Springloaded porphyrin NHC hybrid rhodium(III) complexes: carbene dissociation and oxidation catalysis
Juan Olguin; Helge Muller-Bunz; Martin Albrecht; Chem.Commun. 50 (2014) 3488–; doi:10.1039/C4CC00497C3

data_7112121
_publ_section_title
;
 Springloaded porphyrin NHC hybrid rhodium(III) complexes: carbene
 dissociation and oxidation catalysis
;
_journal_name_full               Chem.Commun.
_journal_page_first              3488
_journal_paper_doi               10.1039/C4CC00497C3
_journal_volume                  50
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C48 H34 Cl N6 Rh, 0.75 (C H2 Cl2)'
_chemical_formula_sum            'C48.75 H35.5 Cl2.5 N6 Rh'
_chemical_formula_weight         896.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6618(1)
_cell_length_b                   17.3989(2)
_cell_length_c                   25.1987(3)
_cell_measurement_reflns_used    26269
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.3820
_cell_measurement_theta_min      3.4160
_cell_volume                     4236.02(8)
_computing_cell_refinement
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET) 
(compiled Dec 19 2012,11:08:27) 
;
_computing_data_collection
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET) 
(compiled Dec 19 2012,11:08:27) 
;
_computing_data_reduction
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET) 
(compiled Dec 19 2012,11:08:27) 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3196
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            43286
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         29.53
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET) 
(compiled Dec 19 2012,11:08:27) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1830
_exptl_crystal_size_max          0.1818
_exptl_crystal_size_mid          0.1708
_exptl_crystal_size_min          0.1033
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.056(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         10592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0312P)^2^+5.3806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0829
_reflns_number_gt                10035
_reflns_number_total             10592
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c4cc00497c3.cif
_cod_data_source_block           alb203(1)
_cod_original_formula_sum        'C48.75 H35.50 Cl2.50 N6 Rh'
_cod_database_code               7112121