Unprecedented flexibility of the 1,1'-bis(o-carborane) ligand: catalytically-active species stabilised by B-agostic B-H⇀Ru interactions.
Riley, Laura E.; Chan, Antony P. Y.; Taylor, James; Man, Wing Y.; Ellis, David; Rosair, Georgina M.; Welch, Alan J.; Sivaev, Igor B.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 1127–1137; doi:10.1039/c5dt03417e

data_7037276
_publ_section_title
;
 Unprecedented flexibility of the 1,1'-bis(o-carborane) ligand:
 catalytically-active species stabilised by B-agostic B-H&#x21C0;Ru
 interactions.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1127
_journal_page_last               1137
_journal_paper_doi               10.1039/c5dt03417e
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C25 H35 B20 O3 P Ru, C H2 Cl2'
_chemical_formula_sum            'C26 H37 B20 Cl2 O3 P Ru'
_chemical_formula_weight         816.67
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-07
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_audit_update_record
;
2015-08-11 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                63.017(11)
_cell_angle_beta                 79.932(10)
_cell_angle_gamma                80.026(10)
_cell_formula_units_Z            2
_cell_length_a                   10.774(2)
_cell_length_b                   14.223(3)
_cell_length_c                   14.245(3)
_cell_measurement_reflns_used    7236
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.74
_cell_measurement_theta_min      2.377
_cell_volume                     1904.3(7)
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.0743
_diffrn_reflns_laue_measured_fraction_full 0.987
_diffrn_reflns_laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46419
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.357
_diffrn_reflns_theta_min         2.377
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.7035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0713 before and 0.0557 after correction.
The Ratio of minimum to maximum transmission is 0.9428.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         12119
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0350P)^2^+0.0436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0920
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8834
_reflns_number_total             12119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03417e2.cif
_cod_data_source_block           5267
_cod_depositor_comments
'Adding full bibliography for 7037273--7037280.cif.'
_cod_original_cell_volume        1904.4(7)
_cod_database_code               7037276
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.788
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
2. Shared sites
{B3', C3'}
{B2, C2}
{B3, C3}
{B2', C2'}
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl1A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C1S \\sim C2S: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(B3') = Uanis(C3')
Uanis(B2) = Uanis(C2)
Uanis(B3) = Uanis(C3)
Uanis(B2') = Uanis(C2')
4. Others
 Sof(Cl1A)=Sof(Cl2A)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=FVAR(1)
 Sof(B2')=Sof(C3')=Sof(B2)=Sof(C3)=1-FVAR(2)
 Sof(C2')=Sof(B3')=Sof(C2)=Sof(B3)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C1S(H1SA,H1SB)
5.b Aromatic/amide H refined with riding coordinates:
 C112(H112), C113(H113), C114(H114), C115(H115), C116(H116), C122(H122),
 C123(H123), C124(H124), C125(H125), C126(H126), C132(H132), C133(H133),
 C134(H134), C135(H135), C136(H136)
;
_shelx_res_checksum              55660