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_7038802
_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_moiety         'C45 H85 O3 Os P2, C32 H12 B F24'
_chemical_formula_sum            'C77 H97 B F24 O3 Os P2'
_chemical_formula_weight         1789.49
_chemical_name_systematic
;
 ?
;
_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   mixed
_audit_creation_date             2014-05-23
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_audit_update_record
;
2016-01-11 deposited with the CCDC.
2016-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.723(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1764(10)
_cell_length_b                   23.3573(14)
_cell_length_c                   22.9450(13)
_cell_measurement_reflns_used    9354
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      60.69
_cell_measurement_theta_min      3.34
_cell_volume                     8093.0(9)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.820
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'BRUKER GADDS D8 Discover'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 0.820
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            63051
_diffrn_reflns_point_group_measured_fraction_full 0.820
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         59.999
_diffrn_reflns_theta_min         2.706
_exptl_absorpt_coefficient_mu    4.233
_exptl_absorpt_correction_T_max  0.7522
_exptl_absorpt_correction_T_min  0.5923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0736 before and 0.0566 after correction.
The Ratio of minimum to maximum transmission is 0.7874.
The \l/2 correction factor is Not present
;
_exptl_crystal_colour            colorless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       plate
_exptl_crystal_F_000             3640
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3 and MeOH'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.615
_refine_diff_density_min         -2.163
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         12017
_refine_ls_number_restraints     175
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0628
_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^)+(0.1122P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1705
_refine_ls_wR_factor_ref         0.1812
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8426
_reflns_number_total             12017
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00692b2.cif
_cod_data_source_block           jgb
_cod_depositor_comments
'Adding full bibliography for 7038796--7038804.cif.'
_cod_database_code               7038802
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.569
_shelx_estimated_absorpt_t_min   0.418
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All Os(H) groups
2. Restrained distances
 Os1-H1
 1.4 with sigma of 0.02
3. Rigid bond restraints
 C32, C33, C34, C35, C36, C37, C38, C39, C40
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C17, C18, C19, C20, C21, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C53, F4, F5, F6, C68, F13, F14, F15, C69, F16, F17, F18, F22, F23, F24
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim
C40: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C53 \\sim F4 \\sim F5 \\sim F6 \\sim C68 \\sim F13 \\sim F14 \\sim F15 \\sim
C69 \\sim F16 \\sim F17 \\sim F18 \\sim F22 \\sim F23 \\sim F24: within 1.7A
with sigma of 0.005 and sigma for terminal atoms of 0.01
5.a Riding coordinates:
 Os1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
  C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
 C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B)
5.c Aromatic/amide H refined with riding coordinates:
 C47(H47), C49(H49), C51(H51), C55(H55), C57(H57), C59(H59), C63(H63),
 C65(H65), C67(H67), C71(H71), C73(H73), C75(H75)
;
_shelx_res_checksum              68197