Synthesis and molecular structure of Cr(salen)(μ-N)RhCl(COD): the first example of a heterobimetallic nitride-bridged complex containing chromium
Vibenholt, Johan; Magnussen, Magnus; Anthon, Christian; Bendix, Jesper; Acta Crystallographica Section C 66 (2010) m177–m179; doi:10.1107/S0108270110018238

data_2017695
_publ_section_title
;
 Synthesis and molecular structure of Cr(salen)(\m-N)RhCl(COD): the
 first example of a heterobimetallic nitride-bridged complex containing
 chromium
;
_journal_coeditor_code           EG3042
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m177
_journal_page_last               m179
_journal_paper_doi               10.1107/S0108270110018238
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Cr Rh (C16 H14 N2 O2) Cl N (C8 H12)]'
_chemical_formula_moiety         'C24 H26 Cl Cr N3 O2 Rh'
_chemical_formula_sum            'C24 H26 Cl Cr N3 O2 Rh'
_chemical_formula_weight         578.84
_chemical_name_common
;
 (salen)chromium(V)-(\m-nitrido)-chloro(COD)rhodium(I)
;
_chemical_name_systematic
;chlorido-2\k<i>Cl</i>-[2(\h^4^)-1,5-cyclooctadiene]{2,2'-[ethane-1,2-
diylbis(nitrilomethylidyne)]diphenolato-
1\k^4^<i>O</i>,<i>N</i>,<i>N</i>',<i>O</i>'}-\m-nitrido-
1:2\k^2^<i>N</i>:<i>N</i>-chromium(V)rhodium(I)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 107.259(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6140(13)
_cell_length_b                   15.1085(14)
_cell_length_c                   12.6704(17)
_cell_measurement_reflns_used    34038
_cell_measurement_temperature    122.0(10)
_cell_measurement_theta_max      33.99
_cell_measurement_theta_min      1.69
_cell_volume                     2306.0(5)
_computing_cell_refinement       'COLLECT (Nonius, 1999)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'EvalCCD (Duisenberg <i>et al.</i>,  2003)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      122.0(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\w and \f scans'
_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  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            77914
_diffrn_reflns_theta_full        33.99
_diffrn_reflns_theta_max         33.99
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    1.330
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.718
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(Gaussian integration; Coppens, 1970)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.980
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         9382
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0224P)^2^+2.4740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0667
_reflns_number_gt                7611
_reflns_number_total             9382
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            eg3042.cif
_cod_data_source_block           I
_cod_original_cell_volume        2306.0(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2017695
_cod_database_fobs_code          2017695