Triazaphospholes versus Triazoles: An Investigation of the Differences between “Click”-Derived Chelating Phosphorus- and Nitrogen-Containing Heterocycles
Sklorz, Julian A. W.; Hoof, Santina; Sommer, Michael G.; Weißer, Fritz; Weber, Manuela; Wiecko, Jelena; Sarkar, Biprajit; Müller, Christian; Organometallics 33 (2014) 511–; doi:10.1021/om4010077

data_4082324
_publ_contact_author
;
      Prof. Dr.Christian M\"uller
      Freie Universit\"at Berlin
      Institut f\"ur Chemie und Biochemie
      Anorganische Chemie      
      Fabeckstr. 34-36
      14195 Berlin
      Germany
;
_publ_section_title
;
 Triazaphospholes versus Triazoles: An Investigation of the Differences
 between &#x201C;Click&#x201D;-Derived Chelating Phosphorus- and
 Nitrogen-Containing Heterocycles
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              511
_journal_paper_doi               10.1021/om4010077
_journal_volume                  33
_journal_year                    2014
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C14 H16 Br N4 O3 Re Si'
_chemical_formula_sum            'C14 H16 Br N4 O3 Re Si'
_chemical_formula_weight         582.51
_chemical_name_systematic
;
 SH63
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1775(16)
_cell_length_b                   12.6712(18)
_cell_length_c                   10.9575(13)
_cell_measurement_reflns_used    4518
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.58
_cell_measurement_theta_min      3.29
_cell_volume                     1968.5(4)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_publication_material  'X-STEP32, Microsoft Word'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_unetI/netI     0.1519
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7508
_diffrn_reflns_point_group_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.286
_diffrn_reflns_theta_min         3.293
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    8.282
_exptl_absorpt_correction_T_max  0.8283
_exptl_absorpt_correction_T_min  0.4504
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.966
_exptl_crystal_description       needle
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.369
_refine_diff_density_min         -2.042
_refine_diff_density_rms         0.206
_refine_ls_abs_structure_details
;
 Flack x determined using 872 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.884
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         4925
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.884
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0531P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1264
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_full    0.887
_reflns_Friedel_fraction_max     0.848
_reflns_number_gt                2720
_reflns_number_total             4925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om4010077_si_002.cif
_cod_data_source_block           8
_cod_database_code               4082324