A study of the pyramidality index in tris(2,4,6-triisopropylphenyl)phosphonium perchlorate
Boeré, René T.; Zhang, Yuankui; Acta Crystallographica Section C 69 (2013) 1051–1054; doi:10.1107/S0108270113020647

data_2019137
_publ_section_title
;
 A study of the pyramidality index in
 tris(2,4,6-triisopropylphenyl)phosphonium perchlorate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1051
_journal_page_last               1054
_journal_paper_doi               10.1107/S0108270113020647
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C45 H70 P +, Cl O4 -'
_chemical_formula_moiety         'C45 H70 P +, Cl O4 -'
_chemical_formula_sum            'C45 H70 Cl O4 P'
_chemical_formula_weight         741.43
_chemical_name_common
;
Tripp3PH + Cl O4 -
;
_chemical_name_systematic
;
Tris(2,4,6-triisopropylphenyl)phosphonium perchlorate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6822(14)
_cell_length_b                   17.0621(18)
_cell_length_c                   18.660(2)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.18
_cell_volume                     4356.1(8)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2008)'
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
Bruker APEXII CCD area-detector
;
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            61837
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         27.530
_diffrn_reflns_theta_min         1.846
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  0.9731
_exptl_absorpt_correction_T_min  0.9408
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_description       Block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.378
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.168
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.309
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(7)
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         10021
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0506P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                7663
_reflns_number_total             10021
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fn3145.cif
_cod_data_source_block           I
_cod_database_code               2019137
_cod_database_fobs_code          2019137
_shelx_res_checksum              1743
_shelxl_version_number           2.013