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_7710215
_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'
_chemical_formula_sum            'C29 H20 N P Si'
_chemical_formula_weight         441.52
_chemical_name_common            4b
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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
_cell_angle_beta                 96.2607(17)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.2413(3)
_cell_length_b                   10.28157(16)
_cell_length_c                   26.8395(6)
_cell_measurement_reflns_used    30222
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.03
_cell_measurement_theta_min      4.06
_cell_volume                     4455.09(15)
_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 0.973
_diffrn_measured_fraction_theta_max 0.958
_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  0.0589
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            46159
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.508
_diffrn_reflns_theta_min         4.062
_exptl_absorpt_coefficient_mu    1.732
_exptl_absorpt_correction_T_max  0.9736
_exptl_absorpt_correction_T_min  0.4028
_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(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       plate
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         8181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0388P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0788
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5459
_reflns_number_total             8181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00728b2.cif
_cod_data_source_block           4b
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7710215
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.846
_shelx_estimated_absorpt_t_max   0.983
_shelx_res_checksum              35582