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_7127934
_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         'C34 H46 N2 O2 P2'
_chemical_formula_sum            'C33.85 H45.56 N2 O2 P2'
_chemical_formula_weight         574.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 94.086(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4310(12)
_cell_length_b                   8.6721(7)
_cell_length_c                   20.5999(13)
_cell_measurement_reflns_used    3894
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      72.3580
_cell_measurement_theta_min      4.2820
_cell_volume                     3284.2(4)
_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 0.943
_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     30.00 117.00   1.00   55.00    --   42.41  37.00  60.00   87
  2  \w    -28.00  69.00   1.00   55.00    --   42.41 -77.00 -90.00   97
  3  \w     32.00  64.00   1.00  215.00    --  104.40 -61.00 176.00   32
  4  \w     80.00 154.00   1.00  215.00    --  104.40  61.00-120.00   74
  5  \w     32.00  62.00   1.00  215.00    --  104.40 -61.00-120.00   30
  6  \w     36.00  96.00   1.00  215.00    --  104.40 -77.00   0.00   60
  7  \w     28.00  68.00   1.00  215.00    --  104.40 -77.00 -60.00   40
  8  \w     84.00 149.00   1.00  215.00    --  104.40  77.00 -30.00   65
  9  \w     28.00 104.00   1.00  215.00    --  104.40 -77.00  90.00   76
;
_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      -0.0299456000
_diffrn_orient_matrix_UB_12      -0.1561281000
_diffrn_orient_matrix_UB_13      0.0216387000
_diffrn_orient_matrix_UB_21      0.0662206000
_diffrn_orient_matrix_UB_22      -0.0188758000
_diffrn_orient_matrix_UB_23      0.0493499000
_diffrn_orient_matrix_UB_31      -0.0416954000
_diffrn_orient_matrix_UB_32      0.0824985000
_diffrn_orient_matrix_UB_33      0.0521750000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_unetI/netI     0.1153
_diffrn_reflns_Laue_measured_fraction_full 0.943
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9705
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.067
_diffrn_reflns_theta_max         67.067
_diffrn_reflns_theta_min         4.303
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.436
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.602
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.21a (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    1.162
_exptl_crystal_description       plate
_exptl_crystal_F_000             1235
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.298
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         5526
_refine_ls_number_restraints     169
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1502
_refine_ls_R_factor_gt           0.0830
_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^)+(0.0523P)^2^+9.7502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1821
_refine_ls_wR_factor_ref         0.2086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3265
_reflns_number_total             5526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07103j2.cif
_cod_data_source_block           ghmu015_4
_cod_depositor_comments
'Adding full bibliography for 7127930--7127935.cif.'
_cod_database_code               7127934
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C34 H43 N2 O2 P2'
_chemical_oxdiff_usercomment     'crystals from C6H6-n-hex'
_reflns_odcompleteness_completeness 94.14
_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. Restrained distances
 P1B-P2B \\sim P1A-P2A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C3 \\sim C6A \\sim C4A \\sim C5A \\sim C6B \\sim C4B \\sim C5B: within 1.7A
with sigma of 0.2 and sigma for terminal atoms of 0.2
C1A \\sim C2A \\sim C1B \\sim C2B: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.02
C8B \\sim C10A \\sim C10B \\sim C7B \\sim C7A \\sim C8A \\sim C9A \\sim C9B:
within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.02
4. Others
 Sof(P2B)=Sof(P1B)=Sof(C2B)=Sof(C1B)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(H8BC)=
 Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=Sof(C10B)=Sof(H10D)=Sof(H10E)=Sof(H10F)=
 Sof(C7B)=1-FVAR(1)
 Sof(P2A)=Sof(P1A)=Sof(C7A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C2A)=
 Sof(C1A)=Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=
 Sof(H8AC)=FVAR(1)
 Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(H6BC)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(H4BC)=
 Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(H5BC)=1-FVAR(2)
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=
 Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C30(H30), C28(H28), C19(H19), C21(H21)
5.b Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C32(H32A,H32B,
 H32C), C23(H23A,H23B,H23C), C33(H33A,H33B,H33C), C25(H25A,H25B,H25C), C9A(H9AA,
 H9AB,H9AC), C24(H24A,H24B,H24C), C10A(H10A,H10B,H10C), C6A(H6AA,H6AB,H6AC),
 C4A(H4AA,H4AB,H4AC), C8A(H8AA,H8AB,H8AC), C5A(H5AA,H5AB,H5AC), C6B(H6BA,H6BB,
 H6BC), C4B(H4BA,H4BB,H4BC), C5B(H5BA,H5BB,H5BC), C8B(H8BA,H8BB,H8BC), C9B(H9BA,
 H9BB,H9BC), C10B(H10D,H10E,H10F)
;
_shelx_res_checksum              52668
_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 2.146
_oxdiff_exptl_absorpt_empirical_full_min 0.502