Reactivities of phosphaalkynes towards diverse bis-silylenes.
Sun, Xiaofei; Jin, Da; Maier, Stefanie; Hinz, Alexander; Roesky, Peter W.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10220–10225; doi:10.1039/d4dt01367k

data_7716302
_publ_section_title
;
 Reactivities of phosphaalkynes towards diverse bis-silylenes.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10220
_journal_page_last               10225
_journal_paper_doi               10.1039/d4dt01367k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C37 H65 B10 N4 P Si2, 0.5(C6 H18 O Si2)'
_chemical_formula_sum            'C40 H74 B10 N4 O0.5 P Si3'
_chemical_formula_weight         842.37
_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             2024-03-25
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-04 deposited with the CCDC.	2024-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.297(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5007(17)
_cell_length_b                   19.956(3)
_cell_length_c                   21.117(3)
_cell_measurement_reflns_used    14283
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.17
_cell_measurement_theta_min      1.93
_cell_volume                     4832.9(12)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)
;
_computing_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.1, Darmstadt 2022
;
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
 280 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0817
_diffrn_reflns_av_unetI/netI     0.1214
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23166
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         1.934
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  0.9950
_exptl_absorpt_correction_T_min  0.9937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         8735
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1517
_refine_ls_R_factor_gt           0.0803
_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^)+(0.0940P)^2^+9.6880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1776
_refine_ls_wR_factor_ref         0.2178
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5069
_reflns_number_total             8735
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01367k2.cif
_cod_data_source_block           xf-sibsi-tbucp
_cod_depositor_comments
'Adding full bibliography for 7716299--7716302.cif.'
_cod_original_cell_volume        4832.8(12)
_cod_original_formula_sum        'C40 H74 B10 N4 O0.50 P Si3'
_cod_database_code               7716302
_shelx_shelxl_version_number     2019/2
_audit_contact_author
;
      Prof. Dr. Peter W. Roesky
      Karlsruher Institut fuer Technologie (KIT), CS
      Institut fuer Anorganische Chemie (AOC)
      Lehrstuhl fuer Anorganische Funktionsmaterialien
      Engesserstr. 15, Geb. 30.45
      76131 Karlsruhe 
      Bundesrepublik Deutschland
;
_audit_contact_letter
;
;
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.949
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si3-O \\sim Si4-O
 with sigma of 0.02
 Si3-C40 \\sim Si4-C41
 with sigma of 0.02
 C40-O \\sim C41-O
 with sigma of 0.04
 Si3-C39 \\sim Si4-C43
 with sigma of 0.02
 C39-O \\sim C43-O
 with sigma of 0.04
 C38-O \\sim C42-O
 with sigma of 0.04
 Si3-C38 \\sim Si4-C42
 with sigma of 0.02
 C40-C39 \\sim C41-C43
 with sigma of 0.04
 C40-C38 \\sim C41-C42
 with sigma of 0.04
 C39-C38 \\sim C43-C42
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C38 \\sim C38 \\sim C39 \\sim C39 \\sim C40 \\sim C40 \\sim C41 \\sim C41 \\sim
C42 \\sim C42 \\sim C43 \\sim C43 \\sim O \\sim O \\sim Si3 \\sim Si3 \\sim Si4
\\sim Si4: within 2.5A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2.5A
Uanis(Si3) = Uanis(Si4)
4. Others
 Fixed Sof: C38(0.5) H38A(0.5) H38B(0.5) H38C(0.5) C39(0.5) H39A(0.5)
 H39B(0.5) H39C(0.5) C40(0.5) H40A(0.5) H40B(0.5) H40C(0.5) C41(0.5) H41A(0.5)
 H41B(0.5) H41C(0.5) C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5) C43(0.5) H43A(0.5)
 H43B(0.5) H43C(0.5) O(0.5) Si3(0.5) Si4(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33)
5.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C)
5.c Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3), B4(H4), B5(H5), B6(H6), B7(H7), B8(H8), B9(H9),
 B10(H10)
;
_shelx_res_checksum              60360
_shelx_hkl_checksum              49527
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '40.0 mm'
_stoe_detector_pixelsize_x       '0.172 mm'
_stoe_detector_pixelsize_y       '0.172 mm'
_stoe_detector_size_x            '7.0 cm'
_stoe_detector_size_y            '8.4 cm'
_stoe_evaluation_integration_a   5.0
_stoe_evaluation_integration_b   -2.0
_stoe_evaluation_integration_ems 0.015
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 83.6
_stoe_evaluation_lana_dxs_max_order 1
_stoe_evaluation_lana_dys_max_order 1
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 63.1
_stoe_evaluation_lana_max_2theta_desired 63.1
_stoe_evaluation_lana_mean_redundancy 2.3
_stoe_evaluation_lana_number_refls_after_or 31364
_stoe_evaluation_lana_number_refls_outliers 5343
_stoe_evaluation_lana_number_refls_total 36707
_stoe_evaluation_lana_number_refls_unique 13550
_stoe_evaluation_lana_number_refls_written 31364
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group 2/m
_stoe_evaluation_lana_table
;
2Theta           6.1   12.9   19.7   26.5   33.3   40.1   46.9   53.7   60.5
<Resolution>    5.39   3.06   2.02   1.55   1.23   1.03   0.89   0.79   0.72
N(total)         311   1159   2722   4324   5285   6681   7389   7209   1627
<Redundancy>     3.6    3.4    3.7    3.3    2.7    2.5    2.2    1.9    1.2
Complet. [%%]   100.0  100.0  100.0   99.8   99.9  100.0   99.9   95.0   35.9
<I/sigma>       83.7   36.2   14.5    9.5    5.8    3.1    1.5    0.9    0.4
R(int)         0.050  0.029  0.039  0.053  0.079  0.140  0.253  0.356  0.590
;
_stoe_measurement_identifier     XF-SiBSi-tBuCP
_stoe_measurement_max_exposure_per_frame '90.0 s'
_stoe_measurement_mean_exposure_per_frame '90.0 s'
_stoe_measurement_min_exposure_per_frame '90.0 s'
_stoe_measurement_total_exposure_time '7.0 h'
_stoe_measurement_total_frame_number 280
_stoe_measurement_total_run_number 4
_stoe_measurement_tube_power     '50.0 W'