Dioxaphosphabicyclooctanes: small caged phosphines from tris(hydroxymethyl)phosphine
Nobbs, James David; Tay, Dillon; Yeap, Yoon Hui; Tiong, Yong-Lun; Ye, Suming; Aitipamula, Srinivasulu; Wang, Cun; Cheong, Choon Boon; van Meurs, Martin; Dalton Transactions  (2023) –; doi:10.1039/D3DT02577B

data_7714423
_publ_section_title
;
 Dioxaphosphabicyclooctanes: small caged phosphines from
 tris(hydroxymethyl)phosphine
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02577B
_journal_year                    2023
_chemical_formula_moiety         'C32 H60 O8 P4 Pd'
_chemical_formula_sum            'C32 H60 O8 P4 Pd'
_chemical_formula_weight         803.08
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-17 deposited with the CCDC.	2023-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3803(2)
_cell_length_b                   20.3803(2)
_cell_length_c                   9.0334(2)
_cell_measurement_reflns_used    2182
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.8940
_cell_measurement_theta_min      6.1270
_cell_volume                     3752.08(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2945
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -110.00 -19.00   1.00   10.00    --  -39.87 -38.00 -90.00   91
  2  \w     23.00  58.00   1.00    1.00    --  107.57 -94.00  60.00   35
  3  \w    117.00 176.00   1.00    1.00    --  107.57 125.00 120.00   59
  4  \w     84.00 178.00   1.00    1.00    --  107.57  15.00-180.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0544176000
_diffrn_orient_matrix_UB_12      -0.0495522000
_diffrn_orient_matrix_UB_13      0.0385040000
_diffrn_orient_matrix_UB_21      0.0518721000
_diffrn_orient_matrix_UB_22      0.0545504000
_diffrn_orient_matrix_UB_23      -0.0158757000
_diffrn_orient_matrix_UB_31      -0.0077390000
_diffrn_orient_matrix_UB_32      0.0168414000
_diffrn_orient_matrix_UB_33      0.1653983000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2953
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.048
_diffrn_reflns_theta_min         5.356
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.977
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pale colourless'
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       plate
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.00033(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         1830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0702P)^2^+3.3253P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1140
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1703
_reflns_number_total             1830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02577b2.cif
_cod_data_source_block           yyh1-10
_cod_original_cell_volume        3752.08(11)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7714423
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C32H60O8P4Pd1
_chemical_oxdiff_usercomment     'James David Nobbs'
_shelx_estimated_absorpt_t_max   0.510
_shelx_estimated_absorpt_t_min   0.297
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C8A(0.6) H8AA(0.6) H8AB(0.6) H8AC(0.6) C8B(0.4) H8BA(0.4)
 H8BB(0.4) H8BC(0.4) C7A(0.6) H7AA(0.6) H7AB(0.6) H7AC(0.6) C7B(0.4) H7BA(0.4)
 H7BB(0.4) H7BC(0.4)
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C4(H4A,H4B), C2(H2A,H2B)
3.b Idealised Me refined as rotating group:
 C8A(H8AA,H8AB,H8AC), C8B(H8BA,H8BB,H8BC), C6(H6A,H6B,H6C), C7A(H7AA,H7AB,
 H7AC), C7B(H7BA,H7BB,H7BC)
;
_shelx_res_checksum              22443
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.374
_oxdiff_exptl_absorpt_empirical_full_min 0.699