Springloaded porphyrin NHC hybrid rhodium(III) complexes: carbene dissociation and oxidation catalysis.
Olguín, Juan; Müller-Bunz, Helge; Albrecht, Martin; Chemical communications (Cambridge, England) 50 (2014) 3488–3490; doi:10.1039/c4cc00497c

data_7124559
_publ_section_title
;
 Springloaded porphyrin NHC hybrid rhodium(III) complexes: carbene
 dissociation and oxidation catalysis.
;
_journal_issue                   26
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3488
_journal_page_last               3490
_journal_paper_doi               10.1039/c4cc00497c
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C54 H44 N8 Rh, Cl, 1.25 (C H Cl3)'
_chemical_formula_sum            'C55.25 H45.25 Cl4.75 N8 Rh'
_chemical_formula_weight         1092.54
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.679(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1167(2)
_cell_length_b                   19.9147(2)
_cell_length_c                   17.2364(2)
_cell_measurement_reflns_used    23392
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2470
_cell_measurement_theta_min      3.1180
_cell_volume                     5188.56(11)
_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 0.989
_diffrn_measured_fraction_theta_max 0.885
_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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            53398
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.53
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    0.619
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.934
_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            red
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2234
_exptl_crystal_size_max          0.2299
_exptl_crystal_size_mid          0.1583
_exptl_crystal_size_min          0.1183
_platon_squeeze_details
; 
 PLATON: A.L. Spek, J. Appl. Cryst. 36 (2003), 7-13 
 PLATON version from 27.07.2012 
;
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         12825
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0515P)^2^+4.6832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1086
_reflns_number_gt                10892
_reflns_number_total             12825
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c4cc00497c2.cif
_cod_data_source_block           alb209(3)
_cod_depositor_comments
;

2025-03-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C221 H181 Cl19 N32 Rh4'
_cod_original_formula_weight         4370.17
_cod_original_formula_moiety         '4 (C54 H44 N8 Rh), 4 Cl, 5 (C H Cl3)'
_cod_original_formula_units_Z            1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7124559