Synthesis of Fused Metallaaromatics via Intramolecular C‒H Activation of Thiophenes
Zhuo, Qingde; Zhou, Xiaoxi; Kang, Huijun; Chen, Zhiyong; Yang, Yuhui; Han, Feifei; Zhang, Hong; Xia, Haiping; Organometallics 35 (2016) 1497–; doi:10.1021/acs.organomet.6b00083

data_4088439
_publ_section_title
;
 Synthesis of Fused Metallaaromatics via Intramolecular C--H Activation of
 Thiophenes
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1497
_journal_paper_doi               10.1021/acs.organomet.6b00083
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety
'C61 H50 Cl2 Os P3 S 1+, B F4 1-, 2(C H2 Cl2)'
_chemical_formula_sum            'C63 H54 B Cl6 F4 O0 Os P3 S'
_chemical_formula_weight         1425.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-01-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                93.119(2)
_cell_angle_beta                 103.706(2)
_cell_angle_gamma                110.115(3)
_cell_formula_units_Z            2
_cell_length_a                   12.8967(4)
_cell_length_b                   13.0323(4)
_cell_length_c                   19.7300(5)
_cell_measurement_reflns_used    7678
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      27.2020
_cell_measurement_theta_min      3.2160
_cell_volume                     2991.40(17)
_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      173.00(14)
_diffrn_measured_fraction_theta_full 0.973
_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  0.0361
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21622
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.052
_exptl_absorpt_coefficient_mu    2.567
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97696
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.953
_refine_diff_density_min         -1.488
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         10543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+5.3519P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0869
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9517
_reflns_number_total             10543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00083_si_002.cif
_cod_data_source_block           5
_cod_original_cell_volume        2991.40(16)
_cod_database_code               4088439
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C5(H5), C6(H6), C7(H7), C77(H77), C50(H50), C70(H70),
 C10(H10), C11(H11), C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20),
  C21(H21), C22(H22), C26(H26), C28(H28), C29(H29), C31(H31), C32(H32),
 C34(H34), C36(H36), C38(H38), C39(H39), C41(H41), C42(H42), C46(H46), C48(H48),
  C49(H49), C52(H52), C53(H53), C58(H58), C59(H59), C60(H60), C61(H61),
 C62(H62), C66(H66), C67(H67), C69(H69), C76(H76), C84(H84), C78(H78), C82(H82),
  C81(H81), C79(H79), C85(H85), C86(H86)
;
_shelx_res_checksum              53007
_shelx_hkl_checksum              5846
_olex2_submission_special_instructions 'No special instructions were received'