#------------------------------------------------------------------------------
#$Date: 2016-05-06 04:40:01 +0300 (Fri, 06 May 2016) $
#$Revision: 182722 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/88/7038801.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7038801
loop_
_publ_author_name
'Fiedler, Tobias'
'Bhuvanesh, Nattamai'
'Hampel, Frank'
'Reibenspies, Joseph H.'
'Gladysz, John A.'
_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            'C45 H84 O3 Os P2'
_chemical_formula_weight         925.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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
;
2016-01-14 deposited with the CCDC.
2016-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 122.109(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.6848(5)
_cell_length_b                   14.0336(2)
_cell_length_c                   18.2091(4)
_cell_measurement_reflns_used    5313
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.22
_cell_volume                     4693.71(17)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'SHELXTL NT'
_computing_publication_material  'SHELXTL NT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0150
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10253
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    2.820
_exptl_absorpt_correction_T_max  0.6024
_exptl_absorpt_correction_T_min  0.5391
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Scalepack
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.585
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         5368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0197
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0236P)²+1.7630P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0474
_refine_ls_wR_factor_ref         0.0481
_reflns_number_gt                5111
_reflns_number_total             5368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt00692b2.cif
_cod_data_source_block           tf03
_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        4693.71(16)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7038801
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Os1 Os 0.0000 0.989412(6) 0.2500 0.02195(4) Uani 1 2 d S
P1 P 0.12806(3) 0.98758(3) 0.33336(3) 0.02204(10) Uani 1 1 d .
O1 O 0.00540(9) 0.88626(13) 0.10476(11) 0.0538(4) Uani 1 1 d .
C1 C 0.00291(10) 0.92449(14) 0.15952(13) 0.0337(4) Uani 1 1 d .
O2 O 0.0000 1.20715(15) 0.2500 0.0611(7) Uani 1 2 d S
C2 C 0.0000 1.1241(2) 0.2500 0.0356(6) Uani 1 2 d S
C11 C 0.17352(12) 1.00977(12) 0.27401(14) 0.0277(4) Uani 1 1 d .
H11A H 0.2266 1.0156 0.3162 0.033 Uiso 1 1 calc R
H11B H 0.1656 0.9543 0.2364 0.033 Uiso 1 1 calc R
C12 C 0.14660(10) 1.09969(14) 0.21807(13) 0.0303(4) Uani 1 1 d .
H12A H 0.0945 1.0916 0.1726 0.036 Uiso 1 1 calc R
H12B H 0.1506 1.1544 0.2547 0.036 Uiso 1 1 calc R
C13 C 0.18903(11) 1.12206(15) 0.17513(13) 0.0337(4) Uani 1 1 d .
H13A H 0.1938 1.0631 0.1487 0.040 Uiso 1 1 calc R
H13B H 0.2386 1.1433 0.2201 0.040 Uiso 1 1 calc R
C14 C 0.15300(12) 1.19910(15) 0.10525(13) 0.0358(5) Uani 1 1 d .
H14A H 0.1816 1.2070 0.0777 0.043 Uiso 1 1 calc R
H14B H 0.1037 1.1771 0.0600 0.043 Uiso 1 1 calc R
C15 C 0.14637(12) 1.29550(15) 0.13853(14) 0.0358(5) Uani 1 1 d .
H15A H 0.1947 1.3139 0.1886 0.043 Uiso 1 1 calc R
H15B H 0.1127 1.2894 0.1594 0.043 Uiso 1 1 calc R
C16 C 0.11879(13) 1.37508(16) 0.07074(15) 0.0419(5) Uani 1 1 d .
H16A H 0.1162 1.4348 0.0979 0.050 Uiso 1 1 calc R
H16B H 0.1549 1.3849 0.0539 0.050 Uiso 1 1 calc R
C17 C 0.04461(12) 1.35743(15) -0.01114(14) 0.0370(5) Uani 1 1 d .
H17A H 0.0472 1.2984 -0.0392 0.044 Uiso 1 1 calc R
H17B H 0.0335 1.4107 -0.0520 0.044 Uiso 1 1 calc R
C18 C -0.01733(13) 1.34788(16) 0.00485(14) 0.0380(5) Uani 1 1 d .
H18A H -0.0071 1.2932 0.0441 0.046 Uiso 1 1 calc R
H18B H -0.0190 1.4060 0.0346 0.046 Uiso 1 1 calc R
C19 C -0.09124(12) 1.33345(15) -0.07737(14) 0.0364(5) Uani 1 1 d .
