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_4088440
_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 H48 Cl2 Os P3 S 1+, B F4 1-, 2(C H2 Cl2)'
_chemical_formula_sum            'C63 H52 B Cl6 F4 Os P3 S'
_chemical_formula_weight         1423.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.8000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.11140(10)
_cell_length_b                   46.8609(3)
_cell_length_c                   12.70430(10)
_cell_measurement_reflns_used    27312
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      59.4413
_cell_measurement_theta_min      3.6057
_cell_volume                     6012.48(9)
_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      173.0
_diffrn_measured_fraction_theta_full 0.809
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.809
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            40502
_diffrn_reflns_point_group_measured_fraction_full 0.809
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         59.518
_diffrn_reflns_theta_min         3.609
_exptl_absorpt_coefficient_mu    7.969
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45944
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       block
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.045
_refine_diff_density_min         -1.250
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.280
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         8784
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.280
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0006P)^2^+27.2011P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8493
_reflns_number_total             8784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00083_si_002.cif
_cod_data_source_block           7
_cod_database_code               4088440
_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. Uiso/Uaniso restraints and constraints
Uanis(C231) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C1S(H1SA,H1SB)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C216(H216), C336(H336), C135(H135), C226(H226),
 C232(H232), C222(H222), C125(H125), C214(H214), C112(H112), C223(H223),
 C322(H322), C126(H126), C236(H236), C116(H116), C136(H136), C215(H215),
 C122(H122), C225(H225), C124(H124), C212(H212), C326(H326), C332(H332),
 C134(H134), C132(H132), C235(H235), C233(H233), C123(H123), C323(H323),
 C213(H213), C325(H325), C113(H113), C115(H115), C335(H335), C312(H312),
 C133(H133), C324(H324), C234(H234), C333(H333), C224(H224), C315(H315),
 C114(H114), C334(H334), C313(H313), C316(H316), C314(H314)
;
_shelx_res_checksum              19358
_shelx_hkl_checksum              93106
_olex2_submission_special_instructions 'No special instructions were received'