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_7127930
_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         'C20 H22 N4'
_chemical_formula_sum            'C20 H23 N4'
_chemical_formula_weight         319.42
_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                87.935(3)
_cell_angle_beta                 77.417(4)
_cell_angle_gamma                73.219(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0986(3)
_cell_length_b                   9.9827(4)
_cell_length_c                   11.1882(4)
_cell_measurement_reflns_used    3924
_cell_measurement_temperature    151(40)
_cell_measurement_theta_max      72.6550
_cell_measurement_theta_min      4.6050
_cell_volume                     844.85(6)
_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      151(40)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.943
_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    -55.00  34.00   1.00    1.00    --  -42.04  77.00  90.00   89
  2  \w   -114.00 -14.00   1.00    1.00    --  -42.04 -57.00 -30.00  100
  3  \w      6.00  75.00   1.00    1.00    --   42.04-125.00 -90.00   69
  4  \w     82.00 146.00   1.00    1.50    --  104.40  77.00 -30.00   64
  5  \w     32.00 112.00   1.00    1.50    --  104.40-125.00  60.00   80
  6  \w     26.00 106.00   1.00    1.50    --  104.40 -94.00-180.00   80
  7  \w     75.00 140.00   1.00    1.50    --  104.40  61.00  60.00   65
  8  \w     80.00 155.00   1.00    1.50    --  104.40  45.00 -90.00   75
  9  \w     31.00 112.00   1.00    1.50    --  104.40-125.00   0.00   81
 10  \w     30.00 106.00   1.00    1.50    --  104.40 -94.00  90.00   76
 11  \w     92.00 157.00   1.00    1.50    --  104.40  45.00-150.00   65
 12  \w     77.00 148.00   1.00    1.50    --  104.40  30.00 150.00   71
 13  \w     43.00  68.00   1.00    1.50    --  104.40 -61.00  90.00   25
 14  \w     32.00 106.00   1.00    1.50    --  104.40 -77.00-150.00   74
;
_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      -0.1892792000
_diffrn_orient_matrix_UB_12      0.0748447000
_diffrn_orient_matrix_UB_13      0.0694506000
_diffrn_orient_matrix_UB_21      -0.0669768000
_diffrn_orient_matrix_UB_22      0.0006679000
_diffrn_orient_matrix_UB_23      -0.1188306000
_diffrn_orient_matrix_UB_31      -0.0333302000
_diffrn_orient_matrix_UB_32      -0.1428312000
_diffrn_orient_matrix_UB_33      0.0312567000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5328
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.681
_diffrn_reflns_theta_min         4.628
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.241
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       plate
_exptl_crystal_F_000             342
_exptl_crystal_size_max          0.567
_exptl_crystal_size_mid          0.404
_exptl_crystal_size_min          0.145
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3156
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0904P)^2^+0.4271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1590
_refine_ls_wR_factor_ref         0.1629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2908
_reflns_number_total             3156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07103j2.cif
_cod_data_source_block           gh_mu009_p
_cod_depositor_comments
'Adding full bibliography for 7127930--7127935.cif.'
_cod_database_code               7127930
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C20 H16 N18 '
_chemical_oxdiff_usercomment     'crystals from n-hexane'
_reflns_odcompleteness_completeness 97.15
_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. Uiso/Uaniso restraints and constraints
N1B \\sim N2B \\sim N2A \\sim N1A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.01
3. Others
 Sof(N1B)=Sof(N2B)=1-FVAR(1)
 Sof(N2A)=Sof(N1A)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C18(H18), C20(H20), C13(H13), C14(H14), C19(H19), C11(H11),
 C17(H17), C12(H12), C16(H16)
4.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              45690
_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 1.313
_oxdiff_exptl_absorpt_empirical_full_min 0.841