Synthesis, Spectroscopic and Theoretical Studies of Ruthenafuran and Osmafuran Prepared by Activation of Ynone in Alcohol
Tsui, Wai-Kuen; Chung, Lai-Hon; Tsang, Wai-Him; Yeung, Chi-Fung; Chiu, Chun-Hong; Lo, Hoi-Shing; Wong, Chun-Yuen; Organometallics 34 (2015) 1005–; doi:10.1021/acs.organomet.5b00009

data_4085645
_publ_section_title
;
 Synthesis, Spectroscopic and Theoretical Studies of Ruthenafuran and
 Osmafuran Prepared by Activation of Ynone in Alcohol
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1005
_journal_paper_doi               10.1021/acs.organomet.5b00009
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C31 H27 Cl3 N4 O6 Ru'
_chemical_formula_weight         758.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.146(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5070(4)
_cell_length_b                   16.9819(5)
_cell_length_c                   16.3624(5)
_cell_measurement_reflns_used    5383
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      29.2237
_cell_measurement_theta_min      2.9958
_cell_volume                     3137.08(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14556
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.574
_refine_diff_density_min         -1.238
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         6777
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0743P)^2^+12.2658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1631
_reflns_number_gt                5586
_reflns_number_total             6777
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00009_si_001.cif
_cod_data_source_block           COMPLEX_2
_cod_original_cell_volume        3137.08(17)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4085645