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_7038796
_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            'C50 H96 Cl2 O2 Os P2'
_chemical_formula_weight         1052.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-01-11 deposited with the CCDC.
2016-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.261(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.4907(12)
_cell_length_b                   16.8895(10)
_cell_length_c                   36.622(2)
_cell_measurement_reflns_used    7990
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      59.50
_cell_measurement_theta_min      2.53
_cell_volume                     10815.9(11)
_computing_cell_refinement
; 
  CELL-NOW (Sheldrick, 2003) and SAINT (BRUKER-NONIUS, 2003) 
;
_computing_data_collection       'FRAMBO (BRUKER-NONIUS, 2003)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'BRUKER GADDS D8 Discover'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0838
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            83787
_diffrn_reflns_theta_full        60.00
_diffrn_reflns_theta_max         60.00
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    6.169
_exptl_absorpt_correction_T_max  0.8866
_exptl_absorpt_correction_T_min  0.3077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4416
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: C6D6 and MeOH'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.007
_refine_diff_density_min         -1.736
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1373
_refine_ls_number_reflns         15622
_refine_ls_number_restraints     1904
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          2.791
_refine_ls_shift/su_mean         0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+70.4906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1488
_refine_ls_wR_factor_ref         0.1642
_reflns_number_gt                11572
_reflns_number_total             15622
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt00692b2.cif
_cod_data_source_block           jgb
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7038796--7038804.cif.
;
_cod_original_cell_volume        10815.9(12)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7038796