#------------------------------------------------------------------------------
#$Date: 2020-04-05 13:03:10 +0300 (Sun, 05 Apr 2020) $
#$Revision: 250172 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/61/7126160.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7126160
loop_
_publ_author_name
'Kunzmann, Robert'
'Omatsu, Yamato'
'Schnakenburg, Gregor'
'Espinosa Ferao, Arturo'
'Yanagisawa, Tatsuya'
'Tokitoh, Norihiro'
'Streubel, Rainer'
_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_absolute_configuration ad
_chemical_formula_moiety         'C19 H34 N O7 P Si3 W'
_chemical_formula_sum            'C19 H34 N O7 P Si3 W'
_chemical_formula_weight         687.56
_chemical_name_systematic        RK-459
_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     heavy
_audit_creation_date             2018-10-24
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9978(4)
_cell_length_b                   13.3597(5)
_cell_length_c                   21.3413(9)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.82
_cell_measurement_theta_min      2.44
_cell_volume                     2850.5(2)
_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 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25714
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.992
_diffrn_reflns_theta_min         1.798
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.270
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.4896
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1224 before and 0.0463 after correction. The Ratio of minimum to maximum transmission is 0.6561. The λ/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    1.602
_exptl_crystal_description       needle
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.494(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         6863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0196
_refine_ls_R_factor_gt           0.0175
_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/[σ²(Fo²)+(0.0155P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0363
_refine_ls_wR_factor_ref         0.0371
_reflns_Friedel_coverage         0.785
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6586
_reflns_number_total             6863
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0cc00024h2.cif
_cod_data_source_block           5779f
_cod_depositor_comments
'Adding full bibliography for 7126158--7126160.cif.'
_cod_database_code               7126160
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.883
_shelx_estimated_absorpt_t_min   0.415
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.506(5)
 0.494(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C8(H8)
3.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W W 0.46044(2) 0.48167(2) 0.68878(2) 0.01585(4) Uani 1 1 d . . . . .
P P 0.67375(8) 0.49284(7) 0.62873(4) 0.01430(18) Uani 1 1 d . . . . .
Si1 Si 0.87216(10) 0.63533(8) 0.66039(5) 0.0178(2) Uani 1 1 d . . . . .
Si2 Si 0.83244(11) 0.29558(8) 0.62901(5) 0.0213(2) Uani 1 1 d . . . . .
Si3 Si 0.77568(11) 0.40375(8) 0.49703(5) 0.0187(2) Uani 1 1 d . . . . .
O1 O 0.8119(2) 0.5196(2) 0.66568(11) 0.0185(5) Uani 1 1 d . . . . .
O2 O 0.5793(2) 0.6257(2) 0.54389(12) 0.0212(6) Uani 1 1 d . . . . .
O3 O 0.1891(3) 0.4709(3) 0.76422(14) 0.0346(7) Uani 1 1 d . . . . .
O4 O 0.4736(3) 0.24418(19) 0.68900(14) 0.0274(6) Uani 1 1 d . . . . .
O5 O 0.3053(3) 0.4697(2) 0.55876(12) 0.0263(6) Uani 1 1 d . . . . .
O6 O 0.4200(3) 0.7174(2) 0.67628(15) 0.0335(8) Uani 1 1 d . . . . .
O7 O 0.6253(3) 0.5010(3) 0.81615(13) 0.0436(8) Uani 1 1 d . . . . .
N N 0.7687(3) 0.6779(2) 0.59851(15) 0.0171(6) Uani 1 1 d . . . . .
C1 C 0.6699(4) 0.6112(3) 0.58119(16) 0.0159(7) Uani 1 1 d . . . . .
C2 C 1.0520(4) 0.6281(3) 0.64158(18) 0.0234(8) Uani 1 1 d . . . . .
H2A H 1.0632 0.6093 0.5975 0.035 Uiso 1 1 calc GR . . . .
H2B H 1.0947 0.5777 0.6683 0.035 Uiso 1 1 calc GR . . . .
H2C H 1.0938 0.6934 0.6489 0.035 Uiso 1 1 calc GR . . . .
C3 C 0.8384(4) 0.6977(4) 0.73593(19) 0.0286(10) Uani 1 1 d . . . . .
H3A H 0.8769 0.6580 0.7701 0.043 Uiso 1 1 calc GR . . . .
H3B H 0.7416 0.7038 0.7420 0.043 Uiso 1 1 calc GR . . . .
H3C H 0.8789 0.7645 0.7358 0.043 Uiso 1 1 calc GR . . . .
