M-Ge-Si thermolytic molecular precursors and models for germanium-doped transition metal sites on silica.
Dombrowski, James P.; Kalendra, Vidmantas; Ziegler, Micah S.; Lakshmi, K. V.; Bell, Alexis T.; Tilley, T. Don; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7340–7349; doi:10.1039/d4dt00644e

data_7715735
_publ_section_title
;
 M-Ge-Si thermolytic molecular precursors and models for germanium-doped
 transition metal sites on silica.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7340
_journal_page_last               7349
_journal_paper_doi               10.1039/d4dt00644e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_sum            'C36 H81 Cl0 Ge O13 Si3'
_chemical_formula_weight         878.86
_chemical_name_common            jpd20140604
_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
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2024-02-12 deposited with the CCDC.	2024-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                89.814(2)
_cell_angle_beta                 82.779(2)
_cell_angle_gamma                77.669(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5475(4)
_cell_length_b                   13.4409(6)
_cell_length_c                   20.5234(8)
_cell_measurement_reflns_used    6235
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.45
_cell_measurement_theta_min      2.20
_cell_volume                     2551.78(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  SHELXL-2014
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.1030
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19241
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         1.551
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_description       plate
_exptl_crystal_F_000             950
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.304
_refine_diff_density_min         -1.035
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         9408
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0703
_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^)+(0.0649P)^2^+3.7546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1487
_refine_ls_wR_factor_ref         0.1693
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6088
_reflns_number_total             9408
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00644e2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7715734--7715737.cif.'
_cod_database_code               7715735
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.938
_shelx_estimated_absorpt_t_max   0.993
_shelx_res_checksum              50779