First cycloruthenation of 2-alkenylpyridines: synthesis, characterization and properties
Wu, Yuhao; Su, Xianlong; Xie, Chaoyi; Hu, Rongrong; Li, Xianghong; Zhao, Qiang; Zheng, Guoli; Yan, Junkun; RSC Advances 11 (2021) 4138–4146; doi:10.1039/D0RA09833G

data_7242153
_publ_section_title
;
 First cycloruthenation of 2-alkenylpyridines: synthesis, characterization
 and properties
;
_journal_issue                   7
_journal_name_full               'RSC Advances'
_journal_page_first              4138
_journal_page_last               4146
_journal_paper_doi               10.1039/D0RA09833G
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C33 H26 N5 Ru, F6 P,2[CH4O]'
_chemical_formula_sum            'C35 H34 F6 N5 O2 P Ru'
_chemical_formula_weight         802.71
_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
_audit_creation_date             2020-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-22 deposited with the CCDC.	2021-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                99.165(3)
_cell_angle_beta                 93.603(3)
_cell_angle_gamma                91.597(3)
_cell_formula_units_Z            2
_cell_length_a                   7.5639(4)
_cell_length_b                   12.0236(5)
_cell_length_c                   19.0129(9)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.3645
_cell_measurement_theta_min      2.4823
_cell_volume                     1702.43(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0866
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29410
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.717
_exptl_absorpt_coefficient_mu    0.581
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dull blackish black'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.857
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         29410
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1070P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1864
_refine_ls_wR_factor_ref         0.2026
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22141
_reflns_number_total             29410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra09833g2.cif
_cod_data_source_block           1
_cod_database_code               7242153
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.801
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.656(4)
 0.344(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26), C28(H28), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35)
;
_shelx_res_checksum              149
_shelx_fab_checksum              760
_platon_squeeze_special_details
;
A solvent mask was calculated and 72 electrons were 
found in a volume of 238\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 2[CH4O] per
Formula Unit which account for 72 electrons per unit cell.
;
_olex2_submission_special_instructions 'No special instructions were received'