(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_4125191
_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         'C21 H42 B10 O6 P2 Ru'
_chemical_formula_sum            'C21 H42 B10 O6 P2 Ru'
_chemical_formula_weight         661.65
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.6060(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6818(8)
_cell_length_b                   8.9257(3)
_cell_length_c                   19.5607(8)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.13
_cell_measurement_theta_min      2.18
_cell_volume                     3260.4(2)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0967
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            53855
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.383
_diffrn_reflns_theta_max         26.383
_diffrn_reflns_theta_min         2.324
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  0.5623
_exptl_absorpt_correction_T_min  0.5454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0766 before and 0.0602 after correction.
The Ratio of minimum to maximum transmission is 0.9699.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         6658
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0275P)^2^+3.7084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0812
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4973
_reflns_number_total             6658
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b05172_si_002.cif
_cod_data_source_block           be312a
_cod_depositor_comments
'Adding full bibliography for 4125189--4125194.cif.'
_cod_database_code               4125191
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.867
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O5C-H9CB
 -2.2 with sigma of 0.02
 C7C-C6 \\sim C7B-C6 \\sim C7A-C6
 with sigma of 0.01
 O5B-C7B \\sim O5C-C7C \\sim O5A-C7A
 with sigma of 0.01
 O6A-C7A \\sim O6C-C7C \\sim O6B-C7B
 with sigma of 0.01
 O6B-C8B \\sim O6C-C8C \\sim O6A-C8A
 with sigma of 0.01
 C9C-C8C \\sim C9A-C8A \\sim C9B-C8B
 with sigma of 0.01
3. Restrained planarity
 C7A, C8A, O5A, O6A
 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(C7A) = Uanis(C7B) = Uanis(C7C)
Uanis(O6B) = Uanis(O6A) = Uanis(O6C)
Uanis(O5A) = Uanis(O5B) = Uanis(O5C)
Uiso(C8B) = Uiso(C8C) = Uiso(C8A)
Uiso(C9A) = Uiso(C9B) = Uiso(C9C)
Uiso(H4) = Uiso(H5)
5. Same fragment restrains
{C7A, C8A, C9A, O5A, O6A} sigma for 1-2: 0.02, 1-3: 0.04
as
{C7B, C8B, C9B, O5B, O6B}
{C7A, C8A, C9A, O5A, O6A} sigma for 1-2: 0.02, 1-3: 0.04
as
{C7C, C8C, C9C, O5C, O6C}
6. Others
 1*[Sof(C7A)+Sof(C8A)+Sof(H8AA)+Sof(H8AB)+Sof(C9A)+Sof(H9AA)+Sof(H9AB)+
 Sof(H9AC)+Sof(O5A)+Sof(O6A)]+1*[Sof(C7B)+Sof(C8B)+Sof(H8BA)+Sof(H8BB)+Sof(C9B)+
 Sof(H9BA)+Sof(H9BB)+Sof(H9BC)+Sof(O5B)+Sof(O6B)]+1*[Sof(C7C)+Sof(C8C)+
 Sof(H8CA)+Sof(H8CB)+Sof(C9C)+Sof(H9CA)+Sof(H9CB)+Sof(H9CC)+Sof(O5C)+Sof(O6C)]=
 1 with esd of 0.00001
 Sof(C7A)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=
 Sof(O5A)=Sof(O6A)=FVAR(1)
 Sof(C7B)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=
 Sof(O5B)=Sof(O6B)=FVAR(2)
 Sof(C7C)=Sof(C8C)=Sof(H8CA)=Sof(H8CB)=Sof(C9C)=Sof(H9CA)=Sof(H9CB)=Sof(H9CC)=
 Sof(O5C)=Sof(O6C)=FVAR(3)
7.a Ternary CH refined with riding coordinates:
 C11(H11), C21(H21), C31(H31), C41(H41)
7.b Secondary CH2 refined with riding coordinates:
 C8A(H8AA,H8AB), C8B(H8BA,H8BB), C8C(H8CA,H8CB)
7.c Idealised Me refined as rotating group:
 C9A(H9AA,H9AB,H9AC), C9B(H9BA,H9BB,H9BC), C9C(H9CA,H9CB,H9CC), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              3556
_shelx_hkl_checksum              12219
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'