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_2021586
_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 (C3 H5 O2)2 (C21 H21 P1)2 (C O)4], C H2 Cl2'
_chemical_formula_moiety         'C52 H52 O8 Os2 P2, C H2 Cl2'
_chemical_formula_sum            'C53 H54 Cl2 O8 Os2 P2'
_chemical_formula_weight         1332.20
_chemical_name_systematic
;Bis(\m-propanoato-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>),
dichloromethane monosolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 91.806(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4968(6)
_cell_length_b                   18.7369(7)
_cell_length_c                   14.9214(6)
_cell_measurement_reflns_used    11533
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      1.55
_cell_volume                     5168.8(3)
_computing_cell_refinement
;
CrystalClear (Rigaku, 2008)
;
_computing_data_collection
;
CrystalClear (Rigaku, 2008)
;
_computing_data_reduction
;
CrystalClear (Rigaku, 2008)
;
_computing_molecular_graphics
;
XP in SHELXTL/PC (Sheldrick, 1990)
;
_computing_publication_material
;
XP in SHELXTL/PC (Sheldrick, 1990)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2013)
;
_computing_structure_solution
;
SIR97 (Altomare <i>et al.</i>,  1999)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku SCX-Mini Mercury 2+ CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            54214
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_min         3.096
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    5.129
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 2001)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_description       prisms
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.390
_refine_diff_density_min         -1.324
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         11794
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+9.8357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0711
_reflns_number_gt                9639
_reflns_number_total             11794
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yp3178sup1.cif
_cod_data_source_block           7@CH2Cl2
_cod_depositor_comments
'Adding full bibliography for 2021580--2021587.cif.'
_cod_database_code               2021586
_shelx_estimated_absorpt_t_min   0.328
_shelx_estimated_absorpt_t_max   0.655
_shelx_hkl_checksum              44242
_shelx_res_checksum              11989
_shelxl_version_number           .2013