Synthesis of aromatic ruthenabenzothiophenes via C-H activation of thiophenes.
Zhuo, Qingde; Chen, Zhiyong; Yang, Yuhui; Zhou, Xiaoxi; Han, Feifei; Zhu, Jun; Zhang, Hong; Xia, Haiping; Dalton transactions (Cambridge, England : 2003) 45 (2016) 913–917; doi:10.1039/c5dt04557f

data_7037626
_publ_section_title
;
 Synthesis of aromatic ruthenabenzothiophenes via C-H activation of
 thiophenes.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              913
_journal_page_last               917
_journal_paper_doi               10.1039/c5dt04557f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'C52 H44 B N6 P2 Ru S 1+, B F4 1-, 2(C H2 Cl2)'
_chemical_formula_sum            'C54 H48 B2 Cl4 F4 N6 P2 Ru S'
_chemical_formula_weight         1215.47
_chemical_name_systematic
;
 ?
;
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-11-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-11-25 deposited with the CCDC.
2015-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.260(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2188(7)
_cell_length_b                   15.6604(6)
_cell_length_c                   21.8580(9)
_cell_measurement_reflns_used    3745
_cell_measurement_temperature    173
_cell_measurement_theta_max      23.4950
_cell_measurement_theta_min      3.5030
_cell_volume                     5494.2(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0844
_diffrn_reflns_laue_measured_fraction_full 0.970
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26396
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.887
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98985
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       block
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.104
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         9641
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0356P)^2^+0.1994P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1095
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7346
_reflns_number_total             9641
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04557f2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7037626--7037628.cif.'
_cod_database_code               7037626
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1A)
2.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C6(H6), C7(H7), C14(H14), C16(H16), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29),
  C30(H30), C33(H33), C37(H37), C39(H39), C40(H40), C41(H41), C43(H43),
 C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52),
  C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C61(H61),
 C62(H62), C63(H63), C66(H66), C68(H68), C69(H69)
;
_shelx_res_checksum              32606
_olex2_submission_special_instructions 'No special instructions were received'