Further studies of the Enhanced Structural Carborane Effect: tricarbonylruthenium and related derivatives of benzocarborane, dihydrobenzocarborane and biphenylcarborane.
Powley, Samuel L.; Rosair, Georgina M.; Welch, Alan J.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 11742–11752; doi:10.1039/c6dt01888b

data_7039465
_publ_section_title
;
 Further studies of the Enhanced Structural Carborane Effect:
 tricarbonylruthenium and related derivatives of benzocarborane,
 dihydrobenzocarborane and biphenylcarborane.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11742
_journal_page_last               11752
_journal_paper_doi               10.1039/c6dt01888b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C11 H24 B9 O5 P Ru'
_chemical_formula_sum            'C11 H24 B9 O5 P Ru'
_chemical_formula_weight         465.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2016-03-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-05-12 deposited with the CCDC.
2016-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.617(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.8271(4)
_cell_length_b                   15.8356(7)
_cell_length_c                   7.9871(4)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      33.630
_cell_measurement_theta_min      2.562
_cell_volume                     985.22(8)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            27954
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         34.026
_diffrn_reflns_theta_min         2.562
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.896
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0743 before and 0.0588 after correction.
The Ratio of minimum to maximum transmission is 0.8384.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.641
_refine_diff_density_min         -2.088
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details
;
 Flack x determined using 3221 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.034(13)
_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     274
_refine_ls_number_reflns         7823
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0319P)^2^+2.0589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0952
_reflns_Friedel_coverage         0.900
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.948
_reflns_number_gt                7393
_reflns_number_total             7823
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01888b2.cif
_cod_data_source_block           5412
_cod_depositor_comments
'Adding full bibliography for 7039461--7039468.cif.'
_cod_database_code               7039465
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.694
_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.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4A), C5(H5A)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              81653
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'