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_7714424
_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         'C16 H30 Cl2 O4 P2 Pd'
_chemical_formula_sum            'C16 H30 Cl2 O4 P2 Pd'
_chemical_formula_weight         525.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_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                 107.289(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7581(16)
_cell_length_b                   10.6856(15)
_cell_length_c                   8.9245(11)
_cell_measurement_reflns_used    7911
_cell_measurement_temperature    300.00
_cell_measurement_theta_max      28.270
_cell_measurement_theta_min      2.631
_cell_volume                     1070.6(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       Apex4
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      300.00
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker PHOTON'
_diffrn_measurement_method       Diffraction
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0123
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8777
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.363
_diffrn_reflns_theta_min         2.390
_diffrn_source                   'Diamond micro-source'
_diffrn_source_current           1.6
_diffrn_source_power             0.08
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.283
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1037 before and 0.0367 after correction.
The Ratio of minimum to maximum transmission is 0.9087.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   0.880
_exptl_transmission_factor_min   0.731
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         1142
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0193
_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^)+(0.0091P)^2^+2.0405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0431
_refine_ls_wR_factor_ref         0.0436
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1102
_reflns_number_total             1142
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02577b2.cif
_cod_data_source_block           mo_srini_1_2
_cod_database_code               7714424
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.882
_shelx_estimated_absorpt_t_min   0.715
_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: H2A(0.5) H2B(0.5) H6A(0.5) H6B(0.5) H6C(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C2(H2A,H2B)
3.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              36829
_olex2_submission_special_instructions 'No special instructions were received'