Alternating stereoselective self-assembly of SSSS/RRRR or RSSR isomers of tetrakisphosphines in the row of 14-, 16-, 18- and 20-membered macrocycles.
Naumov, Roman N.; Musina, Elvira I.; Kanunnikov, Kirill B.; Fesenko, Tatiana I.; Krivolapov, Dmitry B.; Litvinov, Igor A.; Lönnecke, Peter; Hey-Hawkins, Evamarie; Karasik, Andrey A.; Sinyashin, Oleg G.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 12784–12789; doi:10.1039/c4dt01619j

data_7031505
_publ_section_title
;
 Alternating stereoselective self-assembly of SSSS/RRRR or RSSR isomers of
 tetrakisphosphines in the row of 14-, 16-, 18- and 20-membered
 macrocycles.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12784
_journal_page_last               12789
_journal_paper_doi               10.1039/c4dt01619j
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C68 H96 N4 O2 P4'
_chemical_formula_weight         1125.37
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
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_cell_angle_alpha                90
_cell_angle_beta                 105.974(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.6565(13)
_cell_length_b                   12.9533(4)
_cell_length_c                   16.2958(5)
_cell_measurement_reflns_used    5409
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      28.7279
_cell_measurement_theta_min      2.5562
_cell_volume                     6627.1(4)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX - Version 1.64.05 (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      130(2)
_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- amd \f-scans'
_diffrn_orient_matrix_UB_11      -0.0315041975
_diffrn_orient_matrix_UB_12      -0.0301651826
_diffrn_orient_matrix_UB_13      0.0061550662
_diffrn_orient_matrix_UB_21      -0.0244718152
_diffrn_orient_matrix_UB_22      0.001416774
_diffrn_orient_matrix_UB_23      -0.0211876639
_diffrn_orient_matrix_UB_31      0.020066569
_diffrn_orient_matrix_UB_32      -0.0456251437
_diffrn_orient_matrix_UB_33      -0.0047308518
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0832
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
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_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30265
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.6
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.97401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.04
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         4752
_refine_ls_number_restraints     225
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1394
_reflns_number_gt                2605
_reflns_number_total             4752
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01619j1.cif
_cod_data_source_block           x0349fin
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/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 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7031505--7031506.cif.
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7031505