#------------------------------------------------------------------------------
#$Date: 2022-02-11 01:48:56 +0200 (Fri, 11 Feb 2022) $
#$Revision: 272905 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/94/7709458.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_7709458
loop_
_publ_author_name
'Brehm, Philipp'
'Müller-Feyen , Anne Sophie'
'Schnakenburg, Gregor'
'Streubel, R.'
_publ_section_title
;
 1,3,2-Diheterophospholane complexes: access to new tuneable precursors of
 phosphanoxyl complexes and P-functional polymers
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00027J
_journal_year                    2022
_chemical_formula_moiety         'C11 H13 O7 P W'
_chemical_formula_sum            'C11 H13 O7 P W'
_chemical_formula_weight         472.03
_chemical_name_systematic        PB-213
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-01-03 deposited with the CCDC.	2022-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                99.282(3)
_cell_angle_beta                 101.783(3)
_cell_angle_gamma                91.016(3)
_cell_formula_units_Z            2
_cell_length_a                   7.0371(3)
_cell_length_b                   10.1674(4)
_cell_length_c                   10.6647(4)
_cell_measurement_reflns_used    33982
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.60
_cell_measurement_theta_min      2.58
_cell_volume                     736.17(5)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS-2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25605
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.994
_diffrn_reflns_theta_min         2.961
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    7.980
_exptl_absorpt_correction_T_max  0.3962
_exptl_absorpt_correction_T_min  0.1271
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XRed32 V1.53'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.129
_exptl_crystal_description       block
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.470
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       0.0082(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0156
_refine_ls_R_factor_gt           0.0147
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0101P)²+0.4086P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0347
_refine_ls_wR_factor_ref         0.0350
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3474
_reflns_number_total             3563
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt00027j3.cif
_cod_data_source_block           6b
_cod_database_code               7709458
_shelx_shelxl_version_number     2017/1
_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   0.448
_shelx_estimated_absorpt_t_min   0.401
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 0.28740(2) 0.26397(2) 0.87609(2) 0.01180(4) Uani 1 1 d . . . . .
P P 0.12936(7) 0.22776(5) 0.64791(5) 0.01264(10) Uani 1 1 d . . . . .
H H -0.061(5) 0.200(3) 0.616(3) 0.031(8) Uiso 1 1 d . . . . .
O1 O 0.2052(2) 0.11674(15) 0.54472(15) 0.0158(3) Uani 1 1 d . . . . .
O2 O 0.1477(2) 0.35212(15) 0.57355(15) 0.0142(3) Uani 1 1 d . . . . .
O3 O 0.5149(3) 0.33163(18) 1.16897(17) 0.0229(3) Uani 1 1 d . . . . .
O4 O 0.4351(3) -0.03099(19) 0.8429(2) 0.0322(4) Uani 1 1 d . . . . .
O5 O 0.6681(3) 0.3672(2) 0.79609(19) 0.0281(4) Uani 1 1 d . . . . .
O6 O 0.1105(3) 0.55118(17) 0.89807(19) 0.0245(4) Uani 1 1 d . . . . .
O7 O -0.0812(3) 0.15079(19) 0.9639(2) 0.0298(4) Uani 1 1 d . . . . .
C1 C 0.2491(3) 0.1733(2) 0.4342(2) 0.0134(4) Uani 1 1 d . . . . .
C2 C 0.1319(3) 0.3026(2) 0.4339(2) 0.0137(4) Uani 1 1 d . . . . .
C3 C 0.4678(3) 0.2018(2) 0.4621(2) 0.0190(4) Uani 1 1 d . . . . .
H3A H 0.506437 0.270073 0.539989 0.028 Uiso 1 1 calc GR . . . .
H3B H 0.504182 0.233913 0.387964 0.028 Uiso 1 1 calc GR . . . .
H3C H 0.533902 0.119803 0.476430 0.028 Uiso 1 1 calc GR . . . .
C4 C 0.1840(4) 0.0697(2) 0.3132(2) 0.0204(4) Uani 1 1 d . . . . .
H4A H 0.264252 -0.007730 0.319148 0.031 Uiso 1 1 calc GR . . . .
H4B H 0.198077 0.108021 0.236702 0.031 Uiso 1 1 calc GR . . . .
