Development of a versatile synthesis method for trinuclear Co(iii), Rh(iii), and Ir(iii) dithiolene complexes, and their crystal structures and multi-step redox properties
Shibata, Yusuke; Zhu, Baohua; Kume, Shoko; Nishihara, Hiroshi; Dalton Transactions  (2009) 1939–1943; doi:10.1039/b815560g

data_7000710
_publ_section_title
;
 Development of a versatile synthesis method for trinuclear Co(iii),
 Rh(iii), and Ir(iii) dithiolene complexes, and their crystal
 structures and multi-step redox properties
;
_journal_issue                   11
_journal_name_full               'Dalton Transactions'
_journal_page_first              1939
_journal_page_last               1943
_journal_paper_doi               10.1039/b815560g
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_sum            'C42 H59 Rh3 S6'
_chemical_formula_weight         1064.98
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_date             2008-10-02T15:28:30-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.000
_cell_angle_beta                 104.337(6)
_cell_angle_gamma                90.000
_cell_formula_units_Z            2
_cell_length_a                   12.513(17)
_cell_length_b                   14.546(17)
_cell_length_c                   12.896(18)
_cell_measurement_reflns_used    5575
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      27.8764
_cell_measurement_theta_min      3.2386
_cell_volume                     2274(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device
;
Saturn724 (4x4 bin mode)
;
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17079
_diffrn_reflns_theta_full        27.74
_diffrn_reflns_theta_max         27.74
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    1.379
_exptl_absorpt_correction_T_max  0.8744
_exptl_absorpt_correction_T_min  0.6824
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.335
_refine_diff_density_min         -1.914
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         9127
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_gt           0.0965
_refine_ls_shift/su_max          0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1128P)^2^+20.0305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2671
_reflns_number_gt                6345
_reflns_number_total             9127
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b815560g.txt
_cod_data_source_block           me5cprh
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2274.2(51)
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7000710