H19A H -0.0912 1.2718 -0.1038 0.044 Uiso 1 1 calc R
H19B H -0.0992 1.3845 -0.1191 0.044 Uiso 1 1 calc R
C20 C -0.15451(12) 1.33416(15) -0.06267(15) 0.0393(5) Uani 1 1 d .
H20A H -0.1546 1.3960 -0.0365 0.047 Uiso 1 1 calc R
H20B H -0.2008 1.3295 -0.1196 0.047 Uiso 1 1 calc R
C21 C -0.15229(11) 1.25405(14) -0.00444(13) 0.0343(4) Uani 1 1 d .
H21A H -0.1030 1.2516 0.0486 0.041 Uiso 1 1 calc R
H21B H -0.1871 1.2692 0.0134 0.041 Uiso 1 1 calc R
C22 C -0.17082(12) 1.15609(15) -0.04735(13) 0.0376(5) Uani 1 1 d .
H22A H -0.1498 1.1505 -0.0840 0.045 Uiso 1 1 calc R
H22B H -0.2244 1.1503 -0.0857 0.045 Uiso 1 1 calc R
C23 C -0.14214(12) 1.07410(14) 0.01837(13) 0.0349(4) Uani 1 1 d .
H23A H -0.1562 1.0129 -0.0135 0.042 Uiso 1 1 calc R
H23B H -0.0883 1.0770 0.0535 0.042 Uiso 1 1 calc R
C24 C -0.17068(10) 1.07605(13) 0.07932(12) 0.0276(4) Uani 1 1 d .
H24A H -0.2239 1.0648 0.0449 0.033 Uiso 1 1 calc R
H24B H -0.1623 1.1403 0.1054 0.033 Uiso 1 1 calc R
C31 C 0.16789(10) 0.87480(13) 0.38959(12) 0.0279(4) Uani 1 1 d .
H31A H 0.2216 0.8793 0.4198 0.034 Uiso 1 1 calc R
H31B H 0.1555 0.8653 0.4342 0.034 Uiso 1 1 calc R
C32 C 0.14222(11) 0.78794(13) 0.32980(13) 0.0319(4) Uani 1 1 d .
H32A H 0.0892 0.7938 0.2873 0.038 Uiso 1 1 calc R
H32B H 0.1668 0.7877 0.2970 0.038 Uiso 1 1 calc R
C33 C 0.15701(10) 0.69352(13) 0.37733(12) 0.0294(4) Uani 1 1 d .
H33A H 0.2103 0.6840 0.4151 0.035 Uiso 1 1 calc R
H33B H 0.1368 0.6958 0.4149 0.035 Uiso 1 1 calc R
C34 C 0.12390(11) 0.60963(13) 0.31558(13) 0.0317(4) Uani 1 1 d .
H34A H 0.1449 0.6072 0.2788 0.038 Uiso 1 1 calc R
H34B H 0.0709 0.6204 0.2770 0.038 Uiso 1 1 calc R
C35 C 0.13607(15) 0.51376(13) 0.36033(15) 0.0366(5) Uani 1 1 d .
H35A H 0.1133 0.5150 0.3951 0.044 Uiso 1 1 calc R
H35B H 0.1890 0.5038 0.4006 0.044 Uiso 1 1 calc R
C36 C 0.10480(14) 0.42958(15) 0.29685(15) 0.0433(5) Uani 1 1 d .
H36A H 0.1307 0.4258 0.2656 0.052 Uiso 1 1 calc R
H36B H 0.1153 0.3701 0.3308 0.052 Uiso 1 1 calc R
C37 C 0.02369(13) 0.43389(14) 0.23050(13) 0.0388(5) Uani 1 1 d .
H37A H 0.0100 0.3785 0.1911 0.047 Uiso 1 1 calc R
H37B H 0.0131 0.4923 0.1952 0.047 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C2 Os1 C1 118.44(6) . .
C2 Os1 C1 118.44(6) . 2
C1 Os1 C1 123.11(12) . 2
C2 Os1 P1 90.627(10) . .
C1 Os1 P1 89.00(6) . .
C1 Os1 P1 90.40(6) 2 .
C2 Os1 P1 90.627(10) . 2
C1 Os1 P1 90.40(6) . 2
C1 Os1 P1 89.00(6) 2 2
P1 Os1 P1 178.75(2) . 2
C31 P1 C24 103.28(9) . 2
C31 P1 C11 103.54(9) . .
C24 P1 C11 102.40(9) 2 .
C31 P1 Os1 114.46(6) . .
C24 P1 Os1 115.48(6) 2 .
C11 P1 Os1 115.94(7) . .
O1 C1 Os1 178.92(19) . .
O2 C2 Os1 180.000(1) . .
