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_7037279
_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         'C34 H50 B20 N2 P2 Ru, 3(C2 H3 N)'
_chemical_formula_sum            'C40 H59 B20 N5 P2 Ru'
_chemical_formula_weight         989.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-06
_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                90
_cell_angle_beta                 94.465(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.5530(9)
_cell_length_b                   19.6096(8)
_cell_length_c                   23.5945(10)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.890
_cell_measurement_theta_min      2.466
_cell_volume                     9941.8(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      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_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  0.0429
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            107261
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.099
_diffrn_reflns_theta_min         2.250
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.417
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.7123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0783 before and 0.0488 after correction.
The Ratio of minimum to maximum transmission is 0.9548.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       block
_exptl_crystal_F_000             4064
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         14488
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+15.3671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.1023
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11576
_reflns_number_total             14488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03417e2.cif
_cod_data_source_block           5259
_cod_depositor_comments
'Adding full bibliography for 7037273--7037280.cif.'
_cod_database_code               7037279
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.892
_shelx_estimated_absorpt_t_min   0.800
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N6S) = Uanis(N3S)
Uanis(N12T) = Uanis(N12S)
3. Others
 Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=Sof(C2S)=Sof(N3S)=1-FVAR(1)
 Sof(C4S)=Sof(H4SA)=Sof(H4SB)=Sof(H4SC)=Sof(C5S)=Sof(N6S)=FVAR(1)
 Sof(C11T)=Sof(N12T)=1-FVAR(2)
 Sof(C10S)=Sof(N12S)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C100(H10A,H10B), C200(H20A,H20B)
4.b Aromatic/amide H refined with riding coordinates:
 C102(H102), C103(H103), C104(H104), C105(H105), C106(H106), C112(H112),
 C113(H113), C114(H114), C115(H115), C116(H116), C202(H202), C203(H203),
 C204(H204), C205(H205), C206(H206), C212(H212), C213(H213), C214(H214),
 C215(H215), C216(H216)
4.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C22(H22A,H22B,H22C), C10S(H10C,H10D,H10E), C7S(H7SA,H7SB,
 H7SC), C1S(H1SA,H1SB,H1SC), C4S(H4SA,H4SB,H4SC)
;
_shelx_res_checksum              87176