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_7048146
_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_absolute_configuration rmad
_chemical_formula_sum            'C69 H93 N3 O P4'
_chemical_formula_weight         1104.34
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-07-10 deposited with the CCDC.
2018-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                88.667(3)
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_cell_angle_gamma                64.619(4)
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_cell_length_b                   12.1381(5)
_cell_length_c                   13.2236(4)
_cell_measurement_reflns_used    9054
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      32.2423
_cell_measurement_theta_min      2.6500
_cell_volume                     1576.78(12)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET)
(compiled Nov 29 2007,17:23:28)
;
_computing_data_collection
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CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET)
(compiled Nov 29 2007,17:23:28)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET)
(compiled Nov 29 2007,17:23:28)
;
_computing_molecular_graphics    'ORTEP3 for Windows (L. J. Farrugia, 1997)'
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_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SIR92 (Giacovazzo 1993)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.3560
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ccd Xcalibur S'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0931
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31375
_diffrn_reflns_point_group_measured_fraction_full 0.996
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_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         2.661
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_T_max  1.00000
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_exptl_absorpt_correction_type   multi-scan
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CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET)
(compiled Nov 29 2007,17:23:28)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       plates
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 2534 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         10714
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0701P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1282
_reflns_Friedel_coverage         0.996
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                6768
_reflns_number_total             10714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03214a2.cif
_cod_data_source_block           x0376fin_3S
_cod_depositor_comments
'Adding full bibliography for 7048146--7048148.cif.'
_cod_original_cell_volume        1576.78(11)
_cod_database_code               7048146
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              72742