Crystal structure of hexamethyl 4,4',4'',4''',4'''',4'''''-[(1,3,5,2λ^5^,4λ^5^,6λ^5^-triazatriphosphinine-2,2,4,4,6,6-hexayl)hexakis(oxy)]hexabenzoate
Zhu, Jing; Hou, Guo Hui; Li, Qian; Zheng, Fu Wei; Wei, Hong Liang; Chu, Hui Juan; Wang, Gang; He, Juan; Qu, Ling Bo; Acta Crystallographica Section E 73 (2017) 1252–1254; doi:10.1107/S2056989017010325

data_2242265
_publ_section_title
;
 Crystal structure of hexamethyl
 4,4',4'',4''',4'''',4'''''-[(1,3,5,2\l^5^,4\l^5^,6\l^5^-triazatriphosphinine-2,2,4,4,6,6-hexayl)hexakis(oxy)]hexabenzoate
;
_journal_coeditor_code           RZ5218
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1252
_journal_page_last               1254
_journal_paper_doi               10.1107/S2056989017010325
_journal_volume                  73
_journal_year                    2017
_chemical_formula_moiety         'C48 H42 N3 O18 P3'
_chemical_formula_sum            'C48 H42 N3 O18 P3'
_chemical_formula_weight         1041.75
_chemical_name_systematic
'Hexamethyl 4,4',4'',4''',4'''',4'''''-[(1,3,5,2\l^5^,4\l^5^,6\l^5^-triazatriphosphinine-2,2,4,4,6,6-hexayl)hexakis(oxy)]hexabenzoate'
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                99.134(3)
_cell_angle_beta                 95.917(3)
_cell_angle_gamma                103.941(3)
_cell_formula_units_Z            2
_cell_length_a                   11.4012(4)
_cell_length_b                   13.8443(5)
_cell_length_c                   17.0264(8)
_cell_measurement_reflns_used    5102
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      69.9590
_cell_measurement_theta_min      3.8690
_cell_volume                     2547.07(18)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2104 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur Eos Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18292
_diffrn_reflns_theta_full        67.072
_diffrn_reflns_theta_max         67.072
_diffrn_reflns_theta_min         3.350
_exptl_absorpt_coefficient_mu    1.725
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       ' '
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         9102
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1121P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1661
_refine_ls_wR_factor_ref         0.1813
_reflns_number_gt                6523
_reflns_number_total             9102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            rz5218sup1.cif
_cod_data_source_block           I
_cod_database_code               2242265
_cod_database_fobs_code          2242265
_shelx_estimated_absorpt_t_min   0.724
_shelx_estimated_absorpt_t_max   0.770
_shelx_res_checksum              13013