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_4121223
_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         'C38 H60 N P3 Rh, Cl'
_chemical_formula_sum            'C38 H60 Cl N P3 Rh'
_chemical_formula_weight         762.14
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                77.982(10)
_cell_angle_beta                 81.91(2)
_cell_angle_gamma                75.721(10)
_cell_formula_units_Z            2
_cell_length_a                   10.1464(10)
_cell_length_b                   10.4691(10)
_cell_length_c                   19.064(2)
_cell_measurement_reflns_used    9852
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.41
_cell_measurement_theta_min      2.3045
_cell_volume                     1910.9(4)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_unetI/netI     0.0770
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7656
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         20.582
_diffrn_reflns_theta_min         0.866
_diffrn_source                   'INCOATEC Ag Microsource'
_exptl_absorpt_coefficient_mu    0.355
_exptl_absorpt_correction_T_max  0.744711
_exptl_absorpt_correction_T_min  0.562901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS-2008/2
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       block
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         7656
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0295P)^2^+2.3544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6164
_reflns_number_total             7656
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja409764j_si_004.cif
_cod_data_source_block           twin5
_cod_original_cell_volume        1911.0(4)
_cod_database_code               4121223
_shelxl_version_number           2013-4
_shelx_res_checksum              96672