A New Access to Diazaphospholes via Cycloaddition-Cycloreversion Reactions on Triazaphospholes
Dettling, Lea; Papke, Martin; Sklorz, Julian; Buzsaki, Daniel; Kelemen, Zsolt; Weber, Manuela; Nyulaszi, Laszlo; Muller, Christian; Chemical Communications  (2022) –; doi:10.1039/D2CC02269A

data_7130232
_publ_section_title
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 A New Access to Diazaphospholes via Cycloaddition-Cycloreversion
 Reactions on Triazaphospholes
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02269A
_journal_year                    2022
_chemical_formula_moiety         'C15 H5 F6 N2 O5 P W'
_chemical_formula_sum            'C15 H5 F6 N2 O5 P W'
_chemical_formula_weight         622.03
_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_date             2019-02-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-30 deposited with the CCDC.	2022-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.123(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.6629(3)
_cell_length_b                   18.3901(8)
_cell_length_c                   15.6561(7)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.58
_cell_volume                     1888.50(15)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       APEX2
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.97
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30420
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.557
_diffrn_reflns_theta_min         2.579
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.290
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1166 before and 0.0487 after correction.
The Ratio of minimum to maximum transmission is 0.6495.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.188
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.4846
_refine_diff_density_max         0.569
_refine_diff_density_min         -1.704
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5650
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0192
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0127P)^2^+2.2436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0413
_refine_ls_wR_factor_ref         0.0422
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5238
_reflns_number_total             5650
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02269a2.cif
_cod_data_source_block           pap228_5
_cod_database_code               7130232
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.314
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C3(H3), C2(H2)
;
_shelx_res_checksum              53376
_olex2_submission_special_instructions 'No special instructions were received'