Asymmetric diosmium sawhorse complexes
Wilson, Kylie M.; Swartout, John W.; Touchton, Henry A.; Lambert, Erica N.; Johnstone, James E.; Archambeau, Ashley K.; Marolf, David M.; Mikeska, Emily R.; Lynch, Vincent M.; Nesterov, Vladimir N.; Reinheimer, Eric W.; Powell, Gregory L.; Powell, Cynthia B.; Acta Crystallographica Section C 75 (2019) 529–537; doi:10.1107/S2053229619004236

data_2021583
_publ_section_title
;
 Asymmetric diosmium sawhorse complexes
;
_journal_coeditor_code           YP3178
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              529
_journal_page_last               537
_journal_paper_doi               10.1107/S2053229619004236
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac
'[Os2 (C2 H3 O2)2 (C21 H21 P1)2 (C O)4], 1.5C8 H10'
_chemical_formula_moiety         'C50 H48 O8 Os2 P2, 1.5(C8 H10)'
_chemical_formula_sum            'C62 H63 O8 Os2 P2'
_chemical_formula_weight         1378.46
_chemical_name_systematic
;Bis(\m-acetato-1\k<i>O</i>:2\k<i>O</i>')bis[tris(4-methylphenyl)phosphane]-1\k<i>P</i>,2\k<i>P</i>-bis(dicarbonylosmium)(<i>Os</i>---<i>Os</i>)
<i>p</i>-xylene sesquisolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                98.1785(11)
_cell_angle_beta                 101.7904(11)
_cell_angle_gamma                113.3846(14)
_cell_formula_units_Z            2
_cell_length_a                   12.81225(16)
_cell_length_b                   14.8455(2)
_cell_length_c                   16.6818(2)
_cell_measurement_reflns_used    23482
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.1580
_cell_measurement_theta_min      3.7390
_cell_volume                     2761.39(7)
_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
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>, 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2387
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0662
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            49090
_diffrn_reflns_theta_full        66.597
_diffrn_reflns_theta_max         66.597
_diffrn_reflns_theta_min         3.349
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    9.546
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2017)
;
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             1362
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.024
_refine_diff_density_max         2.090
_refine_diff_density_min         -1.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     678
_refine_ls_number_reflns         9768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+0.5818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0678
_reflns_number_gt                8691
_reflns_number_total             9768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yp3178sup1.cif
_cod_data_source_block           4@1.5C8H10
_cod_depositor_comments
'Adding full bibliography for 2021580--2021587.cif.'
_cod_original_cell_volume        2761.37(7)
_cod_database_code               2021583
_shelx_hkl_checksum              97616
_shelx_res_checksum              28698