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_7131907
_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         'C57 H83 N2 P3 Si, C7 H8'
_chemical_formula_sum            'C64 H91 N2 P3 Si'
_chemical_formula_weight         1009.38
_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             2022-05-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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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.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.041(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.369(3)
_cell_length_b                   23.579(5)
_cell_length_c                   19.827(5)
_cell_measurement_reflns_used    9755
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.09
_cell_measurement_theta_min      2.40
_cell_volume                     5726(2)
_computing_cell_refinement       'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.14'
_computing_data_reduction        'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'zju Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1173
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            104984
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.366
_diffrn_reflns_theta_min         2.247
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1702 before and 0.1114 after correction.
The Ratio of minimum to maximum transmission is 0.6366.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_description       block
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         12688
_refine_ls_number_restraints     237
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0702
_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^)+(0.0722P)^2^+9.1110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1728
_refine_ls_wR_factor_ref         0.1860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10023
_reflns_number_total             12688
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02512h2.cif
_cod_data_source_block           mo_220511_ly_wcf0509_1_0m
_cod_database_code               7131907
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.968
_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
 C58-C63 \\sim C58A-C63A
 with sigma of 0.02
 C58-C59 \\sim C58A-C59A
 with sigma of 0.02
 C63-C62 \\sim C63A-C62A
 with sigma of 0.02
 C63-C64 \\sim C63A-C64A
 with sigma of 0.02
 C62-C61 \\sim C62A-C61A
 with sigma of 0.02
 C61-C60 \\sim C61A-C60A
 with sigma of 0.02
 C60-C59 \\sim C60A-C59A
 with sigma of 0.02
 C58-C62 \\sim C58A-C62A
 with sigma of 0.04
 C58-C60 \\sim C58A-C60A
 with sigma of 0.04
 C58-C64 \\sim C58A-C64A
 with sigma of 0.04
 C63-C61 \\sim C63A-C61A
 with sigma of 0.04
 C63-C59 \\sim C63A-C59A
 with sigma of 0.04
 C62-C60 \\sim C62A-C60A
 with sigma of 0.04
 C62-C64 \\sim C62A-C64A
 with sigma of 0.04
 C61-C59 \\sim C61A-C59A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C58A
\\sim C59A \\sim C60A \\sim C61A \\sim C62A \\sim C63A \\sim C64A: within 2A
with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Others
 Sof(C58A)=Sof(H58A)=Sof(C59A)=Sof(H59A)=Sof(C60A)=Sof(H60A)=Sof(C61A)=
 Sof(H61A)=Sof(C62A)=Sof(H62A)=Sof(C63A)=Sof(C64A)=Sof(H64D)=Sof(H64E)=
 Sof(H64F)=1-FVAR(1)
 Sof(C58)=Sof(H58)=Sof(C63)=Sof(C62)=Sof(H62)=Sof(C61)=Sof(H61)=Sof(C60)=
 Sof(H60)=Sof(C59)=Sof(H59)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C19(H19), C21(H21), C24(H24), C30(H30), C32(H32), C35(H35), C40(H40),
 C42(H42), C45(H45), C50(H50), C52(H52), C55(H55)
5.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C20(H20A,H20B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,
 H25B), C26(H26A,H26B), C29(H29A,H29B), C31(H31A,H31B), C33(H33A,H33B),
 C34(H34A,H34B), C36(H36A,H36B), C37(H37A,H37B), C39(H39A,H39B), C41(H41A,H41B),
  C43(H43A,H43B), C44(H44A,H44B), C46(H46A,H46B), C47(H47A,H47B), C49(H49A,
 H49B), C51(H51A,H51B), C53(H53A,H53B), C54(H54A,H54B), C56(H56A,H56B),
 C57(H57A,H57B)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C58(H58), C62(H62), C61(H61),
 C60(H60), C59(H59), C58A(H58A), C59A(H59A), C60A(H60A), C61A(H61A), C62A(H62A)
5.d Fitted hexagon refined as free rotating group:
 C58(C63,C62,C61,C60,C59)
5.e Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C64(H64A,H64B,H64C), C64A(H64D,H64E,
 H64F)
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_shelx_res_checksum              99900
_shelx_hkl_checksum              86401
_olex2_submission_special_instructions 'No special instructions were received'