Di-<i>tert</i>-butyldiphosphatetrahedrane as a building block for phosphaalkenes and phosphirenes.
Hierlmeier, Gabriele; Uttendorfer, Maria K.; Wolf, Robert; Chemical communications (Cambridge, England) 57 (2021) 2356–2359; doi:10.1039/d0cc07103j

data_7127932
_publ_section_title
;
 Di-<i>tert</i>-butyldiphosphatetrahedrane as a building block for
 phosphaalkenes and phosphirenes.
;
_journal_issue                   19
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2356
_journal_page_last               2359
_journal_paper_doi               10.1039/d0cc07103j
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C14 H17 N3 S'
_chemical_formula_sum            'C14 H17 N3 S'
_chemical_formula_weight         259.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-23 deposited with the CCDC.	2020-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                87.680(3)
_cell_angle_beta                 88.235(3)
_cell_angle_gamma                72.214(3)
_cell_formula_units_Z            4
_cell_length_a                   7.5819(2)
_cell_length_b                   12.0396(4)
_cell_length_c                   15.5332(6)
_cell_measurement_reflns_used    6440
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      72.6720
_cell_measurement_theta_min      3.8370
_cell_volume                     1348.79(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.989
_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    -98.00 -11.00   1.00    1.00    --  -42.29 125.00  90.00   87
  2  \w    -38.00  26.00   1.00    1.00    --   42.29 -19.00-150.00   64
  3  \w      1.00 122.00   1.00    1.00    --   42.29  19.00  30.00  121
  4  \w     23.00  86.00   1.00    2.50    --  104.40 -94.00-180.00   63
  5  \w     34.00 120.00   1.00    2.50    --  104.40-135.00 175.00   86
  6  \w     33.00  71.00   1.00    2.50    --  104.40 -61.00  60.00   38
  7  \w     34.00  71.00   1.00    2.50    --  104.40 -61.00 -90.00   37
  8  \w     32.00 107.00   1.00    2.50    --  104.40-125.00  30.00   75
  9  \w     35.00 111.00   1.00    2.50    --  104.40-125.00 -90.00   76
 10  \w     79.00 152.00   1.00    2.50    --  104.40  45.00  60.00   73
 11  \w     81.00 142.00   1.00    2.50    --  104.40  45.00-150.00   61
 12  \w     83.00 108.00   1.00    2.50    --  104.40  77.00 150.00   25
 13  \w    112.00 158.00   1.00    2.50    --  104.40  77.00 150.00   46
 14  \w     39.00 102.00   1.00    2.50    --  104.40 -94.00 -90.00   63
 15  \w     52.00 158.00   1.00    2.50    --  104.40  15.00 -30.00  106
 16  \w     43.00 106.00   1.00    2.50    --  104.40 -77.00   0.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0073219000
_diffrn_orient_matrix_UB_12      0.0661272000
_diffrn_orient_matrix_UB_13      -0.0874772000
_diffrn_orient_matrix_UB_21      0.0200514000
_diffrn_orient_matrix_UB_22      -0.1136314000
_diffrn_orient_matrix_UB_23      -0.0469436000
_diffrn_orient_matrix_UB_31      -0.2123581000
_diffrn_orient_matrix_UB_32      0.0281519000
_diffrn_orient_matrix_UB_33      0.0005162000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9306
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.746
_diffrn_reflns_theta_min         3.858
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.004
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.574
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.21a (Rigaku Oxford Diffraction, 2019)
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 light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       plate
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.413
_exptl_crystal_size_mid          0.244
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         5154
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0538P)^2^+0.3522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4650
_reflns_number_total             5154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07103j2.cif
_cod_data_source_block           ghmu004_2_p
_cod_depositor_comments
'Adding full bibliography for 7127930--7127935.cif.'
_cod_database_code               7127932
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C14H17N3S
_chemical_oxdiff_usercomment     'crystals from tol/n-hex'
_reflns_odcompleteness_completeness 99.07
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C24(H24), C28(H28), C10(H10), C13(H13), C12(H12), C11(H11),
 C25(H25), C27(H27), C26(H26)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C19(H19A,
 H19B,H19C), C22(H22A,H22B,H22C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              73368
_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 1.551
_oxdiff_exptl_absorpt_empirical_full_min 0.842