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_7127935
_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         'C24 H42 N4 P2'
_chemical_formula_sum            'C24 H42 N4 P2'
_chemical_formula_weight         448.55
_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             2020-04-16
_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                90
_cell_angle_beta                 94.152(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7329(4)
_cell_length_b                   8.3859(2)
_cell_length_c                   19.9061(4)
_cell_measurement_reflns_used    5413
_cell_measurement_temperature    290(13)
_cell_measurement_theta_max      73.7300
_cell_measurement_theta_min      4.3880
_cell_volume                     2619.41(11)
_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      air
_diffrn_ambient_temperature      290(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_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  -2.00   1.00   10.00    --  -42.68 125.00 150.00   96
  2  \w    -22.00  18.00   1.00   10.00    --  -42.68  41.00 -37.00   40
  3  \w   -111.00 -20.00   1.00   10.00    --  -42.68 -57.00  30.00   91
  4  \w     83.00 146.00   1.00   40.00    --  106.63  30.00 150.00   63
  5  \w     37.00 138.00   1.00   40.00    --  106.63 -77.00  30.00  101
  6  \w     40.00  67.00   1.00   40.00    --  106.63 -30.00 120.00   27
  7  \w     32.00  67.00   1.00   40.00    --  106.63 -30.00 -60.00   35
  8  \w     32.00  57.00   1.00   40.00    --  106.63 -30.00 -30.00   25
  9  \w     43.00  69.00   1.00   40.00    --  106.63 -30.00  30.00   26
 10  \w     38.00  67.00   1.00   40.00    --  106.63 -30.00-120.00   29
 11  \w     35.00  65.00   1.00   40.00    --  106.63 -45.00 120.00   30
 12  \w    107.00 138.00   1.00   40.00    --  106.63  45.00 -90.00   31
 13  \w     32.00  59.00   1.00   40.00    --  106.63 -30.00 150.00   27
 14  \w     34.00  66.00   1.00   40.00    --  106.63 -30.00 -90.00   32
 15  \w     35.00  60.00   1.00   40.00    --  106.63 -45.00  30.00   25
 16  \w     98.00 155.00   1.00   40.00    --  106.63  45.00  60.00   57
;
_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      0.0923622000
_diffrn_orient_matrix_UB_12      0.0359920000
_diffrn_orient_matrix_UB_13      -0.0162088000
_diffrn_orient_matrix_UB_21      0.0041814000
_diffrn_orient_matrix_UB_22      -0.1614949000
_diffrn_orient_matrix_UB_23      -0.0365626000
_diffrn_orient_matrix_UB_31      -0.0331151000
_diffrn_orient_matrix_UB_32      0.0797773000
_diffrn_orient_matrix_UB_33      -0.0664770000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            11361
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.069
_diffrn_reflns_theta_min         4.454
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.624
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.666
_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    1.137
_exptl_crystal_description       prism
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.210
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         5186
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0610P)^2^+0.4562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1143
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4273
_reflns_number_total             5186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07103j2.cif
_cod_data_source_block           gh436c_mp
_cod_depositor_comments
'Adding full bibliography for 7127930--7127935.cif.'
_cod_database_code               7127935
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C24 H42 N4 P2'
_chemical_oxdiff_usercomment     'yellow prisms from C6D6 reaction mixture'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C21(H21A,H21B,H21C), C11(H11A,H11B,H11C), C17(H17A,H17B,
 H17C), C10(H10A,H10B,H10C), C22(H22A,H22B,H22C), C18(H18A,H18B,H18C), C12(H12A,
 H12B,H12C), C00P(H00A,H00B,H00C), C15(H15A,H15B,H15C), C7(H7A,H7B,H7C), C6(H6A,
 H6B,H6C), C8(H8A,H8B,H8C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              89925
_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 1.349
_oxdiff_exptl_absorpt_empirical_full_min 0.835