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_7127933
_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         'C31 H42 N2 P2'
_chemical_formula_sum            'C31 H42 N2 P2'
_chemical_formula_weight         504.60
_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             2020-04-15
_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                93.857(2)
_cell_angle_beta                 95.926(2)
_cell_angle_gamma                110.711(2)
_cell_formula_units_Z            4
_cell_length_a                   8.5803(2)
_cell_length_b                   10.6253(2)
_cell_length_c                   35.5315(8)
_cell_measurement_reflns_used    9226
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.3780
_cell_measurement_theta_min      3.7630
_cell_volume                     2995.01(12)
_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      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3546
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.959
_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    -74.00  26.00   1.00   10.00    --  -41.60  77.00 -90.00  100
  2  \w     18.00 113.00   1.00   10.00    --   41.60  57.00 150.00   95
  3  \w    -26.00  68.00   1.00   10.00    --   41.60 -57.00   0.00   94
  4  \w     38.00  77.00   1.00   41.00    --  106.46 -45.00-120.00   39
  5  \w     40.00 109.00   1.00   41.00    --  106.46 -94.00 -90.00   69
  6  \w     30.00  69.00   1.00   41.00    --  106.46 -30.00 150.00   39
  7  \w     46.00  77.00   1.00   41.00    --  106.46 -45.00 -30.00   31
  8  \w     41.00  99.00   1.00   41.00    --  106.46 -94.00-150.00   58
  9  \w     31.00  60.00   1.00   41.00    --  106.46 -30.00-150.00   29
 10  \w     33.00 121.00   1.00   41.00    --  106.46-125.00-150.00   88
 11  \w     43.00 109.00   1.00   41.00    --  106.46 -94.00   0.00   66
 12  \w     31.00 103.00   1.00   41.00    --  106.46 -94.00  90.00   72
 13  \w     77.00 158.00   1.00   41.00    --  106.46  61.00 -30.00   81
 14  \w     36.00  63.00   1.00   41.00    --  106.46 -30.00-180.00   27
 15  \w     78.00 148.00   1.00   41.00    --  106.46  61.00 120.00   70
 16  \w     39.00  66.00   1.00   41.00    --  106.46 -30.00 -60.00   27
 17  \w     27.00 154.00   1.00   41.00    --  106.46 -15.00 -30.00  127
;
_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      -0.1324738000
_diffrn_orient_matrix_UB_12      -0.0282701000
_diffrn_orient_matrix_UB_13      -0.0353568000
_diffrn_orient_matrix_UB_21      -0.1377250000
_diffrn_orient_matrix_UB_22      -0.0171372000
_diffrn_orient_matrix_UB_23      0.0259252000
_diffrn_orient_matrix_UB_31      0.0319888000
_diffrn_orient_matrix_UB_32      0.1524377000
_diffrn_orient_matrix_UB_33      0.0013644000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            20271
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.537
_diffrn_reflns_theta_min         3.776
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.458
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.845
_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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       plate
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         11591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0560P)^2^+1.3656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1317
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9222
_reflns_number_total             11591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07103j2.cif
_cod_data_source_block           gh436b_p
_cod_depositor_comments
'Adding full bibliography for 7127930--7127935.cif.'
_cod_original_cell_volume        2995.00(12)
_cod_database_code               7127933
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C31 H42 N2 P2'
_chemical_oxdiff_usercomment     'from n-hexane'
_reflns_odcompleteness_completeness 99.17
_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:
 C56(H56), C47(H47), C49(H49), C58(H58), C13(H13), C12(H12), C16(H16),
 C18(H18), C27(H27), C25(H25), C43(H43), C44(H44)
2.b Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C40(H40A,H40B,H40C), C51(H51A,H51B,H51C), C53(H53A,H53B,
 H53C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C62(H62A,H62B,H62C), C52(H52A,
 H52B,H52C), C22(H22A,H22B,H22C), C35(H35A,H35B,H35C), C61(H61A,H61B,H61C),
 C29(H29A,H29B,H29C), C36(H36A,H36B,H36C), C41(H41A,H41B,H41C), C20(H20A,H20B,
 H20C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C6(H6A,H6B,H6C), C9(H9A,H9B,
 H9C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C21(H21A,H21B,H21C),
 C10(H10A,H10B,H10C)
;
_shelx_res_checksum              51153
_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 1.282
_oxdiff_exptl_absorpt_empirical_full_min 0.793