Structure and photochemistry of di-<i>tert</i>-butyldiphosphatetrahedrane.
Hierlmeier, Gabriele; Kutta, Roger Jan; Coburger, Peter; Stammler, Hans-Georg; Schwabedissen, Jan; Mitzel, Norbert W.; Dimitrova, Maria; Berger, Raphael J. F.; Nuernberger, Patrick; Wolf, Robert; Chemical science 15 (2024) 5596–5603; doi:10.1039/d4sc00936c

data_1571189
_publ_section_title
;
 Structure and photochemistry of
 di-<i>tert</i>-butyldiphosphatetrahedrane.
;
_journal_issue                   15
_journal_name_full               'Chemical science'
_journal_page_first              5596
_journal_page_last               5603
_journal_paper_doi               10.1039/d4sc00936c
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C10 H18 P2'
_chemical_formula_sum            'C10 H18 P2'
_chemical_formula_weight         200.18
_chemical_melting_point          240
_chemical_name_common            Di-tert-butyldiphosphatetrahedrane
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-10
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-08-11 deposited with the CCDC.	2024-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.935(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.1480(4)
_cell_length_b                   11.2791(7)
_cell_length_c                   8.6416(6)
_cell_measurement_reflns_used    7305
_cell_measurement_temperature    94.0(1)
_cell_measurement_theta_max      32.9300
_cell_measurement_theta_min      2.9960
_cell_volume                     591.97(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      94.00(10)
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_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    -37.00  73.00   1.00  100.00    --   35.05 -19.00  30.00  110
  2  \w     13.00 106.00   1.00  100.00    --   35.05  38.00  30.00   93
  3  \w     11.00  96.00   1.00  100.00    --   35.05-135.00 -33.00   85
  4  \w     39.00 109.00   1.00  100.00    --   35.05 178.00  90.00   70
  5  \w     37.00 110.00   1.00  100.00    --   35.05-178.00 -90.00   73
  6  \w     -1.00  29.00   1.00  100.00    --   35.05  90.00 138.75   30
  7  \w      1.00  30.00   1.00  100.00    --   35.05  88.00 -20.90   29
  8  \w      1.00  31.00   1.00  100.00    --   35.05  87.00-103.96   30
  9  \w    -33.00  54.00   1.00  100.00    --   35.05 -57.00-150.00   87
 10  \w     17.00 103.00   1.00  100.00    --   35.05  57.00 -60.00   86
 11  \w      1.00  30.00   1.00  100.00    --   35.05  88.00  45.38   29
 12  \w     -1.00  29.00   1.00  100.00    --   35.05  90.00-178.21   30
 13  \w     11.00  96.00   1.00  100.00    --   35.05-135.00 146.00   85
 14  \w     17.00 103.00   1.00  100.00    --   35.05  57.00  90.00   86
 15  \w     13.00 106.00   1.00  100.00    --   35.05  38.00-120.00   93
 16  \w      2.00 107.00   1.00  100.00    --   35.05  22.00 156.63  105
 17  \w     39.00 109.00   1.00  100.00    --   35.05 178.00 120.00   70
 18  \w     11.00 103.00   1.00  100.00    --   35.05  68.00-159.47   92
 19  \w    -36.00 106.00   1.00  100.00    --   35.05   0.00-180.00  142
 20  \w    -36.00  46.00   1.00  100.00    --   35.05   0.00-150.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0922
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            50550
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.201
_diffrn_reflns_theta_min         2.993
_exptl_absorpt_coefficient_mu    0.320
_exptl_absorpt_correction_T_max  0.82668
_exptl_absorpt_correction_T_min  0.82383
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_description       cylindrically
_exptl_crystal_F_000             216
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.159
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 1494 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.839
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         4538
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.839
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0270
_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^)+(0.0311P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0555
_reflns_Friedel_coverage         0.916
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3600
_reflns_number_total             4538
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -169.1438\% 
 around [0.02 1.00 -0.02] (reciprocal) or [0.06 1.00 -0.02] (direct)
;
_cod_data_source_file            d4sc00936c3.cif
_cod_data_source_block           compound_1
_cod_depositor_comments
'Adding full bibliography for 1571189--1571190.cif.'
_cod_database_code               1571189
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.883
_olex2_refinement_description
;
;
_shelx_res_checksum              94147
_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
;