Decacarbonyl(μ-ethylidenimino-1κ<i>N</i>:2κ<i>C</i>)-μ-hydrido-<i>triangulo</i>-triosmium(3<i>Os</i>‒<i>Os</i>)
Powell, Cynthia B.; Powell, Gregory L.; Archambeau, Ashley K.; Wilson, Kylie M.; IUCrData 4 (2019) x191386–; doi:10.1107/S2414314619013865

data_1552478
_publ_section_title
;
 Decacarbonyl(\m-ethylidenimino-1\k<i>N</i>:2\k<i>C</i>)-\m-hydrido-<i>triangulo</i>-triosmium(3<i>Os</i>--<i>Os</i>)
;
_journal_coeditor_code           WM4114
_journal_issue                   10
_journal_name_full               IUCrData
_journal_page_first              x191386
_journal_paper_doi               10.1107/S2414314619013865
_journal_volume                  4
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_iupac          '[Os3 (C2 H4 N) H (C O)10]'
_chemical_formula_moiety         'C12 H5 N O10 Os3'
_chemical_formula_sum            'C12 H5 N O10 Os3'
_chemical_formula_weight         893.77
_chemical_name_systematic
'Decacarbonyl(\m-ethylidenimino-1\k<i>N</i>:2\k<i>C</i>)-\m-hydrido-<i>triangulo</i>-triosmium(3 <i>Os</i>--<i>Os</i>)'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.56470(6)
_cell_length_b                   11.59555(8)
_cell_length_c                   15.61610(11)
_cell_measurement_reflns_used    23076
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.4550
_cell_measurement_theta_min      3.7850
_cell_volume                     1731.95(2)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>, 2009)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2387
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku SuperNova AtlasS2 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33313
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.577
_diffrn_reflns_theta_min         4.750
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    41.178
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10920
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(<i>CrysAlis PRO</i>; Rigaku OD, 2017)
;
_exptl_crystal_colour            'clear reddish orange'
_exptl_crystal_density_diffrn    3.428
_exptl_crystal_description       plate
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.153
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.891
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.465(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3487
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0153
_refine_ls_R_factor_gt           0.0152
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
' w=1/[\s^2^(Fo^2^)+(0.0177P)^2^+1.9300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0368
_refine_ls_wR_factor_ref         0.0368
_reflns_number_gt                3471
_reflns_number_total             3487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm4114sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 1552478.cif.'
_cod_database_code               1552478
_cod_database_fobs_code          1552478
_shelx_estimated_absorpt_t_min   0.062
_shelx_estimated_absorpt_t_max   0.451
_shelx_hkl_checksum              20287
_shelx_res_checksum              3741