A synthetic equivalent for unknown 1,3-zwitterions? - A K/OR phosphinidenoid complex with an additional Si-Cl function.
Kunzmann, Robert; Omatsu, Yamato; Schnakenburg, Gregor; Espinosa Ferao, Arturo; Yanagisawa, Tatsuya; Tokitoh, Norihiro; Streubel, Rainer; Chemical communications (Cambridge, England) 56 (2020) 3899–3902; doi:10.1039/d0cc00024h

data_7126159
_publ_section_title
;
 A synthetic equivalent for unknown 1,3-zwitterions? - A K/OR
 phosphinidenoid complex with an additional Si-Cl function.
;
_journal_issue                   27
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3899
_journal_page_last               3902
_journal_paper_doi               10.1039/d0cc00024h
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C17 H34 N O6 P Si4 W'
_chemical_formula_sum            'C17 H34 N O6 P Si4 W'
_chemical_formula_weight         675.63
_chemical_name_systematic        RK-485
_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   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2019-02-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2019-11-06 deposited with the CCDC.	2020-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.193(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.8672(11)
_cell_length_b                   16.5104(11)
_cell_length_c                   22.0806(15)
_cell_measurement_reflns_used    9149
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.15
_cell_measurement_theta_min      2.47
_cell_volume                     5783.3(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            80534
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.284
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.244
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4169
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1481 before and 0.0595 after correction. The Ratio of minimum to maximum transmission is 0.5588. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       plate
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.093
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         13954
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0179P)^2^+5.7306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0542
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12104
_reflns_number_total             13954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00024h2.cif
_cod_data_source_block           5881f
_cod_depositor_comments
'Adding full bibliography for 7126158--7126160.cif.'
_cod_database_code               7126159
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.920
_shelx_estimated_absorpt_t_min   0.225
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1-H1
 1.07 with sigma of 0.001
3. Rigid bond restraints
 Si4', C10'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(O1') \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C1') \\sim Ueq, Uanis(N'S) \\sim Ueq, Uanis(N') \\sim Ueq, Uanis(C1'S)
\\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C10') \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
5. Others
 Sof(C1'S)=Sof(H1'S)=Sof(N'S)=1-FVAR(1)
 Sof(N')=Sof(C1')=Sof(H1')=FVAR(1)
 Sof(O1S)=1-FVAR(2)
 Sof(O1)=FVAR(2)
 Sof(O1'S)=1-FVAR(3)
 Sof(O1')=FVAR(3)
6.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,
 H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10D,H10E,
 H10F), C11(H11D,H11E,H11F), C12(H12D,H12E,H12F), C2'(H2'A,H2'B,H2'C), C3'(H3'A,
 H3'B,H3'C), C4'(H4'A,H4'B,H4'C), C5'(H5'A,H5'B,H5'C), C6'(H6'A,H6'B,H6'C),
 C7'(H7'A,H7'B,H7'C), C8'(H8'A,H8'B,H8'C), C9'(H9'A,H9'B,H9'C), C10'(H10A,H10B,
 H10C), C11'(H11A,H11B,H11C), C12'(H12A,H12B,H12C)
;
_shelx_res_checksum              97908
_olex2_submission_special_instructions 'No special instructions were received'