#------------------------------------------------------------------------------
#$Date: 2022-05-11 01:51:28 +0300 (Wed, 11 May 2022) $
#$Revision: 275309 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/02/7710222.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_7710222
loop_
_publ_author_name
'Gildenast, Hans'
'Gruszien, Lukas'
'Friedt, Felix'
'Englert, Ulli'
_publ_section_title
;
 Phosphorus or nitrogen -- the first phosphatriptycene in coordination
 polymer chemistry
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00728B
_journal_year                    2022
_chemical_formula_moiety         'C29 H20 Au Cl N P Si'
_chemical_formula_sum            'C29 H20 Au Cl N P Si'
_chemical_formula_weight         673.94
_chemical_name_common            6
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-03-01 deposited with the CCDC.	2022-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.483(3)
_cell_angle_beta                 101.156(3)
_cell_angle_gamma                104.033(3)
_cell_formula_units_Z            2
_cell_length_a                   10.0209(3)
_cell_length_b                   11.1466(4)
_cell_length_c                   11.3056(3)
_cell_measurement_reflns_used    18057
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.54
_cell_measurement_theta_min      1.84
_cell_volume                     1199.95(7)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.131.0 (STOE, 2017)
;
_computing_data_reduction
;
X-Area Integrate 1.71.0.0 (STOE, 2016)
X-Area LANA 1.71.4.0 (STOE, 2017)
;
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  SHELXL2018
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_monochromator  multilayer-optics
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0786
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23397
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.475
_exptl_absorpt_coefficient_mu    6.378
_exptl_absorpt_correction_T_max  0.8666
_exptl_absorpt_correction_T_min  0.4485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_description       block
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5714
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0223P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0592
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4497
_reflns_number_total             5714
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt00728b2.cif
_cod_data_source_block           6
_cod_database_code               7710222
_shelx_shelxl_version_number     2018/3
_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_min   0.832
_shelx_estimated_absorpt_t_max   0.832
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
Au1 Au 0.47065(2) 0.83263(2) 0.96084(2) 0.01295(6) Uani 1 1 d . . . . .
Cl1 Cl 0.55215(14) 0.89403(12) 1.15994(10) 0.0216(3) Uani 1 1 d . . . . .
P1 P 0.39310(13) 0.76277(12) 0.76941(10) 0.0104(3) Uani 1 1 d . . . . .
Si1 Si 0.28795(13) 0.65737(12) 0.50948(10) 0.0112(3) Uani 1 1 d . . . . .
N1 N -0.0506(5) 0.1304(4) -0.1412(4) 0.0264(11) Uani 1 1 d . . . . .
C1 C 0.3568(5) 0.5961(4) 0.7479(4) 0.0123(10) Uani 1 1 d . . . . .
C2 C 0.3723(5) 0.5212(4) 0.8463(4) 0.0148(11) Uani 1 1 d . . . . .
H2 H 0.404423 0.557250 0.926384 0.018 Uiso 1 1 calc R U . . .
C3 C 0.3400(5) 0.3941(4) 0.8249(4) 0.0171(11) Uani 1 1 d . . . . .
H3 H 0.350519 0.342574 0.890780 0.021 Uiso 1 1 calc R U . . .
C4 C 0.2923(5) 0.3409(5) 0.7077(4) 0.0181(11) Uani 1 1 d . . . . .
H4 H 0.269188 0.253402 0.694266 0.022 Uiso 1 1 calc R U . . .
C5 C 0.2785(5) 0.4150(4) 0.6105(4) 0.0150(10) Uani 1 1 d . . . . .
H5 H 0.247534 0.377707 0.530891 0.018 Uiso 1 1 calc R U . . .
C6 C 0.3094(5) 0.5440(4) 0.6280(4) 0.0115(10) Uani 1 1 d . . . . .
C7 C 0.2274(5) 0.7923(4) 0.6911(4) 0.0100(9) Uani 1 1 d . . . . .
C8 C 0.1574(5) 0.8607(4) 0.7483(4) 0.0128(10) Uani 1 1 d . . . . .
H8 H 0.192336 0.888605 0.830694 0.015 Uiso 1 1 calc R U . . .
C9 C 0.0355(5) 0.8886(4) 0.6853(4) 0.0164(11) Uani 1 1 d . . . . .
H9 H -0.013659 0.934670 0.724120 0.020 Uiso 1 1 calc R U . . .
