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_7716301
_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         'C49 H73 Cl Ga Ge N4 P, 1.5(C6 D6)'
_chemical_formula_sum            'C58 H73 Cl D9 Ga Ge N4 P'
_chemical_formula_weight         1053.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-07
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-04-04 deposited with the CCDC.	2024-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.909(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   45.9880(12)
_cell_length_b                   12.9413(2)
_cell_length_c                   20.6901(5)
_cell_measurement_reflns_used    67320
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.14
_cell_measurement_theta_min      2.96
_cell_volume                     11342.4(5)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_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 1.84, Darmstadt 2018
;
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
 703 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    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            84476
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.971
_diffrn_source                   Axo_Mo
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    1.119
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2433
_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    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4424
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.068
_refine_diff_density_max         1.760
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         11118
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0710P)^2^+37.2963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1389
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8170
_reflns_number_total             11118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01367k2.cif
_cod_data_source_block           xf487a
_cod_depositor_comments
'Adding full bibliography for 7716299--7716302.cif.'
_cod_database_code               7716301
_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
;
;
_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
 C1-C2 \\sim C1-C2A
 with sigma of 0.02
 C2-C4 \\sim C2A-C3A
 with sigma of 0.02
 C2-C5 \\sim C2A-C4A
 with sigma of 0.02
 C2-C3 \\sim C2A-C5A
 with sigma of 0.02
 C1-C4 \\sim C1-C3A
 with sigma of 0.04
 C1-C5 \\sim C1-C4A
 with sigma of 0.04
 C1-C3 \\sim C1-C5A
 with sigma of 0.04
 C4-C5 \\sim C3A-C4A
 with sigma of 0.04
 C4-C3 \\sim C3A-C5A
 with sigma of 0.04
 C5-C3 \\sim C4A-C5A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C2 \\sim C2A \\sim C3 \\sim C3A \\sim C4 \\sim C4A \\sim C5 \\sim C5A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(C2A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=
 Sof(H4AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=1-FVAR(1)
 Sof(C2)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C27(H27), C30(H30), C44(H44), C47(H47)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C23(H23), C24(H24),
 C25(H25), C34(H34), C40(H40), C41(H41), C42(H42), C50(D50), C51(D51), C52(D52),
  C53(D53), C54(D54), C55(D55), C56(D56), C57(D57), C58(D58)
5.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC), C4(H4A,H4B,H4C), C4A(H4AA,H4AB,H4AC),
 C5(H5A,H5B,H5C), C5A(H5AA,H5AB,H5AC), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              27471
_shelx_hkl_checksum              22654
_olex2_submission_special_instructions 'No special instructions were received'