The Lowest-Energy Ligand to Metal Charge-Transfer Absorption Band of trans-[OsO2(Malonate)2]2-
Sandrine Stanislas; André L. Beauchamp; Christian Reber; Inorganic Chemistry 39 (2000) 2152–2155; doi:10.1021/ic9912777

data_4320942
_publ_section_title
;
 The Lowest-Energy Ligand to Metal Charge-Transfer Absorption Band of
 trans-[OsO2(Malonate)2]2-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2152
_journal_page_last               2155
_journal_paper_doi               10.1021/ic9912777
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source        'synthesized by the authors, see text'
_chemical_formula_moiety         'C38 H76 N2 O10 Os'
_chemical_formula_structural     '(N(C4 H9)4 )2 (OsO2(C3H2O4)2)'
_chemical_formula_sum            'C38 H76 N2 O10 Os'
_chemical_formula_weight         911.20
_chemical_name_systematic
; 
Tetrabutylammonium Bis(malonato)dioxo-osmate(VI) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-96 (Sheldrick, 1996)'
_cell_angle_alpha                90.00
_cell_angle_beta                 102.41(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.667(3)
_cell_length_b                   18.264(8)
_cell_length_c                   13.163(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      20.00
_cell_volume                     2269.7(16)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction        'NRC-2, NRC-2A (Ahmed et al, 1973)'
_computing_molecular_graphics
'ORTEPII (Johnson (1976) in NRCVAX (Gabe et al (1989))'
_computing_publication_material
'NRCVAX (Gabe et al (1989) and SHELXL96 (Sheldrick (1996))'
_computing_structure_refinement
'NRCVAX (Gabe et al, 1989) and SHELXL96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_max 140
_diffrn_measurement_device_type  'Nonius CAD-4'
_diffrn_measurement_method       '\w/2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus xray tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54056
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_av_sigmaI/netI    0.0730
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16779
_diffrn_reflns_theta_max         69.81
_diffrn_reflns_theta_min         4.20
_diffrn_standards_decay_%        2.4
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    5.715
_exptl_absorpt_correction_T_max  0.8273
_exptl_absorpt_correction_T_min  0.3210
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'ABSORP in NRCVAX (Gabe et al, 1989)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.3333
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       needle
_exptl_crystal_F_000             948.0
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.00100(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL96 (Sheldrick, 1996)'
_refine_ls_goodness_of_fit_all   0.803
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         4295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.803
_refine_ls_restrained_S_obs      0.958
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.131
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0096P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0714
_refine_ls_wR_factor_ref         0.0648
_reflns_number_gt                2575
_reflns_number_total             4295
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic9912777.cif
_cod_data_source_block           rebe02
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4320942