Chiral [16]-ane P<sub>4</sub>N<sub>2</sub> macrocycles: stereoselective synthesis and unexpected intermolecular exchange of endocyclic fragments.
Musina, E. I.; Naumov, R. N.; Kanunnikov, K. B.; Dobrynin, A. B.; Gómez-Ruiz, S; Lönnecke, P; Hey-Hawkins, E; Karasik, A. A.; Sinyashin, O. G.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 16977–16984; doi:10.1039/c8dt03214a

data_7048147
_publ_section_title
;
 Chiral [16]-ane P<sub>4</sub>N<sub>2</sub> macrocycles: stereoselective
 synthesis and unexpected intermolecular exchange of endocyclic fragments.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16977
_journal_page_last               16984
_journal_paper_doi               10.1039/c8dt03214a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C62 H82 N2 P4, 4(C6 H6)'
_chemical_formula_sum            'C86 H106 N2 P4'
_chemical_formula_weight         1291.61
_chemical_name_systematic
1,9-bis((R,S)-\a-methylbenzyl)-3,7,11,15-tetramesityl-1,9-diaza-3,7,11,15-(RSSR)-tetraphosphacyclohexadecane
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-10-24 deposited with the CCDC.
2018-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 109.79(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.601(7)
_cell_length_b                   33.967(15)
_cell_length_c                   13.081(4)
_cell_measurement_reflns_used    2383
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.94
_cell_measurement_theta_min      2.47
_cell_volume                     4014(4)
_computing_cell_refinement       'MolEN, 1994'
_computing_data_collection       'MolEN, 1994'
_computing_data_reduction        'MolEN, 1994'
_computing_molecular_graphics    'SHELXS-97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR, 19921'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\t
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8490
_diffrn_reflns_theta_full        74.43
_diffrn_reflns_theta_max         74.43
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    1.179
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         7990
_refine_ls_number_restraints     252
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1183P)^2^+0.5708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1796
_refine_ls_wR_factor_ref         0.2146
_reflns_number_gt                5034
_reflns_number_total             7990
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt03214a2.cif
_cod_data_source_block           s14
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7048146--7048148.cif.
;
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               7048147