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_1571190
_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         '3(C15 H23 N O2 P2), C6 H14'
_chemical_formula_sum            'C51 H83 N3 O6 P6'
_chemical_formula_weight         1020.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-02
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-02 deposited with the CCDC.	2024-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.2530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.79270(10)
_cell_length_b                   27.0421(3)
_cell_length_c                   26.5278(2)
_cell_measurement_reflns_used    28526
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.7250
_cell_measurement_theta_min      2.3010
_cell_volume                     5556.97(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.955
_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     25.00  99.00   0.50    0.70    --   62.52   0.00  90.00  148
  2  \w     48.00 118.00   0.50    0.70    --   75.28  15.00   0.00  140
  3  \w     33.00 103.00   0.50    0.70    --   62.52  15.00 -30.00  140
  4  \w     72.00  99.00   0.50    0.70    --   73.14 144.00 158.00   54
  5  \w     67.00  92.00   0.50    0.70    --   75.28 144.00 158.00   50
  6  \w     32.00  84.00   0.50    0.70    --   75.28-125.00 120.00  104
  7  \w     51.00  76.00   0.50    0.70    --   75.28-144.00 105.00   50
  8  \w     49.00  74.00   0.50    0.70    --   73.14-144.00 105.00   50
  9  \w     53.00  79.00   0.50    0.70    --   62.52-144.00 105.00   52
 10  \w     80.00 105.00   0.50    0.70    --   75.28-127.00 -85.00   50
 11  \w     43.00  92.00   0.50    0.70    --   62.52-127.00 -85.00   98
 12  \w     35.00  70.00   0.50    0.70    --   75.28-127.00 -85.00   70
 13  \w     42.00  67.00   0.50    0.70    --   73.14-127.00 -85.00   50
 14  \w     33.00  87.00   0.50    0.70    --   73.14-125.00 -60.00  108
 15  \w     43.00  91.00   0.50    0.70    --   62.52-125.00 -30.00   96
 16  \w     39.00  65.00   0.50    0.70    --   75.28-125.00 -30.00   52
 17  \w     76.00 104.00   0.50    0.70    --   75.28-125.00 -30.00   56
 18  \w     36.00 104.00   0.50    0.70    --   75.28-125.00  30.00  136
 19  \w     30.00  91.00   0.50    0.70    --   62.52-125.00  30.00  122
 20  \w   -107.00 -36.00   0.50    0.70    --  -70.22   0.00  30.00  142
 21  \w    -88.00 -63.00   0.50    0.70    --  -63.96 144.00 158.00   50
 22  \w    -94.00 -69.00   0.50    0.70    --  -70.22 144.00 158.00   50
 23  \w    -94.00 -47.00   0.50    0.70    --  -70.22 125.00  90.00   94
 24  \w    -99.00 -32.00   0.50    0.70    --  -70.22 127.00 -10.00  134
 25  \w    -81.00 -56.00   0.50    0.70    --  -63.96 127.00 -10.00   50
 26  \w   -110.00 -61.00   0.50    0.70    --  -70.22-144.00 105.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0022992000
_diffrn_orient_matrix_UB_12      -0.0380980000
_diffrn_orient_matrix_UB_13      -0.0432822000
_diffrn_orient_matrix_UB_21      -0.0167482000
_diffrn_orient_matrix_UB_22      0.0422263000
_diffrn_orient_matrix_UB_23      -0.0391812000
_diffrn_orient_matrix_UB_31      0.1981534000
_diffrn_orient_matrix_UB_32      0.0030797000
_diffrn_orient_matrix_UB_33      0.0025662000
_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  0.0214
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            50947
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.173
_diffrn_reflns_theta_min         2.340
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.178
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.602
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.81a (Rigaku Oxford Diffraction, 2020)
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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_description       block
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.063
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         10640
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0496P)^2^+4.4967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1041
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9786
_reflns_number_total             10640
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc00936c3.cif
_cod_data_source_block           gh576'_mc_smallcell
_cod_depositor_comments
'Adding full bibliography for 1571189--1571190.cif.'
_cod_database_code               1571190
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C17 H27.7 N O2 P2'
_chemical_oxdiff_usercomment     'crystals from n-hexane'
_reflns_odcompleteness_completeness 99.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C27(H27), C26(H26), C11(H11), C41(H41), C42(H42), C12(H12)
2.b Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C50(H50A,H50B), C47(H47A,H47B), C48(H48A,H48B)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C45(H45A,H45B,H45C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C),
 C30(H30A,H30B,H30C), C25(H25A,H25B,H25C), C10(H10A,H10B,H10C), C6(H6A,H6B,H6C),
  C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C4(H4A,H4B,H4C), C24(H24A,H24B,
 H24C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C8(H8A,H8B,H8C), C34(H34A,
 H34B,H34C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C36(H36A,H36B,H36C),
 C35(H35A,H35B,H35C), C40(H40A,H40B,H40C), C46(H46A,H46B,H46C), C51(H51A,H51B,
 H51C)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.478
_oxdiff_exptl_absorpt_empirical_full_min 0.769