-dibenzyl-3,7,11,15-tetramesityl-1,9-diaza-3,7,11,15-tetraphosphacyclohexadecane.
Naumov, Roman N.; Karasik, Andrey A.; Sinyashin, Oleg G.; Lönnecke, Peter; Hey-Hawkins, Evamarie; Dalton transactions (Cambridge, England : 2003)  (2004) 357–358; doi:10.1039/b313487c

data_7013727
_publ_section_title
;
 Unexpected formation of a novel macrocyclic tetraphosphine:
 (RSSR)-1,9-dibenzyl-3,7,11,15-tetramesityl-1,9-diaza-3,7,11,15-tetraphosphacyclohexadecane.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              357
_journal_page_last               358
_journal_paper_doi               10.1039/b313487c
_journal_year                    2004
_chemical_formula_sum            'C66 H84 N2 P4'
_chemical_formula_weight         1029.23
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.741(3)
_cell_angle_beta                 80.065(3)
_cell_angle_gamma                74.491(3)
_cell_formula_units_Z            1
_cell_length_a                   8.9312(14)
_cell_length_b                   12.909(2)
_cell_length_c                   14.848(2)
_cell_measurement_reflns_used    1554
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      27.424
_cell_measurement_theta_min      2.584
_cell_volume                     1511.1(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXS-97'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_sigmaI/netI    0.1428
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15597
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.165
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             554
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         7101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.1494
_refine_ls_R_factor_gt           0.0683
_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^)+(0.0691P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1534
_reflns_number_gt                3444
_reflns_number_total             7101
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b313487c.txt
_cod_data_source_block           c1628fin
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1511.2(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7013727