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_1564049
_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            'C44 H36 O10 P2 Ru2'
_chemical_formula_weight         988.81
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 99.086(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4234(9)
_cell_length_b                   19.0090(13)
_cell_length_c                   20.6686(15)
_cell_measurement_reflns_used    8620
_cell_measurement_temperature    103.(2)
_cell_measurement_theta_max      28.1722
_cell_measurement_theta_min      2.2652
_cell_volume                     4043.9(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2018)'
_computing_data_collection       'APEX3 (Bruker AXS Inc., 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2018)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2018)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT (Bruker AXS Inc., 2018)'
_diffrn_ambient_temperature      103.(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10048
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.58
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker D8 Quest'
_exptl_absorpt_coefficient_mu    0.886
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.240
_refine_diff_density_max         1.730
_refine_diff_density_min         -0.703
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         10048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+8.3790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.1036
_reflns_number_gt                7989
_reflns_number_total             10048
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lwk338.cif
_cod_data_source_block           lwk338
_cod_database_code               1564049
_shelx_res_checksum              51607
_shelx_hkl_checksum              85646