Optically active P5-deltacyclenes: selective oxidation, ligand properties, and a diastereoselective rearrangement reaction.
Keller, I. C.; Bauer, W.; Heinemann, F. W.; Höhn, C; Rohwer, L.; Zenneck, U.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 7267–7277; doi:10.1039/c6dt00548a

data_7038970
_publ_section_title
;
 Optically active P5-deltacyclenes: selective oxidation, ligand
 properties, and a diastereoselective rearrangement reaction.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7267
_journal_page_last               7277
_journal_paper_doi               10.1039/c6dt00548a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C26 H43 Cl2 O P5 Ru, 3(C4 H8 O)'
_chemical_formula_sum            'C38 H67 Cl2 O4 P5 Ru'
_chemical_formula_weight         914.73
_chemical_properties_physical    'Moisture-sensitive, Heat-sensitive'
_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   mixed
_audit_creation_date             2015-08-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-26 deposited with the CCDC.
2016-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                100.2990(10)
_cell_angle_beta                 108.0440(10)
_cell_angle_gamma                109.1480(10)
_cell_formula_units_Z            2
_cell_length_a                   10.8060(2)
_cell_length_b                   15.2568(2)
_cell_length_c                   15.4858(2)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.67
_cell_measurement_theta_min      2.38
_cell_volume                     2178.61(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      200.15
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.860
_diffrn_measurement_device_type  'Bruker Smart APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.860
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44124
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.659
_diffrn_reflns_theta_min         2.070
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0620 before and 0.0443 after correction.
The Ratio of minimum to maximum transmission is 0.8993.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofuran'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         9636
_refine_ls_number_restraints     181
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+2.5244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.1037
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7567
_reflns_number_total             9636
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00548a1.cif
_cod_data_source_block           is1205a
_cod_depositor_comments
'Adding full bibliography for 7038967--7038971.cif.'
_cod_database_code               7038970
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.817
_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 C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O1-H1
 0.9 with sigma of 0.02
 C301-C302 = C302-C303 = C303-C304
 1.52 with sigma of 0.02
 C311-C312 = C312-C313 = C313-C314
 1.52 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O300 \\sim C301 \\sim C302 \\sim C303 \\sim C304 \\sim O310 \\sim C311 \\sim
C312 \\sim C313 \\sim C314: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Same fragment restrains
{O100, C101, C102, C103, C104} sigma for 1-2: 0.01, 1-3: 0.02
{O300, C314, C313, C312, C311} sigma for 1-2: 0.01, 1-3: 0.02
as
{O300, C301, C302, C303, C304}
{O100, C101, C102, C103, C104} sigma for 1-2: 0.01, 1-3: 0.02
as
{O310, C311, C312, C313, C314}
5. Others
 Sof(O310)=Sof(C311)=Sof(H31D)=Sof(H31E)=Sof(C312)=Sof(H31F)=Sof(H31G)=
 Sof(C313)=Sof(H31H)=Sof(H31I)=Sof(C314)=Sof(H31J)=Sof(H31K)=1-FVAR(1)
 Sof(O300)=Sof(C301)=Sof(H30A)=Sof(H30B)=Sof(C302)=Sof(H30C)=Sof(H30D)=
 Sof(C303)=Sof(H30E)=Sof(H30F)=Sof(C304)=Sof(H30G)=Sof(H30H)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C102(H10C,H10D), C103(H10E,H10F), C104(H10G,H10H), C201(H20A,
 H20B), C202(H20C,H20D), C203(H20E,H20F), C204(H20G,H20H), C301(H30A,H30B),
 C302(H30C,H30D), C303(H30E,H30F), C304(H30G,H30H), C311(H31D,H31E), C312(H31F,
 H31G), C313(H31H,H31I), C314(H31J,H31K)
6.b Aromatic/amide H refined with riding coordinates:
 C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56)
6.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C)
;
_shelx_res_checksum              16252
_olex2_submission_special_instructions 'No special instructions were received'