Nonacarbonyl-μ~2~-hydrido-μ~2~-(<i>N</i>-methylcarboxamido)-<i>C</i>:<i>O</i>-(<i>N</i>-trimethylamine)triosmium(3 <i>Os</i>—<i>Os</i>)
Andrés Vega; Evgenia Spodine; Alejandro Arce; Jorge Manzur; Ana María García; María Teresa Garland; Acta Crystallographica Section C 55 (1999) 322–323; doi:10.1107/S0108270198012839

data_2008202
_publ_section_title
;Nonacarbonyl-\m~2~-hydrido-\m~2~-(<i>N</i>-methylcarboxamido)-<i>C</i>:<i>O</i>-(<i>N</i>-trimethylamine)triosmium(3
 <i>Os</i>---<i>Os</i>)
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              322
_journal_page_last               323
_journal_paper_doi               10.1107/S0108270198012839
_journal_volume                  55
_journal_year                    1999
_chemical_formula_moiety         '[Os3 H (C2 H4 NO)(C3 H9 N)(CO)9 ]'
_chemical_formula_sum            'C14 H14 N2 O10 Os3'
_chemical_formula_weight         940.87
_chemical_name_systematic
;(\m~2~-Hydrydo)-(\m~2~-N-methylcarboxamido-C,O)-trimethylamine)-
 nonacarbonyl-
tri-osmium
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.160(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.932(2)
_cell_length_b                   11.273(2)
_cell_length_c                   14.921(3)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      7.5
_cell_volume                     2141.1(7)
_computing_cell_refinement       'P3/P4-PC Diffractometer Program'
_computing_data_collection
'P3/P4-PC Diffractometer Program (Siemens, 1991)'
_computing_data_reduction        'XDISK in SHELXTL/PC (Sheldrick, 1991)'
_computing_molecular_graphics    'XP in SHELXTL'
_computing_publication_material  'XCIF in SHELXTL'
_computing_structure_refinement  'XL in SHELXTL'
_computing_structure_solution    'XS in SHELXTL (Sheldrick, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'R3m Siemens'
_diffrn_measurement_method       \q/2\q
_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  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3978
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        '< 1'
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    17.810
_exptl_absorpt_correction_T_max  0.1685
_exptl_absorpt_correction_T_min  0.0405
_exptl_absorpt_correction_type   '\y scans (SHELXTL; Sheldrick, 1993)'
_exptl_crystal_colour            Amber
_exptl_crystal_density_diffrn    2.919
_exptl_crystal_density_meas      ?
_exptl_crystal_description       polyhedra
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.803
_refine_diff_density_min         -0.758
_refine_ls_extinction_coef       0.00040(3)
_refine_ls_extinction_method     SHELXTL/PC
_refine_ls_goodness_of_fit_all   1.016
_refine_ls_goodness_of_fit_obs   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_restrained_S_obs      1.059
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_obs          0.0362
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0305P)^2^+3.3364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0787
_refine_ls_wR_factor_obs         0.0671
_reflns_number_observed          2724
_reflns_number_total             3800
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bk1418.cif
_cod_data_source_block           arcennew
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_bond_publ_flag' value 'N' changed to 'n' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (21
time).

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (9 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0305P)^2^+3.3364P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0305P)^2^+3.3364P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2141.2(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2008202