Adsorption of Ruthenium and Iron Metallocenes on Silica: A Solid-State NMR Study
Cluff, Kyle J.; Bhuvanesh, Nattamai; Blümel, Janet; Organometallics 33 (2014) 2671–; doi:10.1021/om500254w

data_4083172
_publ_section_title
;
 Adsorption of Ruthenium and Iron Metallocenes on Silica: A Solid-State
 NMR Study
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2671
_journal_paper_doi               10.1021/om500254w
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C18 H22 Ru'
_chemical_formula_sum            'C18 H22 Ru'
_chemical_formula_weight         339.42
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-01-08
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.262(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3717(14)
_cell_length_b                   6.5709(7)
_cell_length_c                   17.5678(19)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      61.01
_cell_measurement_theta_min      3.59
_cell_volume                     1419.6(3)
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.839
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.839
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29166
_diffrn_reflns_point_group_measured_fraction_full 0.839
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         61.056
_diffrn_reflns_theta_min         3.594
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.772
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.4831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1332 before and 0.0793 after correction.
The Ratio of minimum to maximum transmission is 0.6425.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.496(10)
_refine_ls_extinction_coef       0.0037(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         4278
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0209
_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^)+(0.0322P)^2^+0.0394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0514
_refine_ls_wR_factor_ref         0.0514
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.839
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                4260
_reflns_number_total             4278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500254w_si_001.cif
_cod_data_source_block           adi8
_cod_depositor_comments          'Adding full bibliography for 4083172.cif.'
_cod_database_code               4083172
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.720
_shelx_estimated_absorpt_t_min   0.474
_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:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C15(H15A,H15B), C16(H16A,
 H16B), C17(H17A,H17B), C18(H18A,H18B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C27(H27A,H27B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B),
  C36(H36A,H36B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C12(H12), C13(H13), C14(H14), C21(H21), C22(H22),
 C23(H23), C30(H30), C31(H31), C32(H32)
;
_shelx_res_checksum              70091
_shelx_hkl_checksum              35375