H4C H 0.047468 0.041741 0.305214 0.031 Uiso 1 1 calc GR . . . .
C5 C 0.2204(3) 0.4125(2) 0.3799(2) 0.0184(4) Uani 1 1 d . . . . .
H5A H 0.139766 0.490011 0.384294 0.028 Uiso 1 1 calc GR . . . .
H5B H 0.226921 0.380330 0.289232 0.028 Uiso 1 1 calc GR . . . .
H5C H 0.351715 0.438160 0.431212 0.028 Uiso 1 1 calc GR . . . .
C6 C -0.0814(3) 0.2759(2) 0.3688(2) 0.0203(4) Uani 1 1 d . . . . .
H6A H -0.135804 0.202311 0.401802 0.030 Uiso 1 1 calc GR . . . .
H6B H -0.093847 0.251999 0.274631 0.030 Uiso 1 1 calc GR . . . .
H6C H -0.152187 0.356339 0.388037 0.030 Uiso 1 1 calc GR . . . .
C7 C 0.4312(3) 0.3055(2) 1.0641(2) 0.0158(4) Uani 1 1 d . . . . .
C8 C 0.3845(3) 0.0752(2) 0.8562(2) 0.0196(4) Uani 1 1 d . . . . .
C9 C 0.5306(3) 0.3319(2) 0.8235(2) 0.0181(4) Uani 1 1 d . . . . .
C10 C 0.1758(3) 0.4494(2) 0.8904(2) 0.0164(4) Uani 1 1 d . . . . .
C11 C 0.0481(3) 0.1921(2) 0.9314(2) 0.0184(4) 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'
O O 0.0106 0.0060 '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
C7 W P 175.76(6) . . ?
C7 W C8 91.60(9) . . ?
C7 W C9 88.57(9) . . ?
C7 W C10 90.70(9) . . ?
C7 W C11 90.57(9) . . ?
C8 W P 90.52(7) . . ?
C8 W C9 89.79(9) . . ?
C8 W C10 176.96(9) . . ?
C8 W C11 88.88(9) . . ?
C9 W P 87.77(7) . . ?
C9 W C10 92.25(9) . . ?
C9 W C11 178.40(8) . . ?
C10 W P 87.31(7) . . ?
C10 W C11 89.11(9) . . ?
C11 W P 93.14(7) . . ?
O1 P W 120.36(6) . . ?
O2 P W 115.41(6) . . ?
O2 P O1 96.57(8) . . ?
C1 O1 P 112.07(12) . . ?
C2 O2 P 109.49(12) . . ?
O1 C1 C2 103.97(15) . . ?
O1 C1 C3 106.93(17) . . ?
O1 C1 C4 107.61(16) . . ?
C3 C1 C2 113.11(17) . . ?
C4 C1 C2 113.73(19) . . ?
C4 C1 C3 110.88(18) . . ?
O2 C2 C1 102.70(16) . . ?
O2 C2 C5 106.41(17) . . ?
O2 C2 C6 109.01(16) . . ?
C5 C2 C1 114.54(16) . . ?
C5 C2 C6 110.13(18) . . ?
C6 C2 C1 113.43(18) . . ?
O3 C7 W 178.12(19) . . ?
O4 C8 W 178.5(2) . . ?
O5 C9 W 178.2(2) . . ?
O6 C10 W 178.67(19) . . ?
O7 C11 W 178.3(2) . . ?
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 2.4260(6) . ?
W C7 2.026(2) . ?
W C8 2.042(2) . ?
W C9 2.048(2) . ?
W C10 2.050(2) . ?
W C11 2.054(2) . ?
P O1 1.6217(16) . ?
P O2 1.6136(15) . ?
O1 C1 1.476(2) . ?
O2 C2 1.474(3) . ?
O3 C7 1.139(3) . ?
O4 C8 1.140(3) . ?
O5 C9 1.134(3) . ?
O6 C10 1.137(3) . ?
O7 C11 1.135(3) . ?
C1 C2 1.564(3) . ?
C1 C3 1.520(3) . ?
C1 C4 1.513(3) . ?
C2 C5 1.516(3) . ?
C2 C6 1.519(3) . ?
