Half-sandwich cycloruthenated complexes from aryloxazolines: synthesis, structures, and catalytic activities.
Jia, Wei-Guo; Zhang, Tai; Xie, Dong; Xu, Qiu-Tong; Ling, Shuo; Zhang, Qing; Dalton transactions (Cambridge, England : 2003) 45 (2016) 14230–14237; doi:10.1039/c6dt02734b

data_7040253
_publ_section_title
;
 Half-sandwich cycloruthenated complexes from aryloxazolines: synthesis,
 structures, and catalytic activities.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14230
_journal_page_last               14237
_journal_paper_doi               10.1039/c6dt02734b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C19 H21 Br Cl N O Ru'
_chemical_formula_sum            'C19 H21 Br Cl N O Ru'
_chemical_formula_weight         495.80
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-01-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r5133)
;
_audit_update_record
;
2016-01-07 deposited with the CCDC.
2016-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 112.8040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.0729(12)
_cell_length_b                   12.2096(7)
_cell_length_c                   16.3538(9)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      27.2163
_cell_measurement_theta_min      2.6095
_cell_volume                     3878.8(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32953
_diffrn_reflns_theta_full        27.64
_diffrn_reflns_theta_max         27.64
_diffrn_reflns_theta_min         1.97
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.012
_exptl_absorpt_correction_T_max  0.6132
_exptl_absorpt_correction_T_min  0.5704
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         8979
_refine_ls_number_restraints     553
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0323P)^2^+2.8155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0835
_reflns_number_gt                6518
_reflns_number_total             8979
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt02734b2.cif
_cod_data_source_block           jwg2e
_cod_depositor_comments
'Adding full bibliography for 7040251--7040253.cif.'
_cod_database_code               7040253
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=
 Sof(H9AC)=1-FVAR(1)
 Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C22(H22), C23(H23), C25(H25),
 C26(H26), C27(H27), C8A(H8A)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C30(H30A,H30B), C31(H31A,H31B)
5.c Me refined with riding coordinates:
 C10(H10A,H10B,H10C), C10(H10D,H10E,H10F), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C)
5.d Aromatic/amide H refined with riding coordinates:
 C18(H18), C16(H16), C15(H15), C37(H37), C35(H35), C34(H34)
5.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C20(H20A,H20B,H20C), C9A(H9AA,H9AB,H9AC)
;
_olex2_submission_special_instructions 'No special instructions were received'