Phosphorus or nitrogen – the first phosphatriptycene in coordination polymer chemistry
Gildenast, Hans; Gruszien, Lukas; Friedt, Felix; Englert, Ulli; Dalton Transactions  (2022) –; doi:10.1039/D2DT00728B

data_7710228
_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         'C58 H40 Au2 Cl4 N2 P2 Si2 Zn, 2 (C H Cl3)'
_chemical_formula_sum            'C60 H42 Au2 Cl10 N2 P2 Si2 Zn'
_chemical_formula_weight         1722.88
_chemical_name_common            10a
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-04-13 deposited with the CCDC.	2022-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.717(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.338(5)
_cell_length_b                   11.733(3)
_cell_length_c                   24.598(6)
_cell_measurement_reflns_used    6551
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.26
_cell_volume                     6206(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT-PLUS (Bruker, 2009)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega 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  0.1108
_diffrn_reflns_av_unetI/netI     0.0934
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            93492
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.612
_diffrn_reflns_theta_min         1.441
_exptl_absorpt_coefficient_mu    5.661
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5460
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_description       needle
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_platon_squeeze_details
;
TITL h21_27_a.res in P2(1)/n
CELL   22.3380   11.7330   24.5980     90.00    105.72     90.00
SPGR P21/n
C101 0.196 0.079 0.186 !      22.35 eA-3
C102 0.878 0.431 0.747 !      15.10 eA-3
C103 0.846 0.142 0.771 !      15.07 eA-3
C104 0.830 0.936 0.706 !      15.03 eA-3
C105 0.971 0.596 0.804 !      13.25 eA-3
C106 0.342 0.867 0.303 !      11.60 eA-3
C107 0.026 0.448 0.150 !       9.47 eA-3
C108 0.968 0.277 0.197 !       7.23 eA-3
C109 0.404 0.813 0.263 !       6.59 eA-3
C110 0.148 0.016 0.224 !       5.31 eA-3
C111 0.399 0.966 0.306 !       5.11 eA-3
C112 0.618 0.410 0.760 !       3.38 eA-3
C113 0.250 0.426 0.230 !       3.16 eA-3
Q114 0.415 0.053 0.472 !       3.10 eA-3
C115 0.995 0.401 0.158 !       2.69 eA-3
Q116 0.383 0.230 0.342 !       2.53 eA-3
Q117 0.470 0.043 0.142 !       2.47 eA-3
C118 0.708 0.707 0.741 !       2.41 eA-3
C119 0.397 0.988 0.266 !       2.39 eA-3
C120 0.881 0.187 0.798 !       2.36 eA-3
Q121 0.584 0.329 0.321 !       2.32 eA-3
C122 0.280 0.048 0.284 !       2.23 eA-3
Q123 0.134 0.998 0.188 !       2.21 eA-3
C124 0.192 0.537 0.195 !       2.20 eA-3
Q125 0.242 0.252 0.199 !       2.17 eA-3
C126 0.322 0.466 0.256 !       2.09 eA-3
C127 0.860 0.582 0.780 !       2.07 eA-3
Q128 0.531 0.312 0.199 !       2.04 eA-3
C129 0.343 0.455 0.281 !       2.03 eA-3
Q130 0.405 0.828 0.469 !       2.02 eA-3
C131 0.193 0.013 0.222 !       2.02 eA-3
Q132 0.704 0.051 0.908 !       2.01 eA-3
C133 0.338 0.091 0.235 !       2.00 eA-3
C134 0.777 0.369 0.795 !       1.99 eA-3
C135 0.173 0.655 0.202 !       1.99 eA-3
C136 0.727 0.033 0.710 !       1.98 eA-3
C137 0.097 0.648 0.248 !       1.96 eA-3
Q138 0.374 0.906 0.413 !       1.94 eA-3
