Ruthenium and osmium complexes of novel carbohydrate derived salen ligands: Synthesis, characterization and in situ ligand reduction
Soumik Mandal; Santanu Mandal; Dipravath K. Seth; Balaram Mukhopadhyay; Parna Gupta; Inorganica Chimica Acta 398 (2013) 83–88; doi:10.1016/j.ica.2012.12.016

data_1513207
_publ_section_title
;
 Ruthenium and osmium complexes of novel carbohydrate derived salen
 ligands: Synthesis, characterization and in situ ligand reduction
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              83
_journal_page_last               88
_journal_paper_doi               10.1016/j.ica.2012.12.016
_journal_volume                  398
_journal_year                    2013
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C41 H39 N2 O6 Os P, C6 H6'
_chemical_formula_sum            'C47 H45 N2 O6 Os P'
_chemical_formula_weight         955.05
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.595(6)
_cell_length_b                   16.977(7)
_cell_length_c                   19.141(8)
_cell_measurement_reflns_used    5283
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.01
_cell_measurement_theta_min      2.40
_cell_volume                     4418(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0862
_diffrn_reflns_av_sigmaI/netI    0.0892
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33602
_diffrn_reflns_theta_full        25.77
_diffrn_reflns_theta_max         25.77
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    2.969
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Bruker 2008'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.898
_refine_diff_density_min         -1.180
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.008(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         8259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0456P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                6071
_reflns_number_total             8259
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-398-83-88-2.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               1513207