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_7710220
_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 N P Si, 0.5(C4 H8 O2)'
_chemical_formula_sum            'C31 H24 N O P Si'
_chemical_formula_weight         485.57
_chemical_name_common            4ea
_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                 90.065(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9479(3)
_cell_length_b                   21.8833(8)
_cell_length_c                   14.4641(5)
_cell_measurement_reflns_used    30123
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.48
_cell_measurement_theta_min      4.04
_cell_volume                     2515.69(16)
_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 0.963
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_monochromator  multilayer-optics
_diffrn_radiation_source         microsource
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            23998
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         69.994
_diffrn_reflns_theta_min         5.069
_exptl_absorpt_coefficient_mu    1.611
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4077
_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(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       plate
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
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_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0866P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3649
_reflns_number_total             4530
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00728b2.cif
_cod_data_source_block           4ea
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7710220
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.739
_shelx_estimated_absorpt_t_max   0.953
_shelx_res_checksum              90844