Two tris(3,5-disubstituted phenyl)phosphines and their isostructural P^V^ oxides
Hill, Nathan D. D.; Boeré, René T.; Acta Crystallographica Section E 74 (2018) 889–894; doi:10.1107/S2056989018007831

data_2242520
_publ_section_title
;
 Two tris(3,5-disubstituted phenyl)phosphines and their isostructural P^V^
 oxides
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              889
_journal_page_last               894
_journal_paper_doi               10.1107/S2056989018007831
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C27 H33 O4 P'
_chemical_formula_moiety         'C27 H33 O4 P'
_chemical_formula_sum            'C27 H33 O4 P'
_chemical_formula_weight         452.50
_chemical_name_common
;
Tris(4-methoxy-3,5-dimethylphenyl)phosphine oxide
;
_chemical_name_systematic
;
Tris(4-methoxy-3,5-dimethylphenyl(oxo)-\l^5^-phosphane
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_method
;
OLEX2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.28601(11)
_cell_length_b                   11.90008(11)
_cell_length_c                   36.3801(3)
_cell_measurement_reflns_used    16756
_cell_measurement_temperature    108.3(4)
_cell_measurement_theta_max      80.0240
_cell_measurement_theta_min      4.5910
_cell_volume                     4886.01(8)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>olex2.solve</i> (Bourhis et al., 2015)
;
_diffrn_ambient_temperature      108.3(4)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction SuperNova, Dual, Cu at zero, Pilatus 200/300K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            29719
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.256
_diffrn_reflns_theta_min         4.611
_exptl_absorpt_coefficient_mu    1.235
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       plate
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.405
_refine_ls_extinction_coef       0.00025(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2016 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+2.7320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1003
_reflns_number_gt                4821
_reflns_number_total             5325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7751sup1.cif
_cod_data_source_block           IV
_cod_database_code               2242520
_cod_database_fobs_code          2242520
_shelx_res_checksum              56469