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_4121221
_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 Cl N P2 Rh'
_chemical_formula_sum            'C20 H40 Cl N P2 Rh'
_chemical_formula_weight         494.83
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 113.31(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.452(2)
_cell_length_b                   8.527(2)
_cell_length_c                   13.432(3)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.508
_cell_measurement_theta_min      2.389
_cell_volume                     1204.6(5)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2012.2'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'Mercury Version 2.4'
_computing_publication_material  'Mercury Version 2.4'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart Apex II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_source         'INCOATEC Mo Microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33444
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.520
_diffrn_reflns_theta_min         1.936
_exptl_absorpt_coefficient_mu    0.957
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_correction_T_min  0.3999
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       plate
_exptl_crystal_F_000             518
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         3683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0183
_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^)+(0.0246P)^2^+0.3583P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0472
_refine_ls_wR_factor_ref         0.0481
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3427
_reflns_number_total             3683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja409764j_si_002.cif
_cod_data_source_block           p2c_a
_cod_database_code               4121221
_shelxl_version_number           2012-9
_shelx_res_checksum              26335