(BB)-Carboryne Complex of Ruthenium: Synthesis by Double B-H Activation at a Single Metal Center.
Eleazer, Bennett J.; Smith, Mark D.; Popov, Alexey A.; Peryshkov, Dmitry V.; Journal of the American Chemical Society 138 (2016) 10531–10538; doi:10.1021/jacs.6b05172

data_4125192
_publ_section_title
;
 (BB)-Carboryne Complex of Ruthenium: Synthesis by Double B-H Activation
 at a Single Metal Center.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10531
_journal_page_last               10538
_journal_paper_doi               10.1021/jacs.6b05172
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C15 H36 B10 I2 O3 P2 Ru, 0.5(C6 D6)'
_chemical_formula_sum            'C18 H36 B10 D3 I2 O3 P2 Ru'
_chemical_formula_weight         831.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.388(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7357(8)
_cell_length_b                   12.9295(7)
_cell_length_c                   15.8165(8)
_cell_measurement_reflns_used    9434
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.57
_cell_measurement_theta_min      2.61
_cell_volume                     3130.5(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEXII v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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(2)
_diffrn_detector                 'Bruker PHOTON-100 area detector'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            95071
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        32.633
_diffrn_reflns_theta_max         32.633
_diffrn_reflns_theta_min         2.278
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.596
_exptl_absorpt_correction_T_max  0.3834
_exptl_absorpt_correction_T_min  0.3114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0995 before and 0.0420 after correction.
The Ratio of minimum to maximum transmission is 0.8122.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_description       plate
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.794
_refine_diff_density_min         -1.628
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       0.00054(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         5939
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0188
_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^)+(0.0208P)^2^+7.5436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0452
_refine_ls_wR_factor_ref         0.0472
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5324
_reflns_number_total             5939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b05172_si_002.cif
_cod_data_source_block           be337_2
_cod_depositor_comments
'Adding full bibliography for 4125189--4125194.cif.'
_cod_database_code               4125192
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.575
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C2S) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
3. Rigid body (RIGU) restrains
 C1S, C2S, C3S, C4S, C5S, C6S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C1S(0.25) D1S(0.25) C2S(0.25) D2S(0.25) C3S(0.25) D3S(0.25)
 C4S(0.25) D4S(0.25) C5S(0.25) D5S(0.25) C6S(0.25) D6S(0.25)
5.a Ternary CH refined with riding coordinates:
 C11(H11), C21(H21)
5.b Aromatic/amide H refined with riding coordinates:
 C1S(D1S), C2S(D2S), C3S(D3S), C4S(D4S), C5S(D5S), C6S(D6S)
5.c Fitted hexagon refined as free rotating group:
 C1S(C2S,C3S,C4S,C5S,C6S)
5.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C)
;
_shelx_res_checksum              89282
_shelx_hkl_checksum              1181
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'