Encapsulating ruthenium in silica using a single source precursor: Differing outcomes for a cycloaddition reaction
Barik, Chandan Kr; Ganguly, Rakesh; Garcia, Felipe; Leong, Weng Kee; Inorganica Chimica Acta 512 (2020) 119833–; doi:10.1016/j.ica.2020.119833

data_1564051
_publ_section_title
;
 Encapsulating ruthenium in silica using a single source precursor:
 Differing outcomes for a cycloaddition reaction
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119833
_journal_paper_doi               10.1016/j.ica.2020.119833
_journal_volume                  512
_journal_year                    2020
_chemical_formula_sum            'C56.66 H65.32 Cl1.32 O16 P2 Ru2 Si2'
_chemical_formula_weight         1369.38
_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
_cell_angle_alpha                99.0370(16)
_cell_angle_beta                 98.5968(17)
_cell_angle_gamma                117.3761(14)
_cell_formula_units_Z            2
_cell_length_a                   12.6618(4)
_cell_length_b                   13.7592(4)
_cell_length_c                   20.8909(6)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      28.53
_cell_measurement_theta_min      2.35
_cell_volume                     3088.14(17)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'APEX3 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2015)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XS, VERSION 2013/1'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            109581
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.169
_diffrn_reflns_theta_min         2.040
_exptl_absorpt_coefficient_mu    0.701
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction 
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1403
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.347
_refine_diff_density_min         -1.208
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         19922
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+4.7944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                14928
_reflns_number_total             19922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lwk501.cif
_cod_data_source_block           lwk501
_cod_original_cell_volume        3088.13(16)
_cod_database_code               1564051
_shelx_estimated_absorpt_t_min   0.872
_shelx_estimated_absorpt_t_max   0.946
_shelx_res_checksum              33385
_shelx_hkl_checksum              47811