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_7710225
_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
'C118 H80 F6 N4 O6 P4 S2 Si4 Zn, 3(C6 H5 Cl), 0.75(C5 H12)'
_chemical_formula_sum            'C139.75 H104 Cl3 F6 N4 O6 P4 S2 Si4 Zn'
_chemical_formula_weight         2521.34
_chemical_name_common            9
_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
;
2022-04-13 deposited with the CCDC.	2022-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                100.034(3)
_cell_angle_beta                 99.951(4)
_cell_angle_gamma                103.892(10)
_cell_formula_units_Z            2
_cell_length_a                   17.981(18)
_cell_length_b                   18.767(16)
_cell_length_c                   19.161(16)
_cell_measurement_reflns_used    598
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.000
_cell_measurement_theta_min      0.878
_cell_volume                     6023(9)
_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 0.968
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type
;
kappa goniometer at EH1 P24, DESY
;
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.56356
_diffrn_reflns_av_R_equivalents  0.0784
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            101570
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        19.763
_diffrn_reflns_theta_max         21.000
_diffrn_reflns_theta_min         0.878
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  0.8624
_exptl_absorpt_correction_T_min  0.7117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       block
_exptl_crystal_F_000             2603
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_platon_squeeze_details
;
TITL lg41 prop_aug20 p24
CELL   17.9810   18.7670   19.1610    100.03     99.95    103.89
SPGR P-1
C101 0.093 0.226 0.108 !       5.74 eA-3
Q102 0.869 0.968 0.020 !       2.79 eA-3
C103 0.106 0.069 0.049 !       2.75 eA-3
C104 0.037 0.183 0.041 !       2.72 eA-3
C105 0.085 0.140 0.027 !       2.38 eA-3
Q106 0.403 0.410 0.380 !       2.25 eA-3
Q107 0.941 0.869 0.010 !       1.97 eA-3
Q108 0.062 0.861 0.470 !       1.53 eA-3
Q109 0.919 0.983 0.064 !       1.36 eA-3
Q110 0.805 0.794 0.189 !       1.34 eA-3
Q111 0.052 0.935 0.453 !       1.21 eA-3
Q112 0.850 0.735 0.340 !       1.15 eA-3
Q113 0.876 0.862 0.190 !       1.15 eA-3
Q114 0.019 0.782 0.423 !       1.14 eA-3
C115 0.064 0.979 0.015 !       1.06 eA-3
Q116 0.951 0.765 0.393 !       1.02 eA-3
C117 0.054 0.028 0.031 !       0.98 eA-3
Q118 0.984 0.931 0.418 !       0.97 eA-3
Q119 0.439 0.454 0.443 !       0.91 eA-3
Q120 0.373 0.268 0.339 !       0.89 eA-3
Q121 0.876 0.864 0.136 !       0.85 eA-3
Q122 0.913 0.914 0.039 !       0.82 eA-3
C123 1.000 1.000 0.000 !       0.81 eA-3
Q124 0.889 0.795 0.397 !       0.78 eA-3
Q125 1.002 0.894 0.470 !       0.78 eA-3
Q126 0.720 1.001 0.180 !       0.76 eA-3
Q127 0.963 0.934 0.084 !       0.73 eA-3
Q128 0.926 0.873 0.432 !       0.70 eA-3
Q129 0.141 0.655 0.372 !       0.67 eA-3
Q130 0.931 0.877 0.388 !       0.63 eA-3
Q131 0.733 0.342 0.450 !       0.61 eA-3
Q132 0.811 0.722 0.398 !       0.60 eA-3
Q133 0.554 0.184 0.019 !       0.58 eA-3
Q134 0.576 0.615 0.129 !       0.58 eA-3
Q135 0.468 0.907 0.292 !       0.55 eA-3
C136 0.977 0.128 0.012 !       0.53 eA-3
Q137 0.894 0.893 0.056 !       0.52 eA-3
Q138 0.830 0.377 0.419 !       0.52 eA-3
;
_refine_diff_density_max         2.225
_refine_diff_density_min         -1.819
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1415
_refine_ls_number_reflns         24165
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0661
_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/[\s^2^(Fo^2^)+(0.1121P)^2^+10.2501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1918
_refine_ls_wR_factor_ref         0.2021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20272
_reflns_number_total             24165
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00728b2.cif
_cod_data_source_block           9
_cod_database_code               7710225
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.975
_shelx_estimated_absorpt_t_max   0.980
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              23574
_shelx_fab_checksum              61580