C10 C -0.0126(5) 0.8477(4) 0.5642(4) 0.0166(11) Uani 1 1 d . . . . .
H10 H -0.094174 0.867886 0.519880 0.020 Uiso 1 1 calc R U . . .
C11 C 0.0564(5) 0.7782(4) 0.5074(4) 0.0137(10) Uani 1 1 d . . . . .
H11 H 0.021312 0.751385 0.424825 0.016 Uiso 1 1 calc R U . . .
C12 C 0.1764(5) 0.7470(4) 0.5694(4) 0.0119(10) Uani 1 1 d . . . . .
C13 C 0.5062(5) 0.8214(4) 0.6631(4) 0.0102(9) Uani 1 1 d . . . . .
C14 C 0.6273(5) 0.9165(4) 0.6982(4) 0.0121(10) Uani 1 1 d . . . . .
H14 H 0.659271 0.944390 0.780793 0.015 Uiso 1 1 calc R U . . .
C15 C 0.7007(5) 0.9702(4) 0.6127(4) 0.0129(10) Uani 1 1 d . . . . .
H15 H 0.782873 1.035722 0.636207 0.016 Uiso 1 1 calc R U . . .
C16 C 0.6542(5) 0.9282(4) 0.4922(4) 0.0122(10) Uani 1 1 d . . . . .
H16 H 0.703945 0.966310 0.433346 0.015 Uiso 1 1 calc R U . . .
C17 C 0.5366(5) 0.8317(4) 0.4572(4) 0.0128(10) Uani 1 1 d . . . . .
H17 H 0.507400 0.803144 0.374596 0.015 Uiso 1 1 calc R U . . .
C18 C 0.4606(5) 0.7759(4) 0.5405(4) 0.0117(10) Uani 1 1 d . . . . .
C19 C 0.2198(5) 0.5745(4) 0.3588(4) 0.0139(10) Uani 1 1 d . . . . .
C20 C 0.3084(5) 0.5389(5) 0.2915(4) 0.0183(11) Uani 1 1 d . . . . .
H20 H 0.406915 0.572323 0.314959 0.022 Uiso 1 1 calc R U . . .
C21 C 0.2564(5) 0.4558(5) 0.1912(4) 0.0188(11) Uani 1 1 d . . . . .
H21 H 0.319718 0.433225 0.147754 0.023 Uiso 1 1 calc R U . . .
C22 C 0.1121(5) 0.4051(4) 0.1535(4) 0.0139(10) Uani 1 1 d . . . . .
C23 C 0.0233(5) 0.4447(4) 0.2186(4) 0.0138(10) Uani 1 1 d . . . . .
H23 H -0.075485 0.414995 0.192703 0.017 Uiso 1 1 calc R U . . .
C24 C 0.0758(5) 0.5263(4) 0.3202(4) 0.0153(10) Uani 1 1 d . . . . .
H24 H 0.012648 0.549211 0.363611 0.018 Uiso 1 1 calc R U . . .
C25 C 0.0561(5) 0.3102(4) 0.0516(4) 0.0148(10) Uani 1 1 d . . . . .
C26 C 0.1303(5) 0.2268(5) 0.0274(4) 0.0245(12) Uani 1 1 d . . . . .
H26 H 0.219230 0.228718 0.076588 0.029 Uiso 1 1 calc R U . . .
C27 C 0.0750(6) 0.1412(5) -0.0681(5) 0.0291(13) Uani 1 1 d . . . . .
H27 H 0.129076 0.085725 -0.083522 0.035 Uiso 1 1 calc R U . . .
C28 C -0.1230(6) 0.2084(5) -0.1163(4) 0.0241(13) Uani 1 1 d . . . . .
H28 H -0.214003 0.200429 -0.164198 0.029 Uiso 1 1 calc R U . . .
C29 C -0.0747(5) 0.3011(4) -0.0247(4) 0.0173(11) Uani 1 1 d . . . . .
H29 H -0.129262 0.357586 -0.013721 0.021 Uiso 1 1 calc R U . . .
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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 '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
P1 Au1 Cl1 176.89(5) . . ?
C1 P1 C13 104.2(2) . . ?
C1 P1 C7 101.59(19) . . ?
C13 P1 C7 100.6(2) . . ?
C1 P1 Au1 113.70(15) . . ?
C13 P1 Au1 117.12(15) . . ?
