Synthesis and characterization of tricarbonyl-molybdenum complexes bearing monoaza-trithia-macrocyclic ligands
Takahiko Ogawa; Koji Koike; Jun Matsumoto; Yuji Kajita; Hideki Masuda; Inorganica Chimica Acta 401 (2013) 101–106; doi:

data_1516984
_publ_section_title
;
 Synthesis and characterization of tricarbonyl-molybdenum complexes
 bearing monoaza-trithia-macrocyclic ligands
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              101
_journal_page_last               106
_journal_volume                  401
_journal_year                    2013
_chemical_formula_moiety         'C13 H21 Mo N O3 S3'
_chemical_formula_sum            'C13 H21 Mo N O3 S3'
_chemical_formula_weight         431.43
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   29.541(4)
_cell_length_b                   8.9741(11)
_cell_length_c                   12.7826(16)
_cell_measurement_reflns_used    9516
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.07
_cell_volume                     3388.7(8)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25693
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.150
_exptl_absorpt_correction_T_max  0.795
_exptl_absorpt_correction_T_min  0.724
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            paleyellow
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1760.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.720
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  3620 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     396
_refine_ls_number_reflns         7676
_refine_ls_number_restraints     3
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0229P)^2^+2.7892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0665
_reflns_number_gt                7239
_reflns_number_total             7676
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ICA-2013-401-101-106-2.cif
_cod_data_source_block           2H
_cod_original_cell_volume        3388.8(8)
_cod_database_code               1516984