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_2021587
_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 (C H O2)2 (C21 H21 P1)2 (C O)4]'
_chemical_formula_moiety         'C48 H44 O8 Os2 P2'
_chemical_formula_sum            'C48 H44 O8 Os2 P2'
_chemical_formula_weight         1191.17
_chemical_name_systematic
Bis(\m-formato-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>)
_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                104.3930(10)
_cell_angle_beta                 91.0090(10)
_cell_angle_gamma                98.9930(10)
_cell_formula_units_Z            2
_cell_length_a                   10.7707(4)
_cell_length_b                   10.8014(4)
_cell_length_c                   20.3790(7)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.072
_cell_measurement_theta_min      2.450
_cell_volume                     2264.27(14)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
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APEX2 (Bruker, 2009)
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_computing_data_reduction
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SAINT (Bruker, 2009)
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_computing_molecular_graphics
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<i>OLEX2</i> (Dolomanov <i>et al.</i>, 2009)
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_computing_publication_material
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<i>OLEX2</i> (Dolomanov <i>et al.</i>, 2009)
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_computing_structure_refinement
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SHELXL2018 (Sheldrick, 2015b)
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_computing_structure_solution
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SHELXT (Sheldrick, 2015a)
;
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_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30910
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.107
_diffrn_reflns_theta_min         1.033
_exptl_absorpt_coefficient_mu    5.729
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            colorless
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_exptl_crystal_description       block
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.037
_refine_diff_density_max         1.190
_refine_diff_density_min         -1.090
_refine_ls_extinction_coef       0.00032(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         9960
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+1.5967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0817
_reflns_number_gt                8554
_reflns_number_total             9960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yp3178sup1.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 2021580--2021587.cif.'
_cod_database_code               2021587
_cod_database_fobs_code          2021587
_shelx_estimated_absorpt_t_min   0.486
_shelx_estimated_absorpt_t_max   0.816
_shelx_hkl_checksum              79012
_shelx_res_checksum              50618