Double deboronation and homometalation of 1,1'-bis(ortho-carborane).
Thiripuranathar, Gobika; Chan, Antony P. Y.; Mandal, Dipendu; Man, Wing Y.; Argentari, Mario; Rosair, Georgina M.; Welch, Alan J.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 1811–1821; doi:10.1039/c6dt04457c

data_7702124
_publ_section_title
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 Double deboronation and homometalation of 1,1'-bis(ortho-carborane).
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_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1811
_journal_page_last               1821
_journal_paper_doi               10.1039/c6dt04457c
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C24 H48 B18 Ru2'
_chemical_formula_sum            'C24 H48 B18 Ru2'
_chemical_formula_weight         733.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
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_audit_update_record
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2016-12-15 deposited with the CCDC.
2016-12-19 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 116.289(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.190(2)
_cell_length_b                   10.7869(11)
_cell_length_c                   17.9357(17)
_cell_measurement_reflns_used    5396
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      24.11
_cell_measurement_theta_min      2.29
_cell_volume                     3328.7(6)
_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 1.000
_diffrn_measured_fraction_theta_max 0.991
_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  0.1180
_diffrn_reflns_av_unetI/netI     0.0980
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            42726
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.145
_diffrn_reflns_theta_min         2.228
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_T_max  0.9639
_exptl_absorpt_correction_T_min  0.6754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       NEEDLE
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.519
_refine_diff_density_min         -1.892
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         6592
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1164
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0966P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1431
_refine_ls_wR_factor_ref         0.1714
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4105
_reflns_number_total             6592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04457c2.cif
_cod_data_source_block           3146m
_cod_original_cell_volume        3328.8(6)
_cod_database_code               7702124
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.675
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C36-C33 = C36X-C33 = C36X-C38' = C36X-C37'
 1.53 with sigma of 0.02
 C37-C30 = C37X-C30 = C37-C38 = C37-C39
 1.53 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C38 \\sim C38' \\sim C37' \\sim C37: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04
C37 \\sim C36: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C36) \\sim Ueq, Uanis(C37') \\sim Ueq, Uanis(C38') \\sim Ueq, Uanis(C37)
\\sim Ueq, Uanis(C37X) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.01
Uanis(C36) = Uanis(C36X)
Uanis(C37) = Uanis(C37X)
4. Others
 Sof(C37X)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38')=Sof(H38D)=Sof(H38E)=
 Sof(H38F)=Sof(C37')=Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(C36X)=Sof(H36X)=1-FVAR(1)
 Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39A)=
 Sof(H39B)=Sof(H39C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C21'(H21'), C22'(H22'), C24'(H24'), C25'(H25'), C27'(H27'), C31(H31),
 C32(H32), C34(H34), C35(H35), C37(H37), C36X(H36X)
5.b Me refined with riding coordinates:
 C37X(H37A,H37B,H37C), C37'(H37D,H37E,H37F), C36(H36A,H36B,H36C)
5.c Idealised Me refined as rotating group:
 C26'(H26A,H26B,H26C), C28'(H28A,H28B,H28C), C29'(H29A,H29B,H29C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C38'(H38D,H38E,H38F)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'