Water and catalytic isomerization of linear allylic alcohols by [RuCp(H2O-κO)(PTA)2](+) (PTA = 1,3,5-triaza-7-phosphaadamantane).
Scalambra, Franco; Serrano-Ruiz, Manuel; Romerosa, Antonio; Dalton transactions (Cambridge, England : 2003)  (2017) –; doi:10.1039/c6dt04262g

data_7043803
_publ_section_title
;
 Water and catalytic isomerization of linear allylic alcohols by
 [RuCp(H2O-\kO)(PTA)2](+) (PTA = 1,3,5-triaza-7-phosphaadamantane).
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/c6dt04262g
_journal_year                    2017
_chemical_formula_moiety
'C17 H31 N6 O P2 Ru, C F3 O3 S, 3(H2 O), 0.25(O)'
_chemical_formula_sum            'C18 H37 F3 N6 O7.25 P2 Ru S'
_chemical_formula_weight         705.60
_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             2017-03-21
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.03.14 svn.r3398 for OlexSys, GUI svn.r5328)
;
_audit_update_record
;
2017-03-23 deposited with the CCDC.
2017-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                76.368(2)
_cell_angle_beta                 80.526(2)
_cell_angle_gamma                78.260(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1001(2)
_cell_length_b                   10.7058(3)
_cell_length_c                   15.0268(3)
_cell_measurement_reflns_used    6416
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.34
_cell_measurement_theta_min      2.81
_cell_volume                     1382.46(6)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  Rigaku_AFC12K_724P_007HF_Mo
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30726
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.346
_diffrn_reflns_theta_min         3.291
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.051
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         6954
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0224
_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^)+(0.0231P)^2^+0.6965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0530
_refine_ls_wR_factor_ref         0.0548
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6416
_reflns_number_total             6954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04262g2.cif
_cod_data_source_block           pta2rucph2o
_cod_database_code               7043803
_shelx_shelxl_version_number     2014/7
_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 O(H,H) groups
2. Others
 Sof(O4W')=0.25*(1-FVAR(2))
 Sof(O4W)=0.25*FVAR(2)
3.a Free rotating group:
 O3W(H3WA,H3WB), O2W(H2WA,H2WB), O1W(H1WA,H1WB)
3.b Rotating group:
 O1(H1A,H1B)
3.c Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,
 H15B), C16(H16A,H16B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B),
 C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B)
3.d Aromatic/amide H refined with riding coordinates:
 C31(H31), C32(H32), C33(H33), C34(H34), C35(H35)
;
_olex2_submission_special_instructions 'No special instructions were received'