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_7131906
_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_absolute_configuration ad
_chemical_formula_moiety         'C49 H63 N2 P Si'
_chemical_formula_sum            'C49 H63 N2 P Si'
_chemical_formula_weight         739.07
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-10-15
_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.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.281(3)
_cell_length_b                   16.693(3)
_cell_length_c                   18.753(4)
_cell_measurement_reflns_used    2716
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      37.518
_cell_measurement_theta_min      3.083
_cell_volume                     4157.5(15)
_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 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.1479
_diffrn_reflns_av_unetI/netI     0.1843
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31628
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         56.999
_diffrn_reflns_theta_min         3.083
_diffrn_source_current           2.85
_diffrn_source_power             0.1992435
_diffrn_source_voltage           69.91
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.6398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0908 before and 0.0787 after correction.
The Ratio of minimum to maximum transmission is 0.8517.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_description       needle
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details
;
 Flack x determined using 1334 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.12(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         8461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1517
_refine_ls_R_factor_gt           0.0837
_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^)+(0.0994P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1914
_refine_ls_wR_factor_ref         0.2414
_reflns_Friedel_coverage         0.794
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                4681
_reflns_number_total             8461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02512h2.cif
_cod_data_source_block           221009_ly_wcf1008_0m
_cod_original_cell_volume        4157.4(14)
_cod_database_code               7131906
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.986
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C27(H27), C25(H25), C19(H19), C22(H22), C23(H23), C14(H14), C12(H12), C16(H16)
2.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C18(H18A,H18B), C24(H24A,H24B), C26(H26A,H26B), C17(H17A,
 H17B), C46(H46A,H46B), C45(H45A,H45B), C11(H11A,H11B), C20(H20A,H20B),
 C15(H15A,H15B), C13(H13A,H13B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C40(H40), C42(H42), C38(H38), C34(H34), C29(H29), C1(H1A), C37(H37),
 C36(H36), C28(H28), C5(H5), C35(H35), C2(H2), C3(H3), C4(H4)
2.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C33(H33A,H33B,H33C),
 C32(H32A,H32B,H32C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              54608
_shelx_hkl_checksum              73040
_olex2_submission_special_instructions 'No special instructions were received'