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_4082323
_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         'C15 H16 Br1 N4 O3 Re1'
_chemical_formula_sum            'C15 H16 Br N4 O3 Re'
_chemical_formula_weight         566.43
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.260(7)
_cell_angle_beta                 76.666(7)
_cell_angle_gamma                86.164(7)
_cell_formula_units_Z            2
_cell_length_a                   7.6834(7)
_cell_length_b                   10.3540(9)
_cell_length_c                   13.0783(11)
_cell_measurement_reflns_used    15220
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.60
_cell_measurement_theta_min      3.25
_cell_volume                     994.34(15)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Ortep(Johnson, 1996)'
_computing_publication_material  'X-STEP32, Microsoft Word'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11855
_diffrn_reflns_theta_full        29.21
_diffrn_reflns_theta_max         29.21
_diffrn_reflns_theta_min         3.25
_diffrn_standards_number         15220
_exptl_absorpt_coefficient_mu    8.138
_exptl_absorpt_correction_T_max  0.6704
_exptl_absorpt_correction_T_min  0.1553
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   numerical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plateless
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.247
_exptl_crystal_size_min          0.050
_platon_squeeze_details
;
The general procedure (based on a preliminary implementation of the technique)
has been described in more detail in: Acta Cryst. (1990), A46, 194 as the 
'BYPASS procedure' P. v.d. Sluis & A.L. Spek) 
;
_refine_diff_density_max         1.314
_refine_diff_density_min         -1.284
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       0.0099(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         5328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0764
_reflns_number_gt                4512
_reflns_number_total             5328
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om4010077_si_002.cif
_cod_data_source_block           7
_cod_original_sg_symbol_Hall     -p_1
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C15 H16 Br1 N4 O3 Re1'
_cod_database_code               4082323