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_7127931
_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         'C37 H54 N2 P2'
_chemical_formula_sum            'C37 H54 N2 P2'
_chemical_formula_weight         588.76
_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             2020-06-12
_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                 92.7130(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8598(2)
_cell_length_b                   18.0388(3)
_cell_length_c                   17.3344(2)
_cell_measurement_reflns_used    11850
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.2320
_cell_measurement_theta_min      4.9050
_cell_volume                     3704.31(10)
_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 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_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   -113.00 -28.00   1.00    1.00    --  -41.42 -77.00 -90.00   85
  2  \w     37.00  86.00   1.00    1.00    --   41.42  37.00-180.00   49
  3  \w     -9.00  82.00   1.00    1.00    --   41.42 -99.00 120.00   91
  4  \w     52.00  99.00   1.00    4.00    --  106.46 -94.00 -30.00   47
  5  \w     30.00  69.00   1.00    4.00    --  106.46 -30.00-120.00   39
  6  \w     82.00 117.00   1.00    4.00    --  106.46  45.00  90.00   35
  7  \w     33.00  58.00   1.00    4.00    --  106.46 -30.00   0.00   25
  8  \w     52.00 108.00   1.00    4.00    --  106.46-125.00 120.00   56
  9  \w     34.00  68.00   1.00    4.00    --  106.46 -30.00 -90.00   34
 10  \w     37.00  73.00   1.00    4.00    --  106.46 -45.00  60.00   36
 11  \w     49.00  75.00   1.00    4.00    --  106.46 -45.00-150.00   26
 12  \w     84.00 116.00   1.00    4.00    --  106.46-125.00-180.00   32
 13  \w     30.00  55.00   1.00    4.00    --  106.46 -30.00 -60.00   25
 14  \w     74.00 147.00   1.00    4.00    --  106.46  77.00-150.00   73
 15  \w     32.00  59.00   1.00    4.00    --  106.46 -30.00 150.00   27
 16  \w    114.00 156.00   1.00    4.00    --  106.46  45.00   0.00   42
 17  \w     31.00 101.00   1.00    4.00    --  106.46 -94.00-180.00   70
;
_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      0.0480844000
_diffrn_orient_matrix_UB_12      0.0675685000
_diffrn_orient_matrix_UB_13      0.0448387000
_diffrn_orient_matrix_UB_21      0.0735434000
_diffrn_orient_matrix_UB_22      -0.0518236000
_diffrn_orient_matrix_UB_23      0.0520097000
_diffrn_orient_matrix_UB_31      0.0958611000
_diffrn_orient_matrix_UB_32      0.0059374000
_diffrn_orient_matrix_UB_33      -0.0566497000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16465
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.399
_diffrn_reflns_theta_min         3.538
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.238
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.263
_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    1.056
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.702
_exptl_crystal_size_mid          0.372
_exptl_crystal_size_min          0.279
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         7280
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0509P)^2^+1.0787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.0987
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6722
_reflns_number_total             7280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07103j2.cif
_cod_data_source_block           gh431a_2_mp
_cod_depositor_comments
'Adding full bibliography for 7127930--7127935.cif.'
_cod_original_cell_volume        3704.30(10)
_cod_database_code               7127931
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C37 H54 N2 P2'
_chemical_oxdiff_usercomment     'from n-hexane'
_reflns_odcompleteness_completeness 99.93
_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
 C4-C3 \\sim C4A-C3 \\sim C6A-C3 \\sim C6-C3 \\sim C5A-C3 \\sim C5-C3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C6A \\sim C6 \\sim C4 \\sim C4A \\sim C5 \\sim C5A: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
4. Others
 Fixed Sof: C4(0.8) H4A(0.8) H4B(0.8) H4C(0.8) C5(0.8) H5A(0.8) H5B(0.8)
 H5C(0.8) C6(0.8) H6A(0.8) H6B(0.8) H6C(0.8) C6A(0.2) H6AA(0.2) H6AB(0.2)
 H6AC(0.2) C5A(0.2) H5AA(0.2) H5AB(0.2) H5AC(0.2) C4A(0.2) H4AA(0.2) H4AB(0.2)
 H4AC(0.2)
5.a Ternary CH refined with riding coordinates:
 C00I(H00I), C23(H23), C32(H32), C35(H35)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C16(H16), C18(H18), C13(H13), C17(H17), C28(H28), C30(H30), C29(H29)
5.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C21(H21A,H21B,H21C), C9(H9A,H9B,H9C), C25(H25A,H25B,
 H25C), C22(H22A,H22B,H22C), C34(H34A,H34B,H34C), C10(H10A,H10B,H10C), C33(H33A,
 H33B,H33C), C8(H8A,H8B,H8C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C36(H36A,H36B,
 H36C), C6(H6A,H6B,H6C), C37(H37A,H37B,H37C), C6A(H6AA,H6AB,H6AC), C5A(H5AA,
 H5AB,H5AC), C4A(H4AA,H4AB,H4AC)
;
_shelx_res_checksum              40691
_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 1.267
_oxdiff_exptl_absorpt_empirical_full_min 0.802