C12 C11 P1 113.44(13) . .
C13 C12 C11 113.02(16) . .
C12 C13 C14 113.05(16) . .
C15 C14 C13 114.33(17) . .
C14 C15 C16 114.01(17) . .
C17 C16 C15 115.28(18) . .
C16 C17 C18 113.98(19) . .
C19 C18 C17 113.54(19) . .
C18 C19 C20 113.67(18) . .
C21 C20 C19 114.57(17) . .
C22 C21 C20 113.88(18) . .
C21 C22 C23 112.91(17) . .
C24 C23 C22 113.55(16) . .
C23 C24 P1 113.87(13) . 2
C32 C31 P1 113.93(13) . .
C33 C32 C31 113.74(16) . .
C34 C33 C32 112.35(16) . .
C33 C34 C35 114.19(17) . .
C34 C35 C36 113.31(19) . .
C37 C36 C35 115.49(18) . .
C36 C37 C37 114.3(2) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Os1 C2 1.891(3) .
Os1 C1 1.913(2) .
Os1 C1 1.913(2) 2
Os1 P1 2.3526(5) .
Os1 P1 2.3526(5) 2
P1 C31 1.8328(18) .
P1 C24 1.8335(18) 2
P1 C11 1.836(2) .
O1 C1 1.159(2) .
O2 C2 1.165(4) .
C11 C12 1.529(3) .
C12 C13 1.524(3) .
C13 C14 1.530(3) .
C14 C15 1.520(3) .
C15 C16 1.531(3) .
C16 C17 1.524(3) .
C17 C18 1.524(3) .
C18 C19 1.517(3) .
C19 C20 1.531(3) .
C20 C21 1.528(3) .
C21 C22 1.526(3) .
C22 C23 1.534(3) .
C23 C24 1.531(3) .
C24 P1 1.8335(18) 2
C31 C32 1.529(3) .
C32 C33 1.521(2) .
C33 C34 1.519(3) .
C34 C35 1.521(3) .
C35 C36 1.536(3) .
C36 C37 1.516(3) .
C37 C37 1.529(4) 2
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C2 Os1 P1 C31 160.70(7) . .
C1 Os1 P1 C31 -80.86(9) . .
C1 Os1 P1 C31 42.25(9) 2 .
P1 Os1 P1 C31 -19.30(7) 2 .
C2 Os1 P1 C24 40.94(7) . 2
C1 Os1 P1 C24 159.38(9) . 2
C1 Os1 P1 C24 -77.51(9) 2 2
P1 Os1 P1 C24 -139.06(7) 2 2
C2 Os1 P1 C11 -78.82(6) . .
C1 Os1 P1 C11 39.62(9) . .
C1 Os1 P1 C11 162.73(9) 2 .
P1 Os1 P1 C11 101.18(6) 2 .
C2 Os1 C1 O1 37(11) . .
C1 Os1 C1 O1 -143(11) 2 .
P1 Os1 C1 O1 -53(11) . .
P1 Os1 C1 O1 128(11) 2 .
C1 Os1 C2 O2 124(100) . .
C1 Os1 C2 O2 -56(100) 2 .
P1 Os1 C2 O2 -147(100) . .
P1 Os1 C2 O2 33(100) 2 .
C31 P1 C11 C12 177.63(14) . .
C24 P1 C11 C12 -75.22(16) 2 .
Os1 P1 C11 C12 51.42(16) . .
P1 C11 C12 C13 175.14(14) . .
C11 C12 C13 C14 168.27(17) . .
C12 C13 C14 C15 62.0(2) . .
C13 C14 C15 C16 173.03(18) . .
C14 C15 C16 C17 58.3(3) . .
C15 C16 C17 C18 62.2(3) . .
C16 C17 C18 C19 178.17(18) . .
C17 C18 C19 C20 -174.03(17) . .
C18 C19 C20 C21 -62.8(3) . .
C19 C20 C21 C22 -72.7(3) . .
C20 C21 C22 C23 158.90(18) . .
C21 C22 C23 C24 58.2(2) . .
C22 C23 C24 P1 -172.73(15) . 2
C24 P1 C31 C32 -178.61(13) 2 .
C11 P1 C31 C32 -72.13(16) . .
Os1 P1 C31 C32 55.02(15) . .
P1 C31 C32 C33 -163.26(14) . .
C31 C32 C33 C34 174.01(16) . .
C32 C33 C34 C35 -178.85(18) . .
C33 C34 C35 C36 -177.71(18) . .
C34 C35 C36 C37 -58.8(3) . .
C35 C36 C37 C37 -61.72(19) . 2