C7 P1 Au1 117.43(15) . . ?
C19 Si1 C6 110.0(2) . . ?
C19 Si1 C18 120.3(2) . . ?
C6 Si1 C18 103.88(19) . . ?
C19 Si1 C12 118.4(2) . . ?
C6 Si1 C12 102.0(2) . . ?
C18 Si1 C12 99.8(2) . . ?
C28 N1 C27 116.1(4) . . ?
C2 C1 C6 121.3(4) . . ?
C2 C1 P1 121.3(3) . . ?
C6 C1 P1 117.3(3) . . ?
C3 C2 C1 118.9(4) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C2 C3 C4 120.7(4) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 120.3(4) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 120.9(4) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C1 117.8(4) . . ?
C5 C6 Si1 126.8(3) . . ?
C1 C6 Si1 115.3(3) . . ?
C8 C7 C12 121.3(4) . . ?
C8 C7 P1 120.8(3) . . ?
C12 C7 P1 117.8(3) . . ?
C7 C8 C9 120.1(4) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C10 C9 C8 118.8(4) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
C11 C10 C9 121.1(4) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C10 C11 C12 121.1(4) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C11 C12 C7 117.5(4) . . ?
C11 C12 Si1 128.1(3) . . ?
C7 C12 Si1 114.3(3) . . ?
C14 C13 C18 120.4(4) . . ?
C14 C13 P1 121.0(3) . . ?
C18 C13 P1 118.3(3) . . ?
C15 C14 C13 119.8(4) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C14 C15 C16 119.8(4) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C17 C16 C15 120.7(4) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C16 C17 C18 120.9(4) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C17 C18 C13 118.2(4) . . ?
C17 C18 Si1 127.5(3) . . ?
C13 C18 Si1 113.9(3) . . ?
C24 C19 C20 117.6(4) . . ?
C24 C19 Si1 119.4(3) . . ?
C20 C19 Si1 121.9(3) . . ?
C21 C20 C19 121.9(4) . . ?
C21 C20 H20 119.1 . . ?
C19 C20 H20 119.1 . . ?
C20 C21 C22 120.8(4) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C21 C22 C23 117.1(4) . . ?
C21 C22 C25 121.2(4) . . ?
C23 C22 C25 121.6(4) . . ?
C24 C23 C22 121.9(4) . . ?
C24 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
C19 C24 C23 120.7(4) . . ?
C19 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C26 C25 C29 116.9(4) . . ?
C26 C25 C22 121.5(4) . . ?
C29 C25 C22 121.7(4) . . ?
C27 C26 C25 119.6(5) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
N1 C27 C26 124.3(5) . . ?
N1 C27 H27 117.9 . . ?
C26 C27 H27 117.9 . . ?
N1 C28 C29 124.2(5) . . ?
N1 C28 H28 117.9 . . ?
C29 C28 H28 117.9 . . ?
C28 C29 C25 118.9(5) . . ?
C28 C29 H29 120.6 . . ?
C25 C29 H29 120.6 . . ?
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
Au1 P1 2.2184(11) . ?
Au1 Cl1 2.2790(11) . ?
P1 C1 1.809(5) . ?
P1 C13 1.827(5) . ?
P1 C7 1.830(4) . ?
Si1 C19 1.854(4) . ?
Si1 C6 1.868(5) . ?
Si1 C18 1.874(5) . ?
Si1 C12 1.879(5) . ?
N1 C28 1.319(7) . ?
N1 C27 1.344(6) . ?
C1 C2 1.404(6) . ?
C1 C6 1.415(6) . ?
C2 C3 1.382(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.393(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.399(6) . ?
C5 H5 0.9500 . ?
C7 C8 1.386(6) . ?
C7 C12 1.415(6) . ?
C8 C9 1.395(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.393(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.383(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.393(6) . ?
C11 H11 0.9500 . ?
C13 C14 1.392(6) . ?
C13 C18 1.419(6) . ?
C14 C15 1.380(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.389(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.378(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.384(6) . ?
C17 H17 0.9500 . ?
C19 C24 1.392(6) . ?
C19 C20 1.397(6) . ?
C20 C21 1.392(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.397(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.403(6) . ?
C22 C25 1.484(6) . ?
C23 C24 1.392(6) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.380(7) . ?
C25 C29 1.402(6) . ?
C26 C27 1.370(6) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.386(6) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
