Covalent self-assembly of the specific RSSR isomer of 14-membered tetrakisphosphine
Wittmann, T. I.; Musina, E. I.; Krivolapov, D. B.; Litvinov, I. A.; Kondrashova, S. A.; Latypov, Sh. K.; Karasik, A. A.; Sinyashin, O. G.; Dalton Trans.  (2017) –; doi:10.1039/C7DT03010J

data_7044078
_publ_section_title
;
 Covalent self-assembly of the specific RSSR isomer of 14-membered
 tetrakisphosphine
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03010J
_journal_year                    2017
_chemical_formula_sum            'C42 H58 N2 P4'
_chemical_formula_weight         714.78
_chemical_name_systematic
1,8-di(iso-pentyl)-3,6,10,13-tetraphenyl-1,8-diaza-3,6,10,13-tetraphosphacyclotetradecane
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-07-07 deposited with the CCDC.
2017-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                112.941(10)
_cell_angle_beta                 95.282(11)
_cell_angle_gamma                96.975(11)
_cell_formula_units_Z            1
_cell_length_a                   5.623(5)
_cell_length_b                   13.319(11)
_cell_length_c                   14.842(13)
_cell_measurement_reflns_used    1558
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.35
_cell_measurement_theta_min      2.68
_cell_volume                     1004.2(15)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.0960
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8329
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.993
_diffrn_reflns_theta_min         1.507
_exptl_absorpt_coefficient_mu    0.219
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_gt           0.0643
_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^)+(0.0928P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1526
_refine_ls_wR_factor_ref         0.1827
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2293
_reflns_number_total             3873
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03010j2.cif
_cod_data_source_block           shelx
_cod_database_code               7044078
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.919
_shelx_estimated_absorpt_t_max   0.972
_shelx_res_checksum              61493