Gyroscope like molecules consisting of trigonal or square planar osmium rotators within three-spoked dibridgehead diphosphine stators: syntheses, substitution reactions, structures, and dynamic properties.
Fiedler, Tobias; Bhuvanesh, Nattamai; Hampel, Frank; Reibenspies, Joseph H.; Gladysz, John A.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 7131–7147; doi:10.1039/c6dt00692b

data_7038803
_publ_section_title
;
 Gyroscope like molecules consisting of trigonal or square planar osmium
 rotators within three-spoked dibridgehead diphosphine stators: syntheses,
 substitution reactions, structures, and dynamic properties.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7131
_journal_page_last               7147
_journal_paper_doi               10.1039/c6dt00692b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C46 H90 O2 Os P2'
_chemical_formula_weight         927.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2016-01-14 deposited with the CCDC.
2016-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.549(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.496(8)
_cell_length_b                   17.609(10)
_cell_length_c                   19.880(11)
_cell_measurement_reflns_used    9841
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.93
_cell_measurement_theta_min      2.36
_cell_volume                     4694(5)
_computing_cell_refinement       'APEXII (Bruker, 2012a)'
_computing_data_collection       'APEXII (Bruker, 2012a)'
_computing_data_reduction        'SAINT (Bruker, 2012b)'
_computing_molecular_graphics    'shelXLe (H\"ubschle 2011)'
_computing_publication_material  'Ciftab (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            56220
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.127
_diffrn_reflns_theta_min         1.549
_exptl_absorpt_coefficient_mu    2.818
_exptl_absorpt_correction_T_max  0.7658
_exptl_absorpt_correction_T_min  0.4852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2009/1 (Bruker,2009) was employed for absorption correction.
The \l/2 correction was not applied
;
_exptl_crystal_colour            'colorless '
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         11876
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0197
_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^)+(0.0146P)^2^+3.0744P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0437
_refine_ls_wR_factor_ref         0.0522
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9230
_reflns_number_total             11876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00692b2.cif
_cod_data_source_block           jg
_cod_depositor_comments
'Adding full bibliography for 7038796--7038804.cif.'
_cod_database_code               7038803
_shelx_estimated_absorpt_t_min   0.485
_shelx_estimated_absorpt_t_max   0.766
_shelxl_version_number           2014-3
_shelx_res_checksum              10281