SiP-heterocycles derived from a bulky phosphanylsilylene
Li, Yan; Wang, Chenfeng; Su, Ming-Der; Fang, Zijie; Zhou, Jiahao; Zhang, Haoqi; Li, Xiaodi; Zuo, Darui; Zhang, Zheng-Feng; Chemical Communications  (2023) –; doi:10.1039/D3CC02512H

data_7131902
_publ_section_title
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 SiP-heterocycles derived from a bulky phosphanylsilylene
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC02512H
_journal_year                    2023
_chemical_formula_moiety         'C35 H53 N2 P Si'
_chemical_formula_sum            'C35 H53 N2 P Si'
_chemical_formula_weight         560.85
_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             2022-02-22
_audit_creation_method
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Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
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_audit_update_record
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2022-11-30 deposited with the CCDC.	2023-07-20 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 100.716(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8037(13)
_cell_length_b                   8.7396(5)
_cell_length_c                   18.1837(10)
_cell_measurement_reflns_used    6805
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      26.422
_cell_measurement_theta_min      2.652
_cell_volume                     3248.4(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      170.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1099
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            55442
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.100
_diffrn_reflns_theta_min         2.312
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1217 before and 0.0728 after correction.
The Ratio of minimum to maximum transmission is 0.8704.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         7136
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0401P)^2^+1.5844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1203
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4922
_reflns_number_total             7136
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02512h2.cif
_cod_data_source_block           mo_220222_ly_lr0221_2_2
_cod_database_code               7131902
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.973
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C39-C7 \\sim C1-C7
 with sigma of 0.02
 C40-C38 \\sim C5-C6
 with sigma of 0.02
 C4-C5 \\sim C38-C37
 with sigma of 0.02
 C2-C1 \\sim C39-C36
 with sigma of 0.02
 C6-C1 \\sim C39-C40
 with sigma of 0.02
 C3-C2 \\sim C36-C0
 with sigma of 0.02
 C0-C37 \\sim C4-C3
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C1, C6, C5, C4, C7, C3, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C0, C7, C39, C40, C38, C37, C36
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Others
 Sof(C0)=Sof(H0)=Sof(C39)=Sof(C40)=Sof(H40)=Sof(C38)=Sof(H38)=Sof(C37)=
 Sof(H37)=Sof(C36)=Sof(H36)=1-FVAR(1)
 Sof(C1)=Sof(C6)=Sof(H6)=Sof(C5)=Sof(H5)=Sof(C4)=Sof(H4)=Sof(C3)=Sof(H3)=
 Sof(C2)=Sof(H2)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C17(H17), C22(H22), C20(H20), C30(H30), C33(H33), C28(H28)
5.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C19(H19A,H19B), C16(H16A,H16B), C18(H18A,H18B), C21(H21A,
 H21B), C23(H23A,H23B), C31(H31A,H31B), C34(H34A,H34B), C32(H32A,H32B),
 C29(H29A,H29B), C35(H35A,H35B), C27(H27A,H27B)
5.c Aromatic/amide H refined with riding coordinates:
 C0(H0), C6(H6), C5(H5), C4(H4), C40(H40), C38(H38), C37(H37), C3(H3), C2(H2),
 C36(H36)
5.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C15(H15A,H15B,
 H15C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C)
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_shelx_res_checksum              65403
_shelx_hkl_checksum              72406
_olex2_submission_special_instructions 'No special instructions were received'