Synthesis and Crystal Structure of the Rhenium(I) Tricarbonyl Complex of 5,10,15,20-Tetra-p-tolyl-21,23-dithiaporphyrin.
Kaur, Tejinder; Ghosh, Avijit; Rajakannu, Palanisamy; Ravikanth, Mangalampalli; Inorganic chemistry 53 (2014) 2355–2357; doi:10.1021/ic4029832

data_4337745
_publ_section_title
;
 Synthesis and Crystal Structure of the Rhenium(I) Tricarbonyl Complex of
 5,10,15,20-Tetra-p-tolyl-21,23-dithiaporphyrin.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2355
_journal_page_last               2357
_journal_paper_doi               10.1021/ic4029832
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C57 H36 Cl3 N2 O9 Re3 S2'
_chemical_formula_weight         1621.95
_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                61.31(2)
_cell_angle_beta                 64.00(2)
_cell_angle_gamma                80.77(3)
_cell_formula_units_Z            2
_cell_length_a                   14.755(5)
_cell_length_b                   14.820(4)
_cell_length_c                   15.716(3)
_cell_measurement_reflns_used    8338
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.8
_cell_measurement_theta_min      2.3
_cell_volume                     2704.1(15)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku Saturn724+'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0643
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_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19684
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    6.982
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.451
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.992
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.778
_refine_diff_density_min         -6.367
_refine_diff_density_rms         0.347
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         9410
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0885
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1090P)^2^+119.9543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2355
_refine_ls_wR_factor_ref         0.2392
_reflns_number_gt                8801
_reflns_number_total             9410
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4029832_si_002.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2704.1(13)
_cod_database_code               4337745