Q139 0.039 0.404 0.048 !       1.92 eA-3
Q140 0.182 0.088 0.336 !       1.90 eA-3
Q141 0.353 0.437 0.008 !       1.89 eA-3
C142 0.831 0.107 0.813 !       1.87 eA-3
C143 0.155 0.384 0.243 !       1.87 eA-3
C144 0.360 0.138 0.303 !       1.87 eA-3
Q145 0.886 0.235 0.657 !       1.86 eA-3
Q146 0.166 0.156 0.295 !       1.84 eA-3
Q147 0.100 0.425 0.008 !       1.83 eA-3
Q148 0.195 0.774 0.196 !       1.80 eA-3
C149 0.142 0.095 0.227 !       1.80 eA-3
Q150 0.905 0.328 0.209 !       1.79 eA-3
Q151 0.461 0.788 0.219 !       1.78 eA-3
Q152 0.919 0.704 0.710 !       1.78 eA-3
C153 0.312 0.471 0.290 !       1.78 eA-3
Q154 0.266 0.359 0.344 !       1.78 eA-3
C155 0.768 0.016 0.705 !       1.77 eA-3
C156 0.233 0.103 0.256 !       1.77 eA-3
C157 0.754 0.325 0.769 !       1.76 eA-3
C158 0.126 0.440 0.169 !       1.76 eA-3
Q159 0.367 0.990 0.414 !       1.75 eA-3
Q160 0.420 0.613 0.243 !       1.75 eA-3
Q161 0.440 0.018 0.111 !       1.74 eA-3
Q162 0.436 0.891 0.180 !       1.74 eA-3
Q163 0.130 0.082 0.193 !       1.74 eA-3
Q164 0.046 0.107 0.382 !       1.73 eA-3
Q165 0.753 0.324 0.195 !       1.72 eA-3
Q166 0.471 0.830 0.143 !       1.71 eA-3
Q167 0.444 0.157 0.334 !       1.71 eA-3
Q168 0.374 0.699 0.328 !       1.70 eA-3
C169 0.093 0.797 0.233 !       1.70 eA-3
Q170 0.751 0.524 0.475 !       1.69 eA-3
Q171 0.428 0.011 0.358 !       1.69 eA-3
Q172 0.260 0.435 0.161 !       1.69 eA-3
C173 0.103 0.031 0.244 !       1.68 eA-3
C174 0.528 0.700 0.303 !       1.67 eA-3
C175 0.404 0.249 0.241 !       1.66 eA-3
C176 0.069 0.266 0.197 !       1.66 eA-3
C177 0.241 0.046 0.245 !       1.66 eA-3
Q178 0.470 0.129 0.147 !       1.66 eA-3
Q179 0.421 0.672 0.322 !       1.66 eA-3
Q180 0.452 0.739 0.092 !       1.65 eA-3
Q181 0.822 0.314 0.470 !       1.65 eA-3
Q182 0.431 0.231 0.187 !       1.65 eA-3
Q183 0.735 0.538 0.875 !       1.64 eA-3
Q184 0.475 0.936 0.118 !       1.64 eA-3
C185 0.876 0.322 0.754 !       1.64 eA-3
C186 0.124 0.678 0.246 !       1.64 eA-3
Q187 0.415 0.361 0.462 !       1.63 eA-3
Q188 0.797 0.206 0.251 !       1.63 eA-3
Q189 0.029 0.389 0.829 !       1.63 eA-3
Q190 0.374 0.891 0.191 !       1.63 eA-3
C191 0.750 0.454 0.800 !       1.62 eA-3
C192 0.205 0.028 0.258 !       1.62 eA-3
Q193 0.720 0.633 0.233 !       1.60 eA-3
C194 0.708 0.492 0.785 !       1.60 eA-3
C195 0.157 0.790 0.261 !       1.60 eA-3
Q196 0.396 0.156 0.438 !       1.58 eA-3
C197 0.366 0.255 0.271 !       1.58 eA-3
C198 0.145 0.516 0.283 !       1.58 eA-3
C199 0.352 0.076 0.274 !       1.58 eA-3
;
_refine_diff_density_max         2.129
_refine_diff_density_min         -1.868
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         18432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+18.5652P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1403
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11936
_reflns_number_total             18432
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00728b2.cif
_cod_data_source_block           10a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7710228
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.413
_shelx_estimated_absorpt_t_max   0.849
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              96418
_shelx_fab_checksum              86540