Pyridylpyrrolido ligand in Ge(ii) and Sn(ii) chemistry: synthesis, reactivity and catalytic application
Pahar, Sanjukta; Sharma, Vishal; Tothadi, Srinu; Sen, Sakya S.; Dalton Transactions  (2021) –; doi:10.1039/D1DT03136H

data_7708782
_publ_section_title
;
 Pyridylpyrrolido ligand in Ge(ii) and Sn(ii) chemistry: synthesis,
 reactivity and catalytic application
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03136H
_journal_year                    2021
_chemical_formula_moiety         'C20 H38 Ge N2 Si4'
_chemical_formula_sum            'C20 H38 Ge N2 Si4'
_chemical_formula_weight         491.49
_chemical_name_systematic        Pypyr_Ge-SiTMS
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_audit_block_doi                 10.5517/ccdc.csd.cc28t8s5
_audit_creation_date             2021-05-27
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.05.01 svn.r6f5a8f70 for OlexSys, GUI svn.r6320)
;
_audit_update_record
;
2021-09-13 deposited with the CCDC.	2021-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                77.6820(10)
_cell_angle_beta                 83.9090(10)
_cell_angle_gamma                69.3980(10)
_cell_formula_units_Z            2
_cell_length_a                   8.7746(3)
_cell_length_b                   9.7135(4)
_cell_length_c                   17.1214(7)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.28
_cell_volume                     1333.75(9)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution
'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.984
_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  0.0470
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26560
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.548
_diffrn_reflns_theta_min         2.281
_exptl_absorpt_coefficient_mu    1.337
_exptl_absorpt_correction_T_max  0.679
_exptl_absorpt_correction_T_min  0.624
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1118 before and 0.0607 after correction.
The Ratio of minimum to maximum transmission is 0.6972.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.010(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         8042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+0.5367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0743
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7294
_reflns_number_total             8173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03136h2.cif
_cod_data_source_block           mo_sp_09102020_0m
_cod_database_code               7708782
_shelx_shelxl_version_number     2018/3
_publ_section_exptl
;
Any special experimental details
;
_shelx_estimated_absorpt_t_max   0.698
_shelx_estimated_absorpt_t_min   0.645
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C9(H9), C5(H5), C4(H4), C2(H2)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C21(H21A,
 H21B,H21C), C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              10938
_shelx_hkl_checksum              4949
_olex2_submission_special_instructions 'No special instructions were received'