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_7131904
_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         'C49 H63 N2 P Si, C7 H8'
_chemical_formula_sum            'C56 H71 N2 P Si'
_chemical_formula_weight         831.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-08-17
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_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                 115.1440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.6045(3)
_cell_length_b                   18.8105(6)
_cell_length_c                   11.9676(3)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      27.102
_cell_measurement_theta_min      2.220
_cell_volume                     2364.82(12)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker Instrument Service vV6.2.14'
_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 0.999
_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  0.0242
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28644
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.111
_diffrn_reflns_theta_min         2.165
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7058
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1380 before and 0.0428 after correction.
The Ratio of minimum to maximum transmission is 0.9467.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_description       block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 4068 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         9836
_refine_ls_number_restraints     196
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0587P)^2^+0.7937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_full    0.923
_reflns_Friedel_fraction_max     0.880
_reflns_number_gt                9489
_reflns_number_total             9836
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02512h2.cif
_cod_data_source_block           mo_220816_ly_wcf0815_0m
_cod_database_code               7131904
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.944
_olex2_refinement_description
;
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. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4.a Ternary CH refined with riding coordinates:
 C46(H46), C43(H43), C48(H48), C34(H34), C31(H31), C36(H36)
4.b Secondary CH2 refined with riding coordinates:
 C42(H42A,H42B), C49(H49A,H49B), C47(H47A,H47B), C45(H45A,H45B), C40(H40A,
 H40B), C44(H44A,H44B), C50(H50A,H50B), C39(H39A,H39B), C37(H37A,H37B),
 C35(H35A,H35B), C32(H32A,H32B), C33(H33A,H33B)
4.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C26(H26), C22(H22), C19(H19), C5(H5), C27(H27), C57(H57), C1(H1),
 C20(H20), C21(H21), C28(H28), C23(H23), C4(H4), C29(H29), C3(H3), C2(H2),
 C53(H53), C54(H54), C56(H56), C55(H55)
4.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C13(H13A,H13B,
 H13C), C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              1232
_shelx_hkl_checksum              89644
_olex2_submission_special_instructions 'No special instructions were received'