Reversible cyclometalation at RhIas a motif for metal‒ligand bifunctional bond activation and base-free formic acid dehydrogenation
Jongbloed, L. S.; de Bruin, B.; Reek, J. N. H.; Lutz, M.; van der Vlugt, J. I.; Catal. Sci. Technol. 6 (2016) 1320–; doi:10.1039/C5CY01505G

data_1540530
_publ_section_title
;
 Reversible cyclometalation at RhIas a motif for metal--ligand
 bifunctional bond activation and base-free formic acid dehydrogenation
;
_journal_issue                   5
_journal_name_full               'Catal. Sci. Technol.'
_journal_page_first              1320
_journal_paper_doi               10.1039/C5CY01505G
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C45 H62 N2 O2 P2 Rh2 S2'
_chemical_formula_sum            'C45 H62 N2 O2 P2 Rh2 S2'
_chemical_formula_weight         994.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-09-02 deposited with the CCDC.
2015-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.046(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7487(4)
_cell_length_b                   19.7725(6)
_cell_length_c                   18.4361(5)
_cell_measurement_reflns_used    40473
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.53
_cell_volume                     4527.3(2)
_computing_cell_refinement       Peakref
_computing_data_collection       Apex2
_computing_data_reduction        'Eval15, SADABS-2012/1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick, 2012)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa ApexII'
_diffrn_measurement_method       '\f and \w 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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            60826
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.930
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         10392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+1.0759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0580
_reflns_number_gt                8330
_reflns_number_total             10392
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c5cy01505g2.cif
_cod_data_source_block           l0492a
_cod_depositor_comments          'Adding full bibliography for 1540530.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1540530