Synthesis, Characterization, and Transition-Metal Complexes of 3,4-Diazaphospholanes
Landis, Clark R.; Nelson, Ryan C.; Jin, Wiechang; Bowman, Amanda C.; Organometallics 25 (2006) 1377–1391; doi:10.1021/om050922g

data_4074827
_publ_section_title
;
 Synthesis, Characterization, and Transition-Metal Complexes of
 3,4-Diazaphospholanes
;
_journal_coden_ASTM              ORGND7
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1377
_journal_page_last               1391
_journal_paper_doi               10.1021/om050922g
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C36 H31 Cl3 F0 N2 O2 P Rh'
_chemical_formula_weight         763.86
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.573(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.860(3)
_cell_length_b                   9.3627(12)
_cell_length_c                   16.269(2)
_cell_measurement_temperature    153(2)
_cell_volume                     3283.4(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0724
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22311
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    0.849
_exptl_absorpt_correction_T_max  0.8157
_exptl_absorpt_correction_T_min  0.7497
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.071
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         8140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1072
_reflns_number_gt                5699
_reflns_number_total             8140
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050922gsi20051024_021932.cif
_cod_data_source_block           n00033
_cod_original_cell_volume        3283.3(7)
_cod_database_code               4074827