C4 C 0.7707(4) 0.7812(3) 0.5706(2) 0.0241(9) Uani 1 1 d . . . . .
C5 C 0.8975(4) 0.8350(3) 0.5925(2) 0.0283(9) Uani 1 1 d . . . . .
H5A H 0.9762 0.8011 0.5753 0.042 Uiso 1 1 calc GR . . . .
H5B H 0.9018 0.8338 0.6384 0.042 Uiso 1 1 calc GR . . . .
H5C H 0.8958 0.9046 0.5780 0.042 Uiso 1 1 calc GR . . . .
C6 C 0.6480(4) 0.8387(3) 0.5931(3) 0.0377(12) Uani 1 1 d . . . . .
H6A H 0.6466 0.8400 0.6390 0.057 Uiso 1 1 calc GR . . . .
H6B H 0.5669 0.8058 0.5776 0.057 Uiso 1 1 calc GR . . . .
H6C H 0.6515 0.9074 0.5771 0.057 Uiso 1 1 calc GR . . . .
C7 C 0.7746(5) 0.7750(3) 0.4987(2) 0.0340(11) Uani 1 1 d . . . . .
H7A H 0.6930 0.7425 0.4835 0.051 Uiso 1 1 calc GR . . . .
H7B H 0.8527 0.7358 0.4857 0.051 Uiso 1 1 calc GR . . . .
H7C H 0.7808 0.8426 0.4812 0.051 Uiso 1 1 calc GR . . . .
C8 C 0.7198(4) 0.3848(3) 0.58224(17) 0.0166(7) Uani 1 1 d . . . . .
H8 H 0.6340 0.3469 0.5781 0.020 Uiso 1 1 calc R . . . .
C9 C 0.8134(4) 0.3041(3) 0.71653(19) 0.0279(10) Uani 1 1 d . . . . .
H9A H 0.7181 0.3045 0.7274 0.042 Uiso 1 1 calc GR . . . .
H9B H 0.8554 0.3659 0.7316 0.042 Uiso 1 1 calc GR . . . .
H9C H 0.8567 0.2463 0.7362 0.042 Uiso 1 1 calc GR . . . .
C10 C 0.7828(5) 0.1652(3) 0.6074(2) 0.0339(11) Uani 1 1 d . . . . .
H10A H 0.7940 0.1557 0.5621 0.051 Uiso 1 1 calc GR . . . .
H10B H 0.6890 0.1541 0.6187 0.051 Uiso 1 1 calc GR . . . .
H10C H 0.8395 0.1173 0.6299 0.051 Uiso 1 1 calc GR . . . .
C11 C 1.0128(4) 0.3218(3) 0.6128(2) 0.0267(9) Uani 1 1 d . . . . .
H11A H 1.0360 0.3882 0.6289 0.040 Uiso 1 1 calc GR . . . .
H11B H 1.0286 0.3197 0.5675 0.040 Uiso 1 1 calc GR . . . .
H11C H 1.0683 0.2711 0.6334 0.040 Uiso 1 1 calc GR . . . .
C12 C 0.8378(5) 0.2839(3) 0.4624(2) 0.0305(10) Uani 1 1 d . . . . .
H12A H 0.7687 0.2323 0.4664 0.046 Uiso 1 1 calc GR . . . .
H12B H 0.9187 0.2625 0.4845 0.046 Uiso 1 1 calc GR . . . .
H12C H 0.8586 0.2942 0.4179 0.046 Uiso 1 1 calc GR . . . .
C13 C 0.9125(4) 0.4971(3) 0.49043(17) 0.0258(9) Uani 1 1 d . . . . .
H13A H 0.9905 0.4738 0.5142 0.039 Uiso 1 1 calc GR . . . .
H13B H 0.8823 0.5614 0.5074 0.039 Uiso 1 1 calc GR . . . .
H13C H 0.9371 0.5053 0.4463 0.039 Uiso 1 1 calc GR . . . .
C14 C 0.6291(5) 0.4424(3) 0.44941(18) 0.0308(10) Uani 1 1 d . . . . .
H14A H 0.5982 0.5084 0.4633 0.046 Uiso 1 1 calc GR . . . .
H14B H 0.5569 0.3935 0.4546 0.046 Uiso 1 1 calc GR . . . .
H14C H 0.6548 0.4458 0.4051 0.046 Uiso 1 1 calc GR . . . .
C15 C 0.2879(4) 0.4745(3) 0.73720(17) 0.0231(8) Uani 1 1 d . . . . .
C16 C 0.4711(4) 0.3294(3) 0.68976(18) 0.0199(7) Uani 1 1 d . . . . .
