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_7131903
_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         'C46 H65 N2 P Si'
_chemical_formula_sum            'C46 H65 N2 P Si'
_chemical_formula_weight         705.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-10-26
_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                87.154(3)
_cell_angle_beta                 73.572(2)
_cell_angle_gamma                67.701(3)
_cell_formula_units_Z            2
_cell_length_a                   11.1312(7)
_cell_length_b                   11.1624(7)
_cell_length_c                   18.2271(11)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      71.699
_cell_measurement_theta_min      3.732
_cell_volume                     2005.6(2)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      170.00
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21618
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.900
_diffrn_reflns_theta_min         2.203
_diffrn_source_current           2.86
_diffrn_source_power             0.19994259999999997
_diffrn_source_voltage           69.91
_exptl_absorpt_coefficient_mu    0.737
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1219 before and 0.0621 after correction.
The Ratio of minimum to maximum transmission is 0.7763.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         7208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0709
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0891P)^2^+2.8440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1840
_refine_ls_wR_factor_ref         0.1899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5857
_reflns_number_total             7208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02512h2.cif
_cod_data_source_block           221025_ly_wcf1024_1_2nd_0m
_cod_database_code               7131903
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.867
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C20(H20), C19(H19), C18(H18), C16(H16), C2(H2), C12(H12), C32(H32), C7(H7),
 C6(H6)
1.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C10(H10A,H10B), C4(H4A,H4B), C9(H9A,H9B), C14(H14A,H14B),
 C17(H17A,H17B), C11(H11A,H11B), C3(H3A,H3B), C1(H1A,H1B), C13(H13A,H13B),
 C8(H8A,H8B)
1.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C41(H41), C38(H38), C37(H37), C42(H42), C21(H21), C36(H36), C43(H43),
 C23(H23), C35(H35)
1.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C31(H31A,
 H31B,H31C)
;
_shelx_res_checksum              49591
_shelx_hkl_checksum              1677
_olex2_submission_special_instructions 'No special instructions were received'