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_2021582
_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) (C O)5]'
_chemical_formula_moiety         'C30 H27 O9 Os2 P'
_chemical_formula_sum            'C30 H27 O9 Os2 P'
_chemical_formula_weight         942.88
_chemical_name_systematic
Bis(\m-acetato-1\k<i>O</i>:2\k<i>O</i>')pentacarbonyl-1\k^2^<i>C</i>,2\k^3^<i>C</i>-[tris(4-methylphenyl)phosphane-1\k<i>P</i>]diosmium(<i>Os</i>---<i>Os</i>)
_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           SHELXL-2013
_cell_angle_alpha                82.813(6)
_cell_angle_beta                 89.157(8)
_cell_angle_gamma                89.457(9)
_cell_formula_units_Z            2
_cell_length_a                   10.452(4)
_cell_length_b                   11.229(4)
_cell_length_c                   13.045(5)
_cell_measurement_reflns_used    4436
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.8
_cell_volume                     1518.8(10)
_computing_cell_refinement
;
CrystalClear (Rigaku, 2008)
;
_computing_data_collection
;
CrystalClear (Rigaku, 2008)
;
_computing_data_reduction
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CrystalClear (Rigaku, 2008)
;
_computing_molecular_graphics
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XP in SHELXTL/PC (Sheldrick, 1990)
;
_computing_publication_material
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XP in SHELXTL/PC (Sheldrick, 1990)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015a)
;
_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 0.997
_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  0.0317
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32350
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.444
_diffrn_reflns_theta_min         3.007
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    8.463
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 2001)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.062
_exptl_crystal_description       prism
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.803
_refine_diff_density_min         -1.047
_refine_ls_extinction_coef       0.00017(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2013 (Sheldrick, 2015a)
;
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         6915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0197
_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^)+(0.0130P)^2^+4.8780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0442
_refine_ls_wR_factor_ref         0.0449
_reflns_number_gt                6534
_reflns_number_total             6915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yp3178sup1.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 2021580--2021587.cif.'
_cod_database_code               2021582
_cod_database_fobs_code          2021582
_shelx_hkl_checksum              55685
_shelx_res_checksum              72338
_shelxl_version_number           .2013