Synthesis and Reactivity of a Transient, Terminal Nitrido Complex of Rhodium
Markus G. Scheibel; Yanlin Wu; A. Claudia Stückl; Lennard Krause; Elena Carl; Dietmar Stalke; Bas de Bruin; Sven Schneider; Journal of the American Chemical Society 135 (2013) 17719–17722; doi:10.1021/ja409764j

data_4121222
_publ_section_title
;
 Synthesis and Reactivity of a Transient, Terminal Nitrido Complex of
 Rhodium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17719
_journal_page_last               17722
_journal_paper_doi               10.1021/ja409764j
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C20 H40 N3 P2 Rh1'
_chemical_formula_sum            'C20 H40 N3 P2 Rh'
_chemical_formula_weight         487.4
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 106.53(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.867(2)
_cell_length_b                   27.050(6)
_cell_length_c                   11.866(2)
_cell_measurement_reflns_used    4429
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.7865
_cell_measurement_theta_min      2.2125
_cell_volume                     2420.8(9)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2011.2'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'shelXle v0.477'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Smart APEX II Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56085
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22081
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         20.943
_diffrn_reflns_theta_min         1.188
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.450
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_correction_T_min  0.5950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       neelde
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.041
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         5218
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0454P)^2^+1.6943P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4288
_reflns_number_total             5218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja409764j_si_003.cif
_cod_data_source_block           P21c_a
_cod_original_formula_sum        'C20 H40 N3 P2 Rh1'
_cod_database_code               4121222
_shelxl_version_number           2012-6
_shelx_res_checksum              40543