C17 C 0.3616(3) 0.4727(3) 0.60509(17) 0.0184(7) Uani 1 1 d . . . . .
C18 C 0.4382(4) 0.6343(3) 0.68195(18) 0.0218(8) Uani 1 1 d . . . . .
C19 C 0.5662(4) 0.4936(3) 0.77097(17) 0.0276(9) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C15 W P 179.29(13) . . ?
C15 W C16 89.54(17) . . ?
C15 W C17 91.79(14) . . ?
C15 W C18 89.48(16) . . ?
C15 W C19 90.38(15) . . ?
C16 W P 91.17(11) . . ?
C16 W C17 88.61(16) . . ?
C16 W C18 175.25(16) . . ?
C16 W C19 92.40(17) . . ?
C17 W P 88.16(10) . . ?
C17 W C18 86.78(16) . . ?
C17 W C19 177.61(15) . . ?
C18 W P 89.81(10) . . ?
C19 W P 89.66(10) . . ?
C19 W C18 92.25(16) . . ?
O1 P W 119.29(9) . . ?
O1 P C1 95.39(16) . . ?
O1 P C8 102.97(16) . . ?
C1 P W 108.10(12) . . ?
C8 P W 116.84(13) . . ?
C8 P C1 112.33(16) . . ?
O1 Si1 N 97.91(14) . . ?
O1 Si1 C2 108.61(16) . . ?
O1 Si1 C3 107.12(17) . . ?
N Si1 C2 115.09(17) . . ?
N Si1 C3 113.52(18) . . ?
C2 Si1 C3 113.06(19) . . ?
C9 Si2 C8 114.78(17) . . ?
C10 Si2 C8 107.2(2) . . ?
C10 Si2 C9 105.9(2) . . ?
C11 Si2 C8 110.69(18) . . ?
C11 Si2 C9 105.7(2) . . ?
C11 Si2 C10 112.6(2) . . ?
C12 Si3 C8 111.04(18) . . ?
C13 Si3 C8 112.03(17) . . ?
C13 Si3 C12 107.46(19) . . ?
C13 Si3 C14 110.7(2) . . ?
C14 Si3 C8 108.98(18) . . ?
C14 Si3 C12 106.5(2) . . ?
P O1 Si1 118.55(16) . . ?
C1 N Si1 114.2(2) . . ?
C1 N C4 119.8(3) . . ?
C4 N Si1 125.6(3) . . ?
O2 C1 P 120.0(3) . . ?
O2 C1 N 127.0(3) . . ?
N C1 P 112.6(3) . . ?
N C4 C5 108.7(3) . . ?
N C4 C6 109.1(3) . . ?
N C4 C7 110.2(3) . . ?
C5 C4 C7 108.0(3) . . ?
C6 C4 C5 109.5(3) . . ?
C6 C4 C7 111.2(4) . . ?
P C8 Si2 111.05(19) . . ?
P C8 Si3 119.24(19) . . ?
Si3 C8 Si2 113.79(19) . . ?
O3 C15 W 179.3(4) . . ?
O4 C16 W 177.8(4) . . ?
O5 C17 W 178.5(4) . . ?
O6 C18 W 176.3(4) . . ?
O7 C19 W 179.3(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W P 2.4926(9) . ?
W C15 2.013(4) . ?
W C16 2.038(4) . ?
W C17 2.045(4) . ?
W C18 2.056(4) . ?
W C19 2.054(4) . ?
P O1 1.630(2) . ?
P C1 1.879(4) . ?
P C8 1.810(4) . ?
Si1 O1 1.664(3) . ?
Si1 N 1.772(3) . ?
Si1 C2 1.845(4) . ?
Si1 C3 1.846(4) . ?
Si2 C8 1.920(4) . ?
Si2 C9 1.881(4) . ?
Si2 C10 1.869(5) . ?
Si2 C11 1.869(4) . ?
Si3 C8 1.919(4) . ?
Si3 C12 1.870(4) . ?
Si3 C13 1.856(4) . ?
Si3 C14 1.857(4) . ?
O2 C1 1.221(4) . ?
O3 C15 1.145(4) . ?
O4 C16 1.138(4) . ?
O5 C17 1.138(4) . ?
O6 C18 1.132(5) . ?
O7 C19 1.135(5) . ?
N C1 1.380(5) . ?
N C4 1.503(5) . ?
C4 C5 1.531(6) . ?
C4 C6 1.525(6) . ?
C4 C7 1.537(6) . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.506(5)
2 0.494(5)
