Rhodium Assisted C−H Activation of Benzaldehyde Thiosemicarbazones and Their Oxidation via Activation of Molecular Oxygen
Acharyya, Rama; Dutta, Swati; Basuli, Falguni; Peng, Shie-Ming; Lee, Gene-Hsiang; Falvello, Larry R.; Bhattacharya, Samaresh; Inorganic Chemistry 45 (2006) 1252–1259; doi:10.1021/ic050505w

data_4331526
_publ_section_title
;
 Rhodium Assisted C&#x2212;H Activation of Benzaldehyde Thiosemicarbazones
 and Their Oxidation via Activation of Molecular Oxygen
;
_journal_issue                   3
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1252
_journal_page_last               1259
_journal_paper_doi               10.1021/ic050505w
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C45 H38.5 N4.5 O2 P2 Rh S'
_chemical_formula_weight         871.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.918(11)
_cell_angle_beta                 101.705(9)
_cell_angle_gamma                101.074(18)
_cell_formula_units_Z            4
_cell_length_a                   13.611(2)
_cell_length_b                   16.166(3)
_cell_length_c                   19.4501(18)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      16.0
_cell_measurement_theta_min      13.7
_cell_volume                     4077.9(11)
_computing_cell_refinement       'CAD4/PC V2.0 (Nonius, 1996)'
_computing_data_collection       'CAD4/PC V2.0 (Nonius, 1996)'
_computing_data_reduction        'XCAD4 (Harms, 1996)'
_computing_molecular_graphics    'SHELXTL Rel. 5.05/V (Siemens, 1996)'
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
 SIR92 - A program for crystal structure solution. 
 Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, 
 A. (1993) J. Appl. Cryst. 26, 343-350.
;
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Nonius CAD-4'
_diffrn_measurement_method       'omega-theta scan'
_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  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0928
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14451
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.01
_diffrn_standards_interval_time  30
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  0.816
_exptl_absorpt_correction_T_min  0.754
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1007
_refine_ls_number_reflns         14386
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+5.9974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1319
_reflns_number_gt                9932
_reflns_number_total             14386
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050505wsup1.cif
_cod_data_source_block           estr374
_cod_depositor_comments
;
 Changing the _atom_site_type_symbol data item value for hydride ion atoms
 from 'Hh' to 'H-'.

 Antanas Vaitkus,
 2017-02-17

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+5.9974P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+5.9974P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4078.1(12)
_cod_original_formula_sum        'C45 H38.50 N4.50 O2 P2 Rh S'
_cod_